text:
|Publication number
|Publication type
|Application number
|Publication date
|Nov 16, 2004
|Filing date
|Feb 10, 2003
|Priority date
|Aug 11, 1995
|Fee status
|Also published as
|Publication number
|Kenneth John Kirsten
|Original Assignee
|Kac Holdings, Inc.
|Export Citation
|BiBTeX, EndNote, RefMan
|Patent Citations (19), Referenced by (4), Classifications (81), Legal Events (7)
|External Links: USPTO, USPTO Assignment, Espacenet
This application is a divisional of U.S. application Ser. No. 08/644,912, filed May 28, 1996 which is a continuation-in-part of application Ser. No. 08/514,049, filed Aug. 11, 1995 now abandoned, the disclosure of which is incorporated herein by reference thereto.
The invention relates generally to electrical interconnection of electrical components to substrates, in particular flip-chip reflow soldering and specifically the development of encapsulant-forming compositions.
Epoxy resin compositions have been used as semiconductor device encapsulants for over 25 years as noted by reference to U.S. Pat. No. 3,449,641, granted Jun. 10, 1969.
Anhydride-cured epoxy resin encapsulants used in flip-chip manufacturing methods are described in U.S. Pat. No. 4,999,699, granted Mar. 12, 1991, and U.S. Pat. No. 5,250,848, granted Oct. 5, 1993. Encapsulant-forming compositions are applied after electrical interconnection.
The application of an encapsulant-forming (encapsulating), composition prior to interconnection by reflow soldering, wherein electrical interconnection occurs in the presence of an encapsulating composition is described in U.S. Pat. No. 5,128,746, granted Jul. 7, 1992. In U.S. Pat. No. 5,128,746, flip-chip production methods are described where electrical interconnection is achieved by adding a fluxing agent to a mixture of epoxy resin and curing agent prior to cure. During reflow soldering, the fluxing agent is activated and the resin is cured.
The use in the prior art of cross-linking agents having flux properties is found in PCT International Publication Number WO 93/06943, published Apr. 15, 1993 and its U.S. counterpart, U.S. Pat. No. 5,376,403, granted Dec. 27, 1994. In the publication, enhanced sintering is described using a protected cross-linking agent with fluxing properties in a metal powder and epoxy resin system where the solder is used to form the conductive film. Solder powder addition is used to sinter the metal powder, typically copper or silver, before setting the resin in order to create solid electrically conductive bridges between the powdered metal particles.
The use of synthetic thermosetting polymer resins together with soldering flux agents is described in U.S. Pat. No. 3,791,027, granted Feb. 12, 1974. Therein epoxide resin compositions are described wherein fluxing agents react with the epoxide resin to strengthen solder joints.
Electrically conductive adhesive compositions in which solder powder, a chemically protected cross-linking agent with fluxing properties and a reactive monomer or polymer (inclusive of epoxy resins) are described in U.S. Pat. No. 5,376,403, granted Dec. 27, 1994.
In the present invention, the fluxing additive of U.S. Pat. No. 5,128,746 is eliminated, while the function of fluxing is retained by selecting a cross-linking agent that has the property of also operating as a fluxing agent. In the flip-chip production method of the present invention, where electrical interconnection occurs within the encapsulating composition, the preferred embodiment of the invention resides in selecting a combination of dual functioning cross-linking agent and thermosetting resin or combination of such agent and thermosetting resin with a selected catalyst and controlling the sequence of flow soldering and gel formation to avoid inhibition of soldering. This is accomplished by providing an encapsulant composition, which, at surface mount reflow profile conditions, in which the gel formation (gel point is reached) after solder melt; that is, the gel is formed/gelation occurs after reflow soldering, whereby soldering is not inhibited.
As noted by reference to "MANUFACTURING TECHNIQUES FOR SURFACE MOUNTED ASSEMBLIES," Wassink, R. K. and Verguld, M. F., 1995 ELECTROCHEMICAL PUBLICATIONS, LTD., soldering methods (and equipment) have converged from various IR soldering concepts to one main method, namely, hot-convection soldering. Besides this method other methods are used, but only in specific cases, such as resistance soldering for outer lead bonding of TAB and for soldering on foils.
In Wassink et al., at pages 275, 276, a typical profile for reflow soldering is described. A hot-air convection soldering oven having a number of zones whose temperature can be controlled separately is used in order to attain the desired temperature profile along the length of the entire oven. Such profile enables all joint areas to reach the soldering temperatures with limited temperature differences between the joint areas of components with different thermal mass.
Wassink et al. describes the typical three step heating approach of the prior art frequently used in reflow soldering using multiple hot-air convection ovens.
As also described in Wassink et al., the three steps are:
(i) starting with rapid heating to bring heat into the product (this reduces the length of the oven);
(ii) second step concerns temperature equalizing, i.e., to reduce the temperature differentials; usually a kind of temperature plateau for the hottest parts is pursued while the temperature rise of the coldest parts is chosen to be relatively slow; the effectiveness of this step can easily be assessed by the temperature differentials that exist on the assembly just before it enters the next step;
(iii) final rapid heating and subsequent cooling.
As further described in Wassink et al., each limit of the profile is determined by the maximum allowable thermal load of one of the parts of the assembly to be soldered.
The maximum (peak) temperature is determined by the base material of the printed board. Higher temperatures than 280� C. will cause delamination. (Note: In most cases the printed board is the hottest component.)
The minimum soldering (peak) temperature is determined by the wetting of component metallizations.
The maximum time and temperature of the equalize region is determined by the solder paste. In the case of too heavy a thermal treatment, the activator (flux) in the solder paste will be consumed already at this stage of the process.
The time for which the solder is in the molten stage (in combination with a maximum temperature) is restricted by the formation of intermetallic layers inside the soldering joint. These layers make the soldered joint more brittle.
The specific values of the mentioned boundaries are determined based on the components and board material used.
A surface mount reflow profile for a 63 Sn/37 Pb solder illustrating the typical ranges is shown in FIG. 4.
In U.S. Pat. No. 3,791,027 ("Angelo"), the disclosure of which is incorporated herein by reference thereto, polymers and other materials which contain chemical functionalities; such as, amide, amino, carboxyl, imino, and mercaptan; which serve as flux agents are described. When soldering metals, these materials can be combined with materials which contain other functionalities; such as, epoxide and isocyanate to produce thermosetting polymers. Angelo describes three polymer categories in his invention which are set forth below.
1. Chemical functionalities; such as, carboxy terminated polybutadiene and carboxy terminated polyisobutylene, which, when used alone, do not harden and are easily removed with solvents. These are in essence fluxes and contain the same chemical functionalities found in traditional soldering fluxes.
2. Formulations that are non-crosslinking and can be softened or melted with the addition of heat. Examples cited in Angelo include Versarid 712 and Acryloidat 70. Since cross-linking does not take place, these formulations are similar to standard rosin or resin based fluxes frequently used in reflow soldering which contain chemical functionalities such as amino, carboxyl, amide, etc. Thus the same chemical functionalities are present both traditional rosin and resin fluxes and in the examples cited in Angelo which do not chemically cross-link to form thermoset polymer and hence may be removed by using a solvent or may be reheated and remelted to enable resoldering of solder joints.
3. Combinations of materials, which contain the chemical functionalities necessary to promote solder wetting; such as, carboxy, amino, etc., and materials that react chemically to form thermosetting polymers that cannot be easily removed through use of a solvent or reheated and remelted. Specifically Angelo shows examples of combinations of materials which contain such functionalities with epoxy resin materials which, when heated, form cross-linked networks which are not easily removable or cannot be remelted. Angelo cites the usefulness of such combinations to reside in their ability to reinforce the strength of the solder joint in situations when there is a low probability that a solder joint will need to be resoldered.
Pennisi, et al., U.S. Pat. No. 5,128,746, also describes the use of combinations of materials which contain chemical functionalities known to serve as fluxes and materials; such as, epoxy resins, which when reacted with the addition of heat, form chemically cross-linked polymers which add strength to solder joints and are not easily removable. Although Pennisi describes the function of the epoxy thermoset polymers as providing environmental protection to the flip-chip, the epoxy encapsulant described by Pennisi is also known to strengthen the fragile solder joints. Pennisi lists flux agents; such as, malic acid and other dicarboxylic acids that remove metal oxides and promote solder wetting. In essence, a material, malic acid, containing the carboxyl functional group, which is known to promote solder wetting, is combined with materials, epoxy resins, that form cross-linking, thermoset polymers.
In a third example, described in Capote, U.S. Pat. No. 5,376,403, a material containing a chemical functionality, such as carboxyl, known to assist in solder wetting, is combined with materials that form cross-linking thermoset polymers that are used in ink systems that assist in the fusing of low melting alloy powders with high melting metals and assist in the adhesion of the resultant metal network to a substrate.
In each case (Angelo, Pennisi, Capote) in which a material containing a chemical functionality, known to promote solder wetting, is combined with materials such as epoxy resins that form thermoset polymers, a method of heating is described in which the assembly is heated rapidly above the solder melt point. The application of temperatures above the solder melt point 183� C. is critical as the solder must liquify in order to wet the surface metal.
As thermosetting polymers are initiated by the application of heat in order to stimulate cross-linking reactions, it becomes necessary to understand the cure kinetics involved in the curing of the material combinations selected. By chemically protecting the cross-linking material of the combination, Capote ensures that the cross-linking reactions are delayed and appropriate during the rapid heating process described in his invention.
Similar heating methods are described in Angelo and Pennisi, who both describe the application of heat during the soldering process as quick and rapid. As described previously in Wassink et al., a three step heating profile is typically used to solder electronic components to substrate boards. Rapid heating, as called for in Angelo, Pennisi and Capote, would adversely affect the parts and assemblies during soldering. This includes damage to components at high thermal excursion rates.
Thus, one frequently finds the heating step to be done using multizone ovens which allow materials in assemblies to achieve thermal equilibrium at temperatures above room temperature but lower than the solder melt point (183� C.) in order to reduce thermal shock and subsequent damage. In SMT, this heating process in known as a surface mount reflow profile.
Therefore, in using combinations, as set forth by Angelo, Pennisi and Capote, in which materials containing chemical functionalities; such as carboxyl and amino, known to promote solder wetting, are combined with materials that form cross-linked thermoset polymers through the addition of the heat, heating processes are used that do not involve a rapid heating rate to the solder temperature but instead allow materials to be used in the final assembly to reach a thermal equilibrium. Above room temperature but lower than soldering temperature, it becomes critical to understand the cure kinetics of the combination of thermosetting materials, in view of the desired non-rapid heating profile in order to prevent significant crosslinking of the combination prior to solder melt point.
The present invention relates to thermosetting resin encapsulating formulations in which the cross-linking agent functions as flux for reflow soldering. Included in such formulation are systems in which the cross-linking of resin with such dual purpose cross-linking agent is effected by a catalyst. In the present invention, the cross-linking agent acts as a fluxing agent at reflow soldering conditions and acts as a cross-linking agent in the involved resin system in a manner such that soldering is not inhibited by premature gelling.
In systems of the present invention, where electrical connections along a single axis are involved and reflow soldering is effected in a liquid resin system, the sequencing of stages of cross-linking vis-a-vis reflow soldering is critical.
It is essential that the gel point of the system not be reached prior to formation of the interconnection by liquid solder which interconnection occurs at reflow solder temperature.
It has been observed that where the gel point is reached before melting of the solder, the solder does not wet and does not effectively engage the opposing locus where the electrical interconnection is to be made because solder flow is restricted.
It is believed that the criticality of this requirement in the system of the present invention derives from the inability of the solder to flow in a resin system where the gel point has been reached. It is believed that where the resin system enveloping the solder is liquid, even where the viscosity is great, the melted solder traverses and bonds to the opposing target area and is fluxed by the cross-linking agent. In fact, where a mixed phase exists, wetting, bonding and fluxing occur; however, once the gel point is reached and melt occurs, observation of the cured product demonstrates the failure of successful interconnection and the failure of wetting and flow.
One aspect of the present invention relates to an epoxy resin based encapsulant-forming composition for use in reflow soldering of an electrical component to a substrate. The composition forms an acid anhydride epoxy resin system. The fluxing encapsulant composition is composed of an epoxy resin, an anhydride cross-linking agent for the resin that also functions as a fluxing agent at reflow soldering conditions and a catalyst. The combination of compounds comprising the encapsulant composition is selected to provide a composition which does not reach gel point prior to formation of electrical interconnection at said reflow soldering conditions.
The thermosetting resin is preferably an epoxy resin and the cross-linking agent is selected from anhydrides that intrinsically possess the added activity of fluxing at reflow soldering temperatures.
Referring specifically to eutectic tin/lead soldering temperatures (183� C.), examples of anhydrides that serve as fluxes include succinic anhydride, methyltetrahydrophthalic anhydride, polyadipic polyanhydrides, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, polyazelaic polyanhydrides, and admixtures thereof. The fluxing agent of choice is methyltetrahydrophthalic anhydride and the catalyst-containing encapsulant composition of choice is tin octoate.
Another aspect of the invention relates to a method of attachment and encapsulation of integrated circuits, such as flip-chips or ball-grid arrays, wherein reflow soldering is effected by the encapsulant-forming composition. It is essential that the catalyst promotes gel formation during or after soldering, but does not form a resin gel (a gel at or past gel point) before soldering in order not to inhibit soldering by formation of the gel prior to soldering.
Yet another aspect of the present invention relates to an electrical component having a plurality of electrical terminations, each termination is composed of a solder bump; a component carrying substrate having a plurality of electrical terminations corresponding to the terminations of the electrical component; and, an encapsulating material that removes metal oxides from the surfaces of the electrical terminations of both the component and substrate. Such encapsulating material is preferably composed of an epoxy resin, an anhydride that functions as a fluxing agent to remove the oxide coatings from the component terminations and the substrate terminations prior to and during soldering and also reacts with the epoxy. The gel point of the encapsulant-forming composition is reached at or above the soldering temperature. In the assembly, the encapsulating material is disposed between and fills the opening between electrical component and substrate. This may be done either by dispensing encapsulant on the board and then pressing the component onto the encapsulant or by dipping the component in the encapsulant prior to placement on the board. After heating to soldering temperature, the solder is reflowed and electrically connects the electrical component to the substrate. The catalyst present in the encapsulation composition promotes gel formation during or after soldering so that soldering is not inhibited by premature gelling. In other words, fluxing and reflow soldering occur prior to resin system gel point.
The physical properties of the cured epoxy encapsulant include such measurable properties as glass transition temperature, tensile strength, modulus, dielectric strength, and dissipation factor. These properties affect reliability of the final encapsulated component. The application of the product containing the encapsulated component determines the physical properties that the encapsulant must possess.
For example, flip-chip components typically require glass transition temperatures at or above 120� C. The choice of the resin and anhydride components will therefore be restricted to compositions which yield glass transition temperatures at or above 120� C. DGEBA resins, EEW 180-190 are among the resins of choice for this application.
The choice of the resin in the system depends on the desired properties of the final product. The functionality of the resin and its chemical structure will influence the cross-link density of the cured system. Typically, DGEBA or novolak resins are preferred with anhydride cured systems. Epoxy resins based on methylene dianiline; such as, MY720 from Ciba Geigy or resins containing an amine will cause premature gelation before soldering, since the amine acts as a catalyst. Therefore, these latter epoxy resins are unacceptable for use in the present invention.
The present invention involves the use of compositions which function as flux and hardener for thermosetting resins and in particular epoxide resins, the resins of choice, in encapsulating formulations which find application in and are adopted for use at surface mount reflow soldering profile conditions adapted for assembly architecture and composition of the bond sites. The encapsulants of the present invention are formulated based on reflow temperature profile and the bond site composition which, after melt, forms the electrical interconnection.
Thus in accordance with the present invention the soldering profile in such instances includes heating the assembly components to a temperature below the soldering temperature to prevent damage to the assembly parts that are susceptible to injury at high thermal excursion rates. This heating step is dependent on the size, mass and materials used in the assemblies and is referred to in the art as the soak or equilibrium stage of the profile. In connection with computer mother boards, telecommunications equipment and panels of smaller assemblies, the target temperature at the end of the soak step preferably approaches the solder melt point and may range from about 20� C. below the solder melt point up to the melt point thereof. The period of application of heat to achieve the target equilibrium temperature typically varies and may be from about 30 to about 120 seconds for large surface mount assemblies. The soaking step is preceded by a rapid increase in temperature, called the ramp step; the rate of increase in temperatures is selected to achieve maximum heat input without injury such as microcracks, warping and the like and is dependent on the involved architecture and materials. In the case of typical large surface mount assembly temperature increases of about 1� C. to about 4� C. per second prior to soak are the norm. The final step involves a rapid heating step following soak where the assembly is quickly heated to a temperature above the solder powder melting point in order to form the metal interconnection between the assembly components. Typically one component of the assembly is an electrical component such as a packaged or unpackaged integrated circuit and the other component is a substrate for microelectronic circuitry on which the metal bond sites are located. In the art this step is referred to as the spike stage with a total time above melt point typically ranging from about 30 to 90 seconds. The peak temperature at any locus on the assembly is preferably in the 205� C. to 235� C. range.
For low thermal mass assemblies; that is, assemblies less than 0.062 inches thick and/or assemblies having an area typically 10 square inches or less, heat input is typically achieved using a smooth non-stepped ramp at the rate of 1�-4� C. per second. Solder melt typically is achieved for low thermal mass assemblies in a time frame varying from something less than a minute up to about three minutes.
As the thermal mass of the assembly increases, slower heating rates and stepped processes are employed to bring such assemblies up to thermal equilibrium prior to reflow.
A criteria for selection and combination of thermosetting resin and cross-linking agent (whether in the presence of catalyst or otherwise) in order to achieve the requisite sequence of achieving solder melt before the gel point is reached resides in selecting a thermosetting resin and cross-linking agent combination that when heated using differential scanning calorimetry ("DSC") displays initiation of exothermic reaction with the range of about 140� C. to 180� C. for lead tin eutectic mixture. Exothermic activity as observed using DSC correlates to cross-linking activity. The peak of said exotherm in turn correlates with the level of cross-linking that indicates gel formation.
Although in the final analysis gel formation for the specific combination is determined empirically and exceptions occur, the criteria for selection that is generally applicable is to choose polymer systems wherein exothermic activity, as observed using DSC, is preferably initiated at a temperature no lower than 40� C. below the solder melting point and where the peak exothermic activity registered occurs at a temperature above the solder melting point.
Anhydrides, including, in particular, highly active polyanhydrides, are the preferred dual-functioning cross-linking and flux agents for the encapsulant of the present invention.
In addition to the aforesaid anhydrides, other cross-linking agents that are suitable for use in the present invention, though not necessarily with the same order of success, include materials containing chemical functionalities, such as carboxyl, amino, imino, amide, and mercaptan, as described in Angelo, that inherently act as fluxing agents as well as cross-linking agents.
Amine cross-linking agents that provide the requisite latency (gel point formation at or above the melting point of the solder powder), such as Aificure—LX-1 (manufactured by Ajinomoto Co., Inc., Tokyo, Japan), which is heterocyclic diamine having an active hydrogen equivalent 67, may be used.
Amides and other known nitrogen containing curing agents such as melamine, dicyandiamide, imidazoles, hydrazides, thioureas and the like may also be used as cross-linking agents.
Also useful as crosslinking agents are the well-known polydric phenols which are polycondensates of one or more phenols such as phenol, various alkylphenols and naphthols with aldehydes such as formaldehyde, acetaldehyde, acrolein, glyoxal, benzaldehyde, naphthaldehyde and hydroxybenzaldehyde or ketones such as cyclohexanone and acetophenone, vinyl polymerization type polyhydric phenols such as polyvinylphenol and polyisopropenylphenols, the polyhydric phenols of the present first invention, Friedel-Crafts type reaction products of phenols with diols such as those represented by the formula (1):
Dialkoxy compounds represented by the following formula (2):
or, dihalogens represented by the following formula (3):
and Friedel-Crafts type reaction products of phenols with diolefins such as dicyclopentadiene and diisopropenylbenzene.
In assemblies where the inherent fluxing ability of the cross-linking agent is insufficient to form proper metallurgical solder connections, it may be necessary to add additional fluxing agents in order to increase the flux activity to the formulation.
To supplement the fluxing activity possessed by the encapsulant attributable to the combination of cross-linking agent and thermosetting resin, other known fluxes may be added in minor amounts so as not to adversely effect the properties of the cured thermoset polymer. Moreover, in choosing the fluxes, whether the basic cross-linking agents of the present invention with flux activity or the supplemental fluxing agents, low molecular weight compositions which generate outgassing at surface mount reflow soldering conditions utilized cannot be used since the integrity of the encapsulation is compromised when outgassing occurs by the presence of voids in the encapsulant. Accordingly, dicarboxylic acid flux agents which produce outgassing should be avoided.
Moreover, in selecting the supplementary fluxing agent, its effect on material properties, such as adhesion, tensile strength, moisture absorption or glass transition temperature must be considered. Accordingly, compounds appearing to be compounds of choice because of high flux activity, such as dicarboxylic acids, which reduce glass transition temperature and bulk physical properties of the final polymer network, need to be used, if at all, in amounts that do not affect the resultant polymer.
It has been found that the carboxy terminated polyesters used in the ink formulations of U.S. Pat. No. 5,439,164 are suitable as supplementary flux additives in the encapsulants of the present invention.
It has also been found, where the cross-linking agent, in the amounts used, has inadequate activity as flux to achieve the required level of oxide removal, that among the preferred additives are those that cross-link or bind chemically into the polymer matrix and do not retard the physical properties of the resultant polymer network. For this purpose carboxy terminated polyesters have been found to be a suitable flux additive.
The present invention relates to an encapsulant suitable for use at surface mount reflow profile conditions and a method of electrically connecting an electrical component having a plurality of metal bond site terminations to a component carrying substrate having a plurality of metal attachments sites corresponding to the terminations of said electrical component, at surface mount reflow profile conditions. These conditions vary based on the solder used on the solder bumps, typically forming the metal bond site on the electrical component and the composition and architecture of electrical component and substrate involved. The protocol followed is equivalent to that described in FIG. 4 herein. The encapsulant utilized is comprised of a thermosetting resin and a cross-linking agent that acts, below the solder melt temperature, as a fluxing agent which removes oxide coatings from the surface of the metal bond sites on said electrical component and on said component carrying substrate when heated to said solder melt temperature. The thermosetting resin and cross-linking agent combination has a gel point at or above the solder melt temperature, and preferably above the solder melt temperature. The method comprises the steps of: a) removing oxide coating from the surface of metal bond sites while the encapsulant is in liquid form; b) melting the solder at the metal bond sites to electrically connect the electrical component which has the plurality of metal bond site terminations to the component carrying substrate which has the plurality of metal bond site terminations corresponding to the terminations of said electrical component while said encapsulant is in liquid form and prior to said encapsulant reaching its gel point; then c) forming an encapsulant gel; that is, reaching the gel point. Thereafter the gel may be cured to form the encapsulant, thereby providing protection and enhancing the mechanical connection.
The thermosetting resin is preferably an epoxide. The preferred cross-linking agents are a polyanhydride and carboxy terminated polyesters.
The present invention also relates to a method of producing a low thermal mass assembly by, simultaneously, during surface mount reflow soldering, encapsulating and electrically connecting an electrical component having a plurality of metal bond site terminations to a component carrying substrate having a plurality of metal attachments sites corresponding to the terminations of said electrical component utilizing an encapsulant comprised of a thermosetting resin and a cross-linking agent that acts, below the solder melt temperature, as a fluxing agent which removes oxide coatings from the surface of the metal bond sites on said electrical component and on said component carrying substrate. The thermosetting resin and cross-linking agent combination has a gel point at or above, and preferably above, the solder melt temperature. In this method the low thermal mass assembly is ramped at the rate of about 1� C. to about 4� C. per second for a time sufficient to achieve solder melt and electrical interconnection. The steps of the method occur sequentially during ramping, as follows:
1. oxide coating is removed from the surface of the metal bond sites, while the encapsulant is in liquid form;
2. The solder, which may comprise one or the other bond sites is melted to electrically connect the electrical component having a plurality of metal bond site terminations to the component carrying substrate having a plurality of metal attachment sites corresponding to the terminations of said electrical component (the encapsulant is in liquid form during this step and solder melt occurs prior to the encapsulant reaching its gel point); then
3. The encapsulant gel is formed at the gel point. Thereafter, the resultant gel is cured to encapsulate said electrical solder connections. The preferred thermosetting resin is an epoxide. The preferred cross-linking agents are polyanhydride and carboxy terminated polyesters.
Yet another aspect of the present invention relates to a specific encapsulant for encapsulating and electrically connecting a metal bond site of a first electrical component to a metal bond site of a second electrical component at surface mount reflow conditions. The encapsulant comprises an epoxy resin; a cross-linking agent for the resin that also acts as a fluxing agent that removes oxide coatings from the surface of the first and second electrical components; and a catalyst for catalyzing cross-linking of said epoxy resin with said cross-linking agent, the peak exotherm of said mixture of catalyst, epoxy resin, and cross-linking agent as measured using DSC at a ramp rate of 10� C. per minute being at or above the solder melting point whereby the gel point of said cross-linked epoxy resin is reached after solder melt. The preferred catalyst is tin octoate. The preferred cross-linking agents are polyanhydrides.
Another aspect of the present invention relates to a method for selecting the components of the encapsulant wherein the encapsulant is comprised of a thermosetting resin, a cross-linking agent that also acts as a flux and optionally a cross-linking catalyst which comprises: a) identifying the melting point of the involved solder at the metal bond sites; b) heating the encapsulant composition to a temperature exceeding the melting point of such solder; c) measuring the exothermic activity of the encapsulant during heating step b); d) identifying the temperature at which peak endothermic activity occurs; and e) selecting as an encapsulant an encapsulant that displays peak exothermic activity at or above the melting point of the solder.
The selection method suitably also includes identification of the initiation of exothermic activity and selection of the encapsulant also based on initiation of thermal reaction. The encapsulant selected is one that wherein initiation of exothermic activity occurs at a temperature that is no lower than 40� C. and preferably no lower than 30� C. below the solder melt temperature.
FIG. 1 is a sectional elevational view of a device prior to attachment to a substrate.
FIG. 2 is a sectional elevational view of a device after being reflowed to a substrate.
FIG. 3 is a reflow soldering profile of the soldering method of the present invention.
FIG. 4 is a surface mount reflow profile for 63 Sn/37 Pb also applicable to Sn 62/Pb 36/Ag 02 solder illustrating typical parameters where such solders are used.
FIG. 5 is the specific profile referred to in Example 4.
FIG. 6 is a graphic representation charting heat change versus temperature of the encapsulant described in Example 1.
FIG. 7 is a graphic representation charting heat change versus temperature of the encapsulant described in Example 4.
The catalytically activated encapsulant of the present invention comprises (1) thermosetting resin, preferably an epoxy resin, (2) a cross-linking agent for such resin, which also functions as a fluxing agent during reflow soldering, and (3) a catalyst. The components of the encapsulant are selected and combined to form, in combination, a composition having a gel point temperature at or above the soldering temperature whereby surface soldering is not inhibited by gelling prior to soldering when using a surface mount temperature profile. As used herein, gel point temperature is the temperature for the involved thermosetting resin system where, after initiation of catalyzed cross-linking, the gel point is reached. Simply stated, the process of the present invention will not produce a satisfactory electrical connection if, prior to solder melt, which occurs at the solder melt temperature, the gel point of the involved epoxy resin system is reached. The cross-linking agent acts as flux during the soldering step. The cross-linking agent cures the epoxy resin and performs this latter function paired with a catalyst that catalyzes cross-linking activity and causes gel formation at or above the soldering temperature at which electrical connection with solder melt occurs. Other objects and advantages will become apparent to those skilled in the art from a review of the detailed description of the invention which follows.
In systems of the present invention, the sequencing of stages of cross-linking vis-a-vis reflow soldering is critical.
It is essential that the gel point of the system not be reached prior to formation of the connection by liquid solder (solder melt) which connection occurs at surface mount reflow solder temperature.
It has been observed that where the gel point is reached before melting of the solder, the solder does not wet and does not effectively engage the opposing loci to be electrically connected because solder flow is restricted.
It is believed that the criticality of this requirement in the system of the present invention derives from the inability of the solder to flow in a resin system where the gel point has been reached. It is believed that where the resin system enveloping the solder melt is liquid, even where the viscosity is great, effective fluxing occurs. In fact, where a mixed phase exists, wetting, bonding and fluxing occur; however, once the gel point is reached and melt formation occurs after the gel point is reached, observation of the encapsulated assembly demonstrates that successful connection is not achieved. There is a failure of proper melt formation, wetting and flow.
Referring to FIG. 1, a substrate 100 with metallization pattern 110 is selectively coated with an encapsulating material 120. The material is an encapsulant-forming composition comprised of a thermosetting resin, a cross-linking agent for said resin, which also acts as a fluxing agent for reflow soldering and a catalyst selected to provide, in combination with resin and flux, a composition in which gelation of the resin does not interfere with soldering.
An example of a suitable encapsulating material comprises (1) an epoxy resin, diglycidal ether of bisphenol A with an epoxy equivalent weight of 188, (2) methyltetrahydrophthalic anhydride cross-linking and fluxing agent and (3) tin octoate catalyst. The cross-linking agent is an anhydride cross-linking agent which also acts as fluxing agent. The MTHPA cross-linking agent is paired with tin octoate catalyst that catalyzes cross-linking at a temperature at or above about the soldering temperature, thereby preventing premature gel formation prior to formation of the electrical interconnections by flow soldering.
The amount of anhydride relative to epoxy, preferably ranges from about 75 parts to about 85 parts of anhydride per hundred parts of epoxy resin (75-85 phr).
The amount of catalyst in the composition preferably ranges from about 0.1 to about 5 weight percent. In the case of tin octoate, the preferred amount is from about 1.5 to about 2.5 weight percent and the optimal amount is about 2.0 weight percent based on the weight of encapsulant-forming composition inclusive of catalyst.
A device 130 containing solder bumps 140 is positioned so that the solder bumps 140 and the active surface 150 are facing the substrate 100 and aligned with the metallization pattern 110 of the substrate 100. Referring to FIG. 2, the bumped device 230 is moved into intimate contact with the metallization pattern 210. The encapsulant-forming composition 220 wets the device 230, insuring complete coverage of the active surfaces 250 of the device 230. The meniscus 260 provides a continuous seal around the periphery of the device 230 to protect the active surface 250 from environmental contamination. The cross-linking agent contained in the encapsulant-forming composition 220 coats the solder bumps 240 and the metallization pattern 210.
It should be appreciated that although the drawings depict the device 130 as an integrated circuit encapsulated and connected to a substrate, embodiments using other types of surface mounted components having solder bumps or not are within the scope of the invention.
The assembly 270 is reflowed in a conventional manner; the cross-linking agent, functioning as flux, reduces the oxides on the solder 240 and the metallization surface 210, and permits alloying of the solder to the metal.
FIG. 3 represents a typical surface mount profile. The present invention can accomplish both soldering and encapsulation following such typical profile followed by post-cure at substantially lower temperatures than soldering, in accordance with the profile, typically 150� C. for about 1 to 2 hours. Illustrating the requirements of the present invention, by reference to the surface mount profile depicted in FIG. 3, gel formation prior to reflow, Zone 3, would impede soldering. Premature gelation before reflow forms a physical barrier preventing the solder from wetting the target metal surface.
In FIG. 3, Zone 1 depicts the step of preheating in terms of the parameters of the temperature (ordinant) and time period (abscissa) that the entire assembly comprising substrate, components and encapsulant is preheated to a temperature typically 25� C. to 50� C. below the solder melting temperature. Zone 2 depicts the soak step illustrating the period of soak where the temperature of the assembly is allowed to equilibrate. Zone 3 depicts the reflow step when reflow occurs. Zone 4 depicts the cooldown step. The surface mount profile illustrated in FIG. 3 is merely illustrative of a typical profile which is applicable, inter alia, to the embodiment of the invention exemplified in Example 1. Time and temperature on which soldering is dependent, is dependent on the encapsulant and other parameters of the process.
Selection of Encapsulant System Components for Given Reflow Profiles
As noted herein, the present invention relates to solder paste formulations and methods of their use specifically adopted for forming protectively encased isotropic electrical interconnections at reflow profile conditions used in the manufacture of small and large mass assemblies. Such reflow profile conditions require application of heat over time and encapsulant formulation is critical to achieving satisfactory wetting and solder melt to provide electrical interconnection at the bond sites as well as satisfactory encasement/mechanical bonding.
In choosing the encapsulant used in the present invention, selection of thermosetting resin and cross-linking agents having the dual functions required in the present invention is critical in order to enable satisfactory electrical and mechanical bonding at the electrical bond sites to take place. The encapsulant requirements and selections are discussed below.
During the reflow profile, the polymer must not reach its gel point before solder melt, since the molten solder must displace the polymer in order to wet the bonding surface. If the polymer reaches its gel point too quickly, a polymer barrier is formed between the metal surfaces. Since this gelation inhibits the solder from wetting the substrate metal bond pad, it is critical to understand the curing mechanism and kinetics of the polymer in order to understand the effect on soldering.
In thermoset polymers, the addition of heat initiates the irreversible reaction between the epoxy resin and the cross-linking agent. During the cure process the epoxy resin molecules react with the cross-linking molecules to form long polymer chains and networks with increasing viscosity. As the network grows, a point of infinite viscosity is reached called the gel point. At this point the polymer changes from a viscous liquid to a solid that does not flow.
The gel time of thermosetting resins is usually found under isothermal conditions. For example, epoxy samples can be heated at a set temperature and tested using viscosimetric methods to find the gel time. An example of such a method is to heat epoxy resins in sample pans while measuring resistance to flow.
Since the method of heat during the process described in this invention is not isothermal but rather involves a slow heating of the sample to soldering temperatures, it is important to instead estimate the gelation of the polymer by examining the cure kinetics.
Several techniques can be used to examine cure kinetics of the thermoset polymers. One such method is dynamic mechanical analysis (DMA), which measures the polymer's ability to store and dissipate mechanical energy. Another common technique is to use differential scanning calorimetry (DSC), which measures changes in heat.
As the chemical reaction of thermoset resins during polymerization is exothermic, this change in heat can be measured using DSC and related to the extent of chemical reaction. As described by Hadad in Epoxy Resins, Chemistry and Technology, May, ed., Marcel Dekker, 1988, p. 1130, "an assumption is made that the amount of energy given off during the cure is proportional to the extent of chemical reaction." Using techniques described by Hadad it is possible to estimate the kinetic activation energy required for initiation of polymerization. One such method involves generating DSC scans using different heating rates as described in ASTM Method E 698-79. However, since the critical gelation point in order to prevent proper soldering interference as described in this invention must be determined empirically, DSC will be shown to serve only as a guide for proper material combinations as the soldering process has previously been described as ranges. Therefore, a single DSC scan at a single heating rate is used to show the relationship between cure kinetics of thermosetting polymers and their applicability for use in the method of soldering described in this invention.
The following examples serve to illustrate a mode of practicing the invention.
An encapsulating material of the present invention with fluxing properties was prepared by combining the following components:
% by Weight
Shell 828 (DGEBA − EEW = 188)
Catachek 860 (tin octoate)
The material was spread on the copper surface of a standard copper clad FR-4 board. A small ring of 63 Sn/37 Pb eutectic solder was placed on the epoxy. The board was placed in an IR reflow oven. The profile was the standard solder paste reflow used for solder paste. The ring soldered to the copper leaving an epoxy residue which was past its gel point.
The encapsulating material prepared is dispensed on the surface of the metal, copper, which has been plated to an organic substrate, such as FR-4. A solid piece of solder, 63 Sn/37 Pb eutectic, is placed on the surface of the epoxy. The test board, now containing both the encapsulating material and the solder on the surface of the metal, are placed in a reflow oven, either IR or convection and subjected to the standard reflow profile shown in FIG. 3. The epoxy material serves first as a flux and assists in the bonding of the solder to the copper. After the reflow, the epoxy is gelled, that is, proper interconnection is observed.
The encapsulating material prepared in Example 1 is dispensed on the metal bond sites on substrates to which a solder bumped component, such as a flip-chip, would attach. The flip-chip die is placed on the encapsulating material so that the encapsulating material completely interfaces the lap between the die and the substrate, the substrate can be organic, such as FR-4, or inorganic, such as, glass or ceramic. The metal bond sites are copper or gold, with or without a plating of solder. The solder bumps on the die are 63 Sn/37 Pb eutectic, on which the solder from the die bumps reflows and bonds to the bond sites on the substrate. Suitably a high melting alloy, such as 63 Sn/37 Pb, can be used, in which case the eutectic solder plating on the metal bond site would reflow and bond to the bumps. On the die, the flip-chip die, encapsulating material and substrate are aligned and placed in a reflow oven, either IR or convection, and subjected to the standard reflow profile shown in FIG. 3. During the reflow process, the MTHPA component of the encapsulating material serves as a flux and enables the soldering of the component to the board. The pairing of MTHPA and tin octoate also provides an appropriate level of cross-linking during the reflow process, which yields a resin gel suitable for post cure and wherein the gel point is reached at a point in the overall process where soldering is not inhibited.
The following examples serve to illustrate a mode of practicing the invention including selection of encapsulant components.
A mixture of a bisphenol A epoxy resin (Shell Epon 828), methyl tetrahydrophthalic anhydride (MTHPA) (Lonza AC220J) and the catalyst Tris(dimethylaminomethyl)-phenol, commonly referred to as DMP-30 (Lonza AC-30) was prepared according to formulations as described in literature available from the chemical suppliers:
Epon 828
55 parts
43 parts
2 parts
The resultant composition was spread onto a copper heated to 250� C. along with a slug of 63Sn/37Pb solder in accordance with the method set forth by Angelo (U.S. Pat. No. 3,791,027) and in heated rapidly as described in Pennisi U.S. Pat. No. 5,128,746 and Capote U.S. Pat. No. 5,376,403. It was observed that the anhydride (MTHPA) cleaned the surface oxides from the metal surfaces which allowed the solder to wet onto the copper and form a metallurgical interconnect.
This same mixture was then spread onto the metal surface of an FR-4 epoxy glass substrate plated with copper along with a slug of 63Sn/37Pb solder. The substrate, containing the epoxy composition and the solder slug, was placed into an IR reflow oven with multiple heating zones. The temperatures of the zones and the belt speed of the oven had previously been profiled to yield substrate surface temperature profile as shown in FIG. 5.
Using this temperature profile the solder slug did not wet the copper surface on the FR-4 and form a metallurgical connection. Instead the solder slug remained in its original shape and was encapsulated in the cured epoxy.
In addition to the empirical soldering tests described above, DSC was used to examine the cure kinetics of the above epoxy. Using a 50 mg sample and a heating rate of 10� C./min from 50� C. to 230� C., the onset of the cure exotherm was observed at 100� C. while the peak exotherm was observed at 130� C., as shown in FIG. 6. Therefore, using a heating rate of 10� C./min., the maximum exotherm of the cure reaction occurs 50� C. below the melting point of the solder.
Using the same resin and anhydride combination as in Example 4, Lonza ACPI (a proprietary imidazole) was used as a catalyst.
Epon 828
55 parts
43 parts
2 parts
This mixtures was used with solder slugs heated rapidly on copper. The anhydride cleaned the metal oxides and the solder wet and spread onto, the copper surface. When the composition was spread onto copper over FR-4 organic substrate and heated in the multiple zone heating oven, however, the result was the same as described in Example 4. The solder did not change shape and did not spread onto the metal surface.
The DSC scan from 50� C. to 230� C. at 10� C./min on a 50 mg sample showed the exotherm onset to begin at 100� C. and peak at 130� C. Again, although rapidly heating the combination of materials allowed the solder to spread onto the copper, when heated slowly to solder melt point using a multiple zone oven the epoxy system described did not have the necessary latency to remain liquid before soldering.
Similar results were observed using the Epon 828 and MTHPA combination with several other known anhydride cured epoxy catalysts, including Dimethylaminomethylphenol (Lonza AC-10), zinc octoate (Shepard Chemicals), Benzyldimethylamine (Lonza BDMA), Diazabicycloundecene (Air Products Amicure DBU-E), 2-ethylhexanoic acid salt of Diazabicycloundecene (Air Products Amicure SA-102), 2-heptadecylimidazole (Air Products Curezol 2MA-OK), 2-Heptadecylimidazole (Air Products C17Z), 2,4-Diamino-6(2′methylimidazoleyl-(1′))ethyl-s-tri (Air Products 2MZ Azine).
In each case the catalyst was used with a bisphenol A resin (EEW 190) such as Shell Epon 828 and Methyl Tetrahydrophthalic anhydride at 80 parts based on the weight of the resin. Using the catalysts stated above at 1-5 parts based on the weight of the resin, the mixtures were found to clean the metal oxides and promote spreading of 63 Sn/37 Pb solder to copper when heated rapidly, but cured too quickly and inhibited soldering when heated slowly in a multizone conveyorized heating oven as described in Example 4.
Stannous octoate (Ferro Bedford Catachek 860) was selected as a catalyst for the bisphenol A resin, MTHPA composition as described in example 1.
Epon 828
55 parts
43 parts
Stannous octoate
2 parts
This mixture was used with solder slugs heated rapidly on copper. The anhydride cleaned the metal oxides and the solder wet and spread onto the copper surface. When the composition was spread onto copper over FR-4 organic substrate and heated in the multiple zone heating oven, the solder spread onto the metal surface of the copper and the epoxy was partially gelled. Thus the catalyst selection with this combination of resin and crosslinking agent provided the latency for gelation to take place after soldering.
The DSC scan from 50� C. to 230� C. at 10� C./min on a 50 mg sample showed the exotherm onset to begin at 150� C. and peaked well above 200� C., as shown in FIG. 7. Thus, the peak exotherm, which is used to predict latency, occurs well above the solder melt point of 183� C.
Using stannous octoate as a catalyst with MTHPA along with a multifunctional resin such as N,N,N′,N′-Tetraglycidal-4,4′-methylenebisbenzenamine (Ciba Geigy MY720). This tetra-functional resin has a higher reactivity than one based on bisphenol A. A mixture of MY720 with MTHPA at 90% of the stoichiometric ratio was prepared with stannous octoate used as the catalyst and added at 1 part based on the weight of the resin.
Stannous octoate
Using this composition in the rapid heating method described in Example 1 the solder spread and formed a metallurgical connection to the copper. However, when using the heating method involving the multizone oven the solder did not spread or wet onto the copper. Eliminating the stannous octoate and using the MY70/MTHPA combination described showed the same result. The solder was inhibited from wetting the copper when heating the sample in the multizone oven.
When cycloaliphatic resins such as 3,4-Epoxycyclohexylmethyl-3,4-epoxycyclohexane carboxylate (Union Carbide ERL-4221) are used in combinations with MTHPA are used with stannous octoate as the catalyst the soldering result observed is similar to Example 1. The composition cures before solder melt point and inhibits the spread of the solder to the copper.
A DSC scan of the composition:
49 parts
49 parts
Stannous Octoate
2 parts
at a heating rate of 10� C./min showed the exotherm onset at 90� C. with a peak exotherm at 155� C. Thus, the exotherm peak, which correlates to the chemical reaction rate, is lower than the melting point of the solder alloy.
A blend of epoxy resins Epon 828 and ERL 4221 was used with MTHPA and stannous octoate as a catalyst.
Epon 828
Stannous Octoate
This system solder soldered 63 Sn/37 Pb alloy to copper when heated rapidly but did not solder using the multizone heating oven. The DSC onset temperature began at a higher temperature of 120� C. compared to the composition using only the cycloaliphatic resin (ERL-4221). Although the peak exotherm was nearly identical in temperature to the single resin system yet the height of the exotherm was lower with the resin blend system indicating less heat given off and therefore less chemical activity. Thus, blends of highly reactive resins such as cycloaliphatic resins with MTHPA do not provide the necessary latency.
A blend of bisphenol A system, MTHPA and a dicyandiamide type catalyst (Ajinomoto Ajicure AH-150) was used at various catalyst levels.
Epon 828
52-56 parts
40-43 parts
1-8 parts
Using catalyst levels of 1-2 parts based on the weight of the resin were found to solder the 63 Sn/37 Pb alloy both using rapid heating as well as using the multizone oven. However, when used at concentrations above 3 parts based on the weight of the resin the compositions inhibited the solder from spreading using the multi-zone heating profile. Thus, the catalyst level is critical to the rate of reaction. DSC exotherms revealed that the onset of the peak exotherm occurs at lower temperatures as catalyst concentration increases.
The Reflow Profile
The cross-linking catalyst (accelerator) selection is based on the need to inhibit gelation during the soldering process. A most important embodiment of the present invention involves the soldering method known as reflow soldering. In reflow soldering, the components to be soldered to the circuit board or substrate are placed onto the PCB or substrate and such assembly is passed through an oven containing different heating zones. Three zones are typical. The first zone, or heating stage, is commonly called the ramp. In this zone, the surface temperature of the board is quickly raised to heat the materials of the board and components. In the second zone, known as the soak, the temperature of the board is allowed to equalize at this temperature range for a period of time that may be of short duration (1-3 minutes) in order to reduce temperature differentials on the surface of the board and components. The soak time will depend on the type of board, solder and components used. The third step involves a quick temperature spike to exceed the solder melt point. Therefore, the solder melting temperature dictates the temperatures of the zones. Since melting point of 63 Sn/37 Pb is 183� C., the soak temperature is generally 120-160� C. The peak temperature at reflow is generally 200-300� C.
When the encapsulant of the present invention includes a catalyst, the selection of the catalyst is critical and is based on the ability of the catalyst in the epoxy system to catalyze the cross-linking to the point of gelation (gel point) during or after the reflow process, without inhibiting reflow soldering.
By way of explanation, an uncatalyzed combination of a bisphenol A resin combined with a phthalic anhydride derivative, such as MTHPA, when used in a reflow soldering process, would not inhibit soldering but would also not reach its gel point during the reflow process. Such systems would require 6-48 hours of post-cure below soldering temperature (typically 150� C.) in order to reach gelation and fully cross-link. Therefore, a catalyst is necessary to reduce the overall time of cure of these systems. However, it has been observed that, if a catalyst is selected which is too active, the system will reach gelation below the soldering temperature and inhibit the soldering process by forming a physical barrier between solder and target metal.
Anhydride catalysts of the amine type have shown this detrimental phenomenon. Examples of unacceptable catalysts are benzyldimethylamine dimethylamino methyl phenol, tris (dimethylamino methyl) phenol, triethanolamine and monoethanolamine. When these amines are used as catalysts together with bisphenol A epoxy resins, such as shell EPON 828, and phthalicanhydride derivatives such as MTHPA using the standard reflow protocol, premature gelation results which inhibits proper soldering.
Other common anhydride-cured epoxy catalysts have been shown to be detrimental to soldering, as detailed in Example 5, when using blends of bisphenol A resins and MTHPA.
Tin octoate, the catalyst of choice for these systems, is a metal salt of tin and 2-ethylhexoic acid. Although not wishing to be bound, it is believed that the activity of the catalyst arises from the oxidation of the tin from Sn+2 to Sn+4 and the dissociation of the tin from the 2-ethylhexoic acid. When tin octoate is tested using differential scanning calorimetry, an exotherm is observed at 185-190� C. It has been observed and therefore it is believed that the temperature at which the exotherm occurs correlates to the temperature at which catalysis of cross-linking occurs. Accordingly, one method of evaluating onsets of catalytic activity where the mechanism of catalysis of the catalyst being evaluated corresponds to that of tin octoate is to correlate the exotherm of the catalyst with the temperature at which catalysis of cross-linking occurs.
When used in combinations with MTHPA and bisphenol A resins stannous octoate has been shown to effectively provide the required latency necessary to prevent premature gelation of polymer before soldering.
The choice of stannous octoate as an accelerator (cross-linking catalyst) prevents significant gelation of the epoxy during the ramp and soak stages to allow the soldering to take place when using a reflow temperature profile for Sn/37 Pb solder or alloys with similar melting points.
Another example of a suitable encapsulant, comprises (1) an epoxy resin, diglycidal ether of bisphenol A with an epoxy equivalent weight of 185-192, (2) MTHPA cross-linking and fluxing agent and (3) tin octoate catalyst. The cross-linking agent is an anhydride cross-linking agent which also acts as fluxing agent. The MTHPA cross-linking agent is paired with tin octoate catalyst that catalyzes cross-linking at a temperature at or above about the soldering temperature, thereby preventing premature gel formation prior to formation of the electrical connection(s) during reflow soldering.
The amount of catalyst in the composition preferably ranges from about 0.1 to about 10 weight % based on total weight of encapsulant. In the case of tin octoate, the preferred amount is from about 2.5 to about 7 weight percent and the optimal amount is about 5 weight % based on the total weight of the encapsulant.
Optional Additives
A component which can optionally and advantageously be included in the encapsulant of the present invention is a surface tension reducing agent. It is used to reduce the contact angle at the bonding surfaces. The surface tension reducing agent may be a surfactant. Among the suitable surfactants are TWEEN�, available from ICI, Wilmington, Del., and potassium perfluoroalkyl sulfonates. When present, the surface tension reducing additive is preferably added in amounts of from about 0.1 weight % to about 1 weight % based on the total weight of encapsulant.
Another component that optionally is added to the encapsulant composition of the present invention is an adhesion promoter which has the ability to enhance epoxy to metal bonding. Suitable adhesion promoters include organo silanes and titanates. A suitable organosilane is 6040, 3-glycidoxy-propyltrimethoxysilane available from Dow Corning Corp. of Midland, Mich. A suitable titanate is LICA 38, neopentyl (diallyl)oxy, tri(diooctyl)pyro-phosphatotitinate available from Kenrich Petro Chemicals, Inc., in Bayonne, N.J. The adhesion promoter is preferably added in amounts of from about 0.1 weight % to about 1% weight % based on the total weight of the encapsulant.
Yet another component that can optionally be used in the encapsulating composition of the present invention is a defoaming agent such as FOAM BLAST™ 1326, an alkoxylate of fatty esters available from Ross Chemicals. The defoaming agent is preferably added in amounts of from about 0.1 weight % to about 1 weight % based on total weight of based on the total weight of the encapsulant.
It is not intended to limit the encapsulant, surface mount reflow soldering method of manufacture, encapsulant selection and composition and assemblies of the present invention to the particular embodiments described herein, and various modifications may be made, including, but not limited to, changes in the surface mount reflow profiles based on variations in the solder and hence solder melt temperature and conditions of solder melt, the dimensions, shape and materials, without departing from the scope and spirit of the invention as set forth in the following claims.
|Cited Patent
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|Hunt Earl R
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|Oct 26, 1982
|Bell Telephone Laboratories, Incorporated
|Conductive adhesive system including a conductivity enhancer
|Jan 28, 1985
|Aug 5, 1986
|International Business Machines Corporation
|Solder interconnection structure for joining semiconductor devices to substrates that have improved fatigue life, and process for making
|Jul 19, 1985
|Feb 10, 1987
|Kollmorgen Technologies Corporation
|Heat activatable adhesive for wire scribed circuits
|Feb 10, 1987
|Aug 8, 1989
|Lord Corporation
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|Jan 24, 1990
|Dec 25, 1990
|Toagosei Chemical Industry, Co., Ltd.
|Curable composition
|Mar 14, 1990
|Mar 12, 1991
|International Business Machines Corporation
|Solder interconnection structure and process for making
|Jul 17, 1990
|Apr 21, 1992
|Nitto Denko Corporation
|Photosemiconductor device and epoxy resin composition for use in molding photosemiconductor
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|May 26, 1992
|Motorola, Inc.
|Semiconductor device having a low temperature uv-cured epoxy seal
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|Aug 4, 1992
|Motorola, Inc.
|Anisotropic conductive adhesive and encapsulant material
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|Oct 1, 1991
|Dec 27, 1994
|Capote; Miguel A.
|Electrically conductive compositions and methods for the preparation and use thereof
|Jan 27, 1994
|May 23, 1995
|Shin-Etsu Chemical Co., Ltd.
|Epoxy resin compositions and semiconductor devices encapsulated therewith
|Jun 4, 1993
|Aug 8, 1995
|Matsushita Electric Industrial Co., Ltd.
|Methods for joining copper or its alloys
|Citing Patent
|Filing date
|Publication date
|Nov 9, 2009
|Sep 3, 2013
|Taiwan Semiconductor Manufacturing Co., Ltd.
|Semiconductor package structures
|Sep 30, 2011
|Nov 22, 2016
|Intel Corporation
|Fluxing-encapsulant material for microelectronic packages assembled via thermal compression bonding process
|Nov 9, 2009
|Mar 4, 2010
|Taiwan Semiconductor Manufacturing Co., Ltd.
|Semiconductor package structures
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|Oct 10, 2013
|Intel Corporation
|Fluxing-encapsulant material for microelectronic packages assembled via thermal compression bonding process
|U.S. Classification
|International Classification
|Cooperative Classification
|European Classification
|Mar 12, 2004
Owner name: KAC HOLDINGS, INC., ILLINOIS
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U.S. Senate candidate of the Reform Party and gadfly Shawn O'Hara once filed a lawsuit against the Forrest Count Democratic Party saying his rights were violated.
O'Hara claimed that he should be allowed to run in 21 elections in Mississippi and his fifth run for governor.
Rather hilariously O'Hara complains in the 2007 suit because the party had the wrong address for him but he didn't get his paperwork because his paperwork was sent to a vacant lot.
O'Hara lists his address as a PO Box and two phone numbers.
P.O. Box 15275, Hattiesburg MS 39404… 601-271-2700 office and 601-584-9020 home…
Reverse phone lookup of the Home number links to a landline associated with Nancy G Schmitz in Hattiesburg at the address: 361 Macedonia Rd. Petal, MS
Reverse look up of the office phone is a number associated with Shawn Richard, same P.O. Box.
The O'Hara's P.O. Box is also the address for the committee for Barbara Dale Washer, who is a 2014 Reform candidate for House 3rd District in MS. Her campaign lists Devon O'Hara as its Treasurer.
Despite the controversial past of O'Hara–he once helped the KKK–the Mississippi GOP's Delbert Hosemann has helped advance his political career. (See "Where In The World?")
@ChuckCJohnson 2012- Delbert recognizes O'Hara's "faction" of the Reform Party over the Nat'l Reform party #mssen pic.twitter.com/ArM0A9GhCE
— Shannon Knutsen (@STKnutsen) August 26, 2014
If O'Hara drops out of the race for U.S. Senate, any write-in votes would count for Chris McDaniel.


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|hsp_ <piccina...@ibest.com.br>
|Search question, with jcr:path.
|Tue, 15 Jul 2008 12:47:53 GMT
Hi; I have a need to search node in a level that not match some names. Take the following tree: A A/B A/B/D A/C A/C/E So, I want to retrieve the nodes only under A, that have the names (or path) not equal to B (node A/C would be the result in this case). I tried some searches with xpath and sql, but without sucess. Well, in the url http://people.apache.org/~mreutegg/jcr-query-translator/translator.html, I post the following xpath: /jcr:root/A/element(*,my:type)[(@jcr:path!='/A/B')] and in SQL Query box appears: SELECT * FROM my:type WHERE jcr:path <> '/A/B' AND jcr:path LIKE '/A[%]/%' AND NOT jcr:path LIKE '/A[%]/%/%' and in JCR Query tree box appears: + Root node + Select properties: * + PathQueryNode + LocationStepQueryNode: NodeTest={} Descendants=false Index=NONE + LocationStepQueryNode: NodeTest={}Documentador Descendants=false Index=NONE + LocationStepQueryNode: NodeTest={}Acervo Descendants=false Index=NONE + LocationStepQueryNode: NodeTest=* Descendants=false Index=NONE + NodeTypeQueryNode: Prop={http://www.jcp.org/jcr/1.0}primaryType Value={my}type + RelationQueryNode: Op: <> Prop=@{http://www.jcp.org/jcr/1.0}path Type=STRING Value=/A/B I did the search in jackrabbit with xpath and nor result nor exception returned. I did the search in jackrabbit with sql and get the exception: "javax.jcr.query.InvalidQueryException: Invalid combination of jcr:path clauses" How can I do the filter in query to get directly the nodes without handle after in my code? I also tried using fn:name but it only works with "=" predicates. Thanks Helio. -- View this message in context: http://www.nabble.com/Search-question%2C-with-jcr%3Apath.-tp18464397p18464397.html Sent from the Jackrabbit - Users mailing list archive at Nabble.com.
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text:
Let us know when your receive great advice so we can thank our lawyers and point others with similar questions in the right direction.Got it!
I am 19. I got caught at kohls with $160 worth of merchandise. The LP girl said she wouldn't call the police, but I was so scared I had never done this before, and never everrrrr will again. I slowly showed everything I had taken. I still had one thing she hadn't asked for and I was so scared, also being afraid that the amount would keep rising. After she discovered the last item she got angry and called the police. This is my first and LAST time ever doing this. I have no type of record at all. WILL THIS STAY ON MY RECORD? IS THERE ANY WAY I CAN GET IT OFF MY RECORD? WILL I SERVE ANY TIME AT ALL? IS THERE A WAY TO PREVENT SERVING TIME?
Your question does not indicate whether you have gone to court for this case or are awaiting your first court date. Either way, my first piece of advice is that you do everything possible to make the best possible impression on the Judge, the prosecutor, and everyone else you encounter in court. Dress as if you are going to church. Answer all questions, "Yes sir, no sir, yes mam, no mam." If you are addressing a judge, it is, "Yes Your Honor, No Your Honor." Based on my experience as a Massachusetts Criminal Defense Attorney, I can't imagine someone with no record going to jail for shoplifting (incidentally one of my first jobs was as an LP for Filenes so I have some knowledge on that front as well). Do not panic. See if you can resolve your case with a disposition that does not involve you admitting guilt. This will preserve your record and protect your future. In Mass we call this Pre-trial Probation, but I am sure California has its own program for first offenders that is called by another name. No matter what you do, seek the advice of an experinced California Criminal Defense attorney. If you can't afford to hire one, you might still benefit from a free consultation. Depending on the rules in California, you might qualify for a court-appointed attorney. In Massachusetts, the court will only appoint an attorney when there is a possibility of incarceration. Good luck, and use better judgement next time.
Nicolas A. GordonAsk a similar question
Incidents like this only get on your record if you're actually charged by the District Attorney's office and you're convicted.
There are many options in California that a defense attorney can try to work out for you and keep this incident off your record. Every jurisdiction and prosecuting office has different programs and deals they can offer. Given the low dollar amount, it's unlikely you will serve time, although petty theft is a priorable offense. What that means is that if you're convicted this first time and serve at least one day in jail, a second offense for petty theft can be charged as a "petty theft with a prior" - a crime that can be filed as a felony. See the links to blog posts on my website for more information. Hope they help answer questions for you.Ask a similar question
The best way to get this off your record is not to let it get on there in the first place. Don't plead guilty, but get a lawyer and fight it. I accept cases in San Jose. You can call me for a free consultation. You should NOT go into this alone. Try to imagine an employer to whom a THEFT conviction WON'T make a difference in hiring or firing? you are more likely to go to jail if you do NOT get an attorney, in my experience.Ask a similar question
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text:
Love is such a shallow term,
A dictionary entry, a cliched word.
Letters are too ordinary to describe the
Evanescence of the entire universe
That exists beyond you and me.
The passion of passion,
The unfathomable depths of the un-breathable trap
And the silky smooth pearl which drew me to the bottom of it.
The evanescence of even myself,
The existence of nothing but you,
Even within myself.
That isn't love. It's more than that.


text:
University of Connecticut, Farmington, CT
Benign tumors of the tracheobronchial tree are rare and their incidence ranges from 1-5% of all tumors.These tumors are usually peripheral and endobronchial involvement is seldom seen. We describe a case of an endobronchial chondroma which was left untreated for 4 years due to non-compliance and grew to cause complete left lung collapse.
A 54 year old male was evaluated in the pulmonary clinic for a positive tuberculin test and persistent cough. Chest radiograph showed left upper lobe collapse. This prompted a bronchoscopy which revealed a tumor at the bifurcation of the left mainstem bronchus with complete occlusion of left upper lobe orifice. Biopsy showed benign cartilaginous tissue consistent with a chondroma. The patient was lost to follow up for 4 years when he returned with increasing cough, dyspnea and fevers. Chest xray and CT showed near total collapse of left lung with post obstructive pneumonia. A bronchoscopy showed a large tumor protuding from the left mainstem bronchus with 100% occlusion of the lumen. Specimens at bronchoscopy were identical to the tissue obtained four years back. V/Q scan did not show any ventilation or perfusion of the left lung. FEV1 was 1.92L which was reduced from 2.4L at the time of the initial presentation.The patient underwent a left pneumonectomy.
Chondromas are rare benign pulmonary tumors. They are almost always found in the lung parenchyma and can be seen in association with Carney's complex(gastric stromal sarcoma, extra-adrenal paraganglioma with pulmonary chondroma). Failure to follow up on part of our patient led to more extensive surgery with greater loss of pulmonary function. He was not a candidate for laser resection of the tumor as the lung distal to the obstruction was destroyed.
Benign endobronchial tumors although rare should be treated early aggressively with either laser resection or surgery. If left alone they have the potential to destroy an entire lung.
P. Grover, None.
Monday, October 27, 2003
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text:
A few months ago I went to a local LuLaRoe consultant's house to try on some leggings I bought from her Facebook group. It was my first LuLaRoe purchase and I was mostly just a little curious about what the fuss what about. While I was there I decided to try on a few more things. I tried on a dress that I thought wouldn't work on me, guess what? IT WORKED ON ME! I was so excited and wanted to try on more. I ended up leaving her house with 11 items! I was probably her favorite customer that day! On the drive home I thought to myself, "You know what? That was a lot of fun! I want to do this!" I was actually so excited about it, that I pulled over and texted my husband right then and there, "I know what I want to do with my life! I want to be a LuLaRoe consultant!" He texted back, "What's LuLaRoe?" Haha! Now, a few months later we have a basement full of LuLaRoe skirts, shirts, leggings, kimonos and dresses. I've hosted parties, taken pictures and become excited overtime I get a new shipment of inventory!
The clothes! You guys, THE CLOTHES! They're are comfortable! Not only are the comfortable but they're affordable, stylish, fun, modest and practically one-of-a-kind. LuLaRoe only makes about 1200-2000 items using one pattern. They ship them out to various consultants around the US and once they're gone, THEY'RE GONE! If you see an item you like, you need to buy it! You might very well be the only person in your area with that exact dress, leggings, shirt or skirt. Also, the patterns are so fun! My favorites so far have been Bigfoot leggings (my husband is a believer and I tease him about it!), feathers, florals, and solid leggings paired with a fun patterned Irma Tunic.
I was lucky enough to snag the Bigfoot leggings, because they were a legit "unicorn" print. If you're knew to LuLaRoe lingo, a Unicorn print is one that everyone wants and that might be difficult to find in the style and size you want! Like I said above, if you see something you love, you better get it before it's gone! :)
LuLaRoe's story is amazing. It all started with a woman, DeAnne Stidham, our leader wanting to make a skirt for her daughter. Here's a video the full story:
LuLaRoe's designer, Patrick is equally amazing.
I read that before LuLaRoe releases any new style, they test is out on multiple body types to makes sure it's flattering for all! No wonder I fell in love with a dress I thought wouldn't work on me! This company is LEGIT! They knew it would look great on me before I did! I keep telling people LuLaRoe uses magic to sew their clothing items. Maybe it's magic or maybe it's just pure genius and passion, either way I'm so grateful for this company and the confidence they've brought back into my life. I'm wearing clothes I love and feel totally comfortable in, AND I'm able to help other women do the same!
It's so fun to have a customer or friend come over and try on clothes. When they find something they love, you can just see it in their face. I'm so grateful I can be a part of it. As an added bonus, I get to be with my kids, make my own hours and help my family get closer to our dreams. We recently bought a house and want to finish the basement and yard -- which we affectionately refer to as our little dirt patch! We also want to be debt free and travel the world. Because of LuLaRoe I'm much closer to these dreams becoming a reality! I get excited just thinking about it! I get excited overtime another box of inventory arrives! It feels like Christmas every few days I open a new box. I'm happy! I'm fulfilled knowing I'm contributing to our family's income. My children get to watch their mom run a business. I want to teach them that if you put your mind to something and work hard, you can accomplish anything!
If you're like I was and want to know what all the fuss is about, join my Facebook group here.
If you're interested in joining my team click here.
Now, I'm about to go snuggle my kids an watch a movie, because I CAN! Added bonus: I'm wearing a cute and comfy Cassie skirt and Irma shirt while doing it! :)


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€ 8,99
Sofort lieferbar
August 2013
Beschreibung1334 BC: Akhenaten the Sun-Pharoah rules supreme in Egypt. The young Tutahkhamun is groomed to be his successor. But then Akhenaten disappears and his legacy is seemingly swallowed up by the sands that lie under modern Cairo and the great pyramids of Giza ... AD 1885: A half-crazed man appears claiming to know of a vast lost labyrinth beneath modern Cairo, of canals and palaces and tombs. His story won't be believed for almost thirty years, with the discovery of Tutahkhamun's tomb in 1924. Present-day: Jack Howard and his team are excavating one of the most amazing underwater sites they have ever encountered. They hear the story of the crazed engineer. What follows is a rollercoaster ride of adventure and action, as they dive into the Nile into a world three thousand years back in history, inhabited by a people who have sworn to guard the greatest secret of all time...
PortraitDavid Gibbins is the author of seven previous historical adventure novels that have sold over two million copies and are published in twenty-nine languages. He taught archaeology, ancient history and art history as a university lecturer, before turning to writing fiction full-time. He is a passionate diver and has led numerous expeditions, some that led to extraordinary discoveries of ten-thousand-year-old artefacts. David divides his time between England and a farm and wilderness tract in Canada where he does most of his writing.
Untertitel: Sprache: Englisch.
Verlag: Headline
Erscheinungsdatum: August 2013
Seitenanzahl: 480 Seiten
Format: kartoniert


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WMC Interviews: Anne Holland
Over the past three years, I've had the honor of interviewing many brilliant marketers, including Laura Ries, bestselling author, blogger and TV personality; Mike Schultz, president of the Wellesley Hiils Group; and Janine Popick, co-founder and CEO of hosted email marketing platform VerticalResponse.
But last week, I had the unique pleasure of corresponding with Anne Holland, founder of MarketingSherpa and legendary marketing guruess. Though Anne announced her retirement on November 10, she graciously agreed to share some of her collected wisdom and plans for what's next. Here's our discussion.
WebMarketCentral (WMC): Thanks so much for your time today, Anne. First off, why do think MarketingSherpa has been so successful, over a long and turbulent period, in a market where so many paid content providers have failed?
Anne Holland (AH): We were always obsessed with market research. We focused on a single primary market (marketing professionals in corporate America with $3 million + year department budgets) and researched what practical information those folks wanted day in and day out. Then we built it for them. In business, it's all about solving a target market's pain points. Sherpa's in an incredibly competitive space, but I suspect we were one of perhaps only two publishers, targeting marketers, who did this kind of ongoing intensive research before developing products and before picking taxonomy for copywriting. We spent hours on the phone with customers and prospects every week in interviews; we conducted multiple surveys every year to different slices; we studied our site's internal search stat data; etc.
A lot of what businesspeople want is actually good old fashioned reporting. It's not easy. You're not rewriting press releases or dashing off opinion columns. Instead we conducted new research projects continually to present the data to readers. We also went out and dug up people to interview for our Case Studies. Every one of our now 900+ Case Studies were exclusive, requiring about $2,000 of staff time just in research, interviews and crafting. Our research reports contained 200-400 charts and tables, compared to about 50 for many fancy research firms. We even spent hours with speakers before our Summits, helping them craft every aspect of their presentations; we didn't just assume whatever they came up with would be ok. If you're willing to roll up your sleeves and really slog through that kind of hard work, you'll please your audience. Very few people really want to work that hard I think though.
WMC: What are the two or three most important pieces of advice you would give to marketers today?
AH: In this economy, frankly your first concern has to be marketing to your boss and your boss's boss. Few marketers are really comfortable with and savvy enough to market themselves internally in the corporation—I think sales pros are far better at it than we marketers are! Create personas of every person who has power over whether you get the budget you want and the power to execute campaigns the way you want; then figure out them as prospects and market to them. Do you know how to impress the CFO, the CIO and the CEO? Great, then make that happen.
Then focus on your marketplace. Don't take anyone's word for who your marketplace is or what they're all about. Find out for yourself. Meet them in person. Survey them. Review recent demographic studies. Often you'll find two or more unique demographics have been conflated into one by mistake (such as "the financial services industry" which is many separate demographics who must be targeted separately in campaigns). Or your company's targeting is fuzzy. Or the taxonomy of your taglines, key benefit propositions, and/or headlines doesn't match the wording your prospects would use.
The biggest question I get asked is about particular types of campaigns. "Does podcasting work?" "Should I be advertising on Facebook?" "Should I zero out my print ad budget?" Etc. This makes me nuts because marketing success is NOT about the tactic or the media channel, it's about what will appeal to the prospect. What media do they like or use? What types of tactics do they respond to? Every prospect segment is different. Learn your prospect and they will lead you to the tactics and media channels you should use.
That said, sometimes what works is unexpected to everyone involved, prospect included. So you have to dedicate at least 10% of your budget (I'd prefer 20%) to an ongoing regular series of tests. Test media buys first, then test everything else about tactical execution. Set a schedule for testing—weekly, monthly, quarterly—whatever makes sense. But be sure to put it on the calendar or it won't happen.
WMC: Anything you'd like to say about the future—either yours or MarketingSherpa's?
AH: It's been a great, amazing run for me; first 16 years in business media and then nine years founding and building MarketingSherpa. Everything I've been able to accomplish has been due to incredible support from the marketing and media communities. I've had so many mentors and friends, I've lost count. Now it's time for me to redefine myself, to figure out what to do with the rest of my life.
Marketing and publishing were very, very good to me. But, I have to look outside my comfort zone and try new things. I'll probably wind up in some field related to gardening and plant nurseries, but who knows? I feel a lot like I've just graduated from college all over again with a new liberal arts degree and a blank slate for a career. It's scary and very, very exciting. If you'd like to keep up (or you're considering early retirement yourself) I'll continue blogging at http://anne-holland.blogspot.com.
250,000 (or so) marketing professionals say...thanks Anne.
Contact Tom Pick: tomATwebmarketcentralDOTcom
Labels: Marketing People
KudoSurf Me!


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Day Two: Establishing A Governance Around CX
Panel REMIX Organize It: Fully Operationalizing CX Within Your Institution
While it may be easy to get some level of c-suite advocacy, convincing your whole company to get onboard for your CX mission might be a bit more involved. While CX should be something that is every department's responsibility, if there is no central body that oversees communications between the different silo-ed departments that work on cx (like an enterprise wide CX team, or a CX council or advisory board), it will be hard to achieve a holistic view of the customer and streamline brand experience and your mission might not be as effective. Join this session to hear about how to be operationalizing this concept within your institution. Panelists will discuss:
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text:
The UK based Bank NatWest has a new Windows 10 app
UK based bank NatWest just released their new Windows 10 app for the Windows 10 users in the United Kingdom. The new NatWest app is now available to download from Microsoft store.
The app is special as it supports the innovation of Microsoft- Windows continuum. The new app comes with some more new features which are listed below:
- Easily send your account number and sort code so people can pay directly into your account
- Get a reminder of your customer number in the menu
- Continuum so that you can connect a monitor, keyboard and mouse to your Windows 10 Phone for a PC-like experience!
The app currently features:
- Get Cash from your account without using your debit card
- Pay a person or bill
- Pay your contacts using their mobile number
- Transfer money between your NatWest accounts
- Check your balance and transactions
- View and cancel your direct debits and standing orders
- Create standing orders to existing payees
- Find your nearest cash machine or branch
- Top up your UK Pay As You Go mobile phones (available for major UK mobile networks only)
Download Now.


text:
Page 3
Getting up Kmazatron's poseable thumb had appeared, angrily he punched both of his balled fists down on the table, he leaned over looking right into Keiranala's face and flaring his nostrils he scowled menacingly.
"I will talk, shout, bellow and scream as loud as I please I am the high elder" said Kmazatron devilishly through gritted teeth.
Not faltering her gaze, Keiranala stood back and still staring at Kmazatron she put her hands down the neck of her beautiful garment. Carefully she unlocked the clasp of a beautiful necklace, she had a beautiful bejewelled locket.
When she opened the locket there was a portrait inside, it was of her Kmazatron and their two sons Kmarazroturc and Boren.
Keiranala put the open locket down and pushed it across the desk, Kmazatron although still in a foul mood looked down, as he gased down at the locket he slumped back into his chair, chucking the glasses off his face Kmazatron ran his claws across his face and pinched either side of the brow of his snout.
"They were so young when we had this painted" said Keiranala as she gazed lovingly at the picture particularly at her sons.
Sighing heavily Kmazatron sat up and took hold of his glasses, putting them on he picked up the locket and smiled.
His robe held tight to his body, the cuffs just hiding the giant plated scales running up his arms.
"I know they were...my darling I'm sorry" said Kmazatron.