CN114213979B - Electronic material glue solution and preparation method thereof - Google Patents
Electronic material glue solution and preparation method thereof Download PDFInfo
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- CN114213979B CN114213979B CN202111326497.2A CN202111326497A CN114213979B CN 114213979 B CN114213979 B CN 114213979B CN 202111326497 A CN202111326497 A CN 202111326497A CN 114213979 B CN114213979 B CN 114213979B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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- Inorganic Chemistry (AREA)
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- Adhesives Or Adhesive Processes (AREA)
- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
Abstract
The invention relates to the technical field of electronic glue, in particular to an electronic material glue solution and a preparation method thereof; the component A and the curing agent are mixed according to the weight ratio of 100: the component A is formed by mixing the following raw materials in parts by weight: 80 to 90 parts of improved high heat conduction component, 10 to 15 parts of epoxy resin, 1 to 3 parts of coupling agent, 2 to 3 parts of viscosity modifier, 0.05 to 0.1 part of catalyst, 1 to 1.5 parts of dispersing agent and 1 to 2 parts of toughening agent. The electronic material glue solution prepared by the invention has moderate curing temperature and convenient operation, and after the epoxy glue is cured, the epoxy glue solution has the advantages of high heat conduction performance, high dielectric property, low viscosity and high filling quantity, and the preparation process is simple, so that the epoxy glue solution has stronger protective capability when being applied to electronic packaging, thereby correspondingly prolonging the service life of electronic appliances and having good practicability.
Description
Technical Field
The invention relates to the technical field of electronic glue, in particular to an electronic material glue solution and a preparation method thereof.
Background
The heat-conducting adhesive is used for bonding and packaging in the electric insulation occasion of electronic and electric devices. With the development of integrated circuits and assembly technologies in the electronic industry, the volumes of electronic components and logic circuits tend to be miniaturized, and the development of the electronic components and logic circuits is towards multifunction and integration, so that the heat productivity tends to be greatly increased, and high requirements are put on the heat conducting performance of bonding and packaging materials, so that the improvement of the heat conductivity is an increasingly urgent problem.
There are two approaches to improving the thermal conductivity of polymers: 1. synthesizing a structural polymer with high heat conductivity coefficient, such as polyacetylene, polyaniline, polypyrrole and the like with good heat conductivity, wherein heat conduction is realized mainly through an electronic heat conduction mechanism, or the structural polymer has complete crystallinity, and heat conduction is realized through phonons; 2. and filling the polymer by adding the high-heat-conductivity inorganic matters to prepare the polymer/inorganic matter heat-conductivity composite material. Because of the high price of the organic polymer with good heat conducting property, the filling of the heat conducting inorganic filler is a widely adopted method at present, and more inorganic heat conducting fillers mainly comprise alumina, boron nitride, aluminum nitride and the like.
Boron Nitride (BN) has extremely high thermal conductivity and extremely high breakdown strength, but because the BN density is small (2.25 g/cm 3), when the BN amount exceeds 30% of the resin system, the viscosity of the resin is increased, the distribution is uneven, the mixing of the resin is extremely difficult, and the preparation process is complicated and the cost is too high.
Aluminum nitride (ALN) is taken as a novel filler, mass production is started only in recent years, product quality and stability need to be inspected, the price is high, and the cost is excessively high when the aluminum nitride (ALN) is singly used.
Non-spherical Alumina (AL) 2 O 3 ) Good electrical insulation performance, mature manufacturing process, low price and most common application. But its thermal conductivity is too low and high packing is required to improve the thermal conductivity. However, high loadings can cause negative effects such as increased viscosity of the gum solution, decreased flowability, and thus processability; in addition, the mechanical properties are also affected.
Therefore, the type, shape and usage amount of the inorganic filler are key points for preparing the high-heat-conductivity electronic pouring sealant. Therefore, by changing the types of inorganic fillers, the invention designs the glue solution with high heat resistance, high heat conductivity, high dielectric property, low viscosity and high filling quantity and simple preparation process, which becomes a necessary trend.
Therefore, an electronic material glue solution and a preparation method thereof are provided.
Disclosure of Invention
The invention aims to provide an electronic material glue solution and a preparation method thereof, which are used for solving the problems in the prior art.
In order to achieve the above object, the technical scheme of the present invention is as follows:
an electronic material glue solution is prepared from component A and a curing agent according to the proportion of 100: the component A is formed by mixing the following raw materials in parts by weight: 80 to 90 parts of improved high heat conduction component, 10 to 15 parts of epoxy resin, 1 to 3 parts of coupling agent, 2 to 3 parts of viscosity modifier, 0.05 to 0.1 part of catalyst, 1 to 1.5 parts of dispersing agent and 1 to 2 parts of toughening agent.
Specifically, the curing agent is 650 low molecular weight polyamide resin.
Specifically, the preparation method of the improved high-heat-conductivity component comprises the following steps:
s1: grinding the non-spherical alumina in a ball mill to obtain fine-particle alumina powder for later use;
s2: absolute ethanol: fine-grained alumina powder: silicone resin: the welan gum is prepared from the following components: 6:1:1 are placed in a stirrer to be uniformly dispersed to prepare spray liquid;
s3: and (3) carrying out spray granulation on the spray liquid, and then drying, cooling, granulating and sieving to obtain the improved high-heat-conductivity component.
Specifically, the median diameter of the fine-particle alumina powder is less than or equal to 10 mu m.
Specifically, the spray liquid is filtered by a 1250-mesh sieve and then is subjected to spray granulation of S3.
Specifically, the speed of spray granulation is 1500 ml-1600 ml/min, and the material temperature of spray granulation is kept at 60-65 ℃.
Specifically, the drying temperature is 70-75 ℃, the drying time is 5-8 min, the material temperature is cooled to be less than or equal to 30 ℃, then the pseudo-caking is broken up through the whole grain, and the powder is screened for later use.
Furthermore, the improved high heat conduction component is prepared from absolute ethyl alcohol, fine-particle alumina powder, silicone resin and welan gum in a specific proportion, wherein the fine-particle alumina powder is firstly subjected to ball milling, so that the median diameter of the non-spherical alumina is less than or equal to 10 mu m, on the one hand, the non-spherical alumina with smaller particle diameter is convenient for the whole particle diameter of the prepared improved high heat conduction component to be smaller in the subsequent granulating process, is convenient for the subsequent dispersion in the electronic material glue solution, and has the advantage of high filling quantity; on the other hand, the prepared improved high-heat-conductivity component has a spherical structure, and the whole structure is regular, so that the improved high-heat-conductivity component has good dispersibility and fluidity in the electronic material glue solution, and the electronic material glue solution is endowed with high heat-conductivity; in addition, the fine-particle alumina powder is modified by using the silicone resin and the welan gum in a specific proportion, wherein the silicone resin is composed of a space network structure with Si-O-Si as a main chain, has excellent high and low temperature resistance, atmospheric aging resistance, electrical insulation and elasticity, is a cross-linked semi-inorganic high polymer with an organic group connected to a silicon atom, is used as a template in an improved high heat conduction component system, and the welan gum is used for attaching the fine-particle alumina powder to the silicone resin network structure, so that the heat conduction performance of the improved high heat conduction component in the electronic material glue solution is effectively regulated, the electronic material glue solution can be ensured to have high heat conduction and high filling quantity, the fine-particle alumina powder can be slowly released in the later use period of the electronic material glue solution, and the durability of the electronic material glue solution is obviously improved.
Specifically, the epoxy resin is E-51 epoxy resin, the coupling agent is titanate coupling agent, the viscosity modifier is 1, 4-butanediol diglycidyl ether, the catalyst is dibutyl tin dilaurate, the dispersing agent is organic silicone oil, and the toughening agent is dibutyl phthalate.
Furthermore, the E-51 epoxy resin and the 650 low molecular weight polyamide resin are adopted for toughness curing, and the viscosity of the whole system of the electronic material glue solution can be further improved due to the fact that the E-51 epoxy resin and the 650 low molecular weight polyamide resin are both low-viscosity material components and are matched with the viscosity modifier for synergistic use.
Furthermore, the invention adopts the titanate coupling agent, the inorganic functional group of the titanate coupling agent is a single functional group, namely Ti-OR'2, the inorganic functional group and the E-51 epoxy resin are subjected to bonding reaction under the action of 650 low molecular weight polyamide resin, the titanate coupling agent plays the role of an intermediate layer, and the titanate coupling agent contains a long soft bond section to form a flexible interface layer which is favorable for stress relaxation, absorbs and disperses impact energy, and has good impact strength and toughness, so that the electronic material glue solution has better medium resistance, water resistance and aging resistance.
Furthermore, the invention adopts the organic silicone oil as the dispersing agent, so that on one hand, in the component A, the wettability among the components can be promoted, and the dispersibility of the system is further improved; on the other hand, in a system of the electronic material glue solution, the dispersibility of the electronic material glue solution can be promoted, and the electronic material glue solution is not easy to settle.
The preparation method of the electronic material glue solution comprises the following steps:
step 1: preparing an improved high thermal conductivity component;
step 2: sequentially placing the improved high-heat-conductivity component, the coupling agent, the viscosity modifier, the dispersing agent and the toughening agent in a stirrer for dispersing, and fully stirring and mixing to obtain a mixture A;
step 3: adding epoxy resin with corresponding weight parts into the obtained mixture A, and uniformly stirring to obtain a mixture B;
step 4: and (3) dispersing the mixture B, the catalyst and the curing agent in the corresponding parts by weight in a stirrer, fully stirring and mixing, and curing for 30-40 h at the room temperature of 25 ℃ or 5h at the temperature of 70 ℃.
Specifically, the rotating speed in the step 2 is 2000-2300 r/min, and the stirring time is 10-20 min; the rotating speed in the step 3 is 2500-2700 r/min, the stirring time is 20-30 min, the rotating speed in the step 4 is 1200-1500 r/min, and the stirring time is 30-40 min.
The beneficial effects of the invention are as follows: the electronic material glue solution prepared by the invention has moderate curing temperature and convenient operation, and after the epoxy glue is cured, the epoxy glue solution has the advantages of high heat conduction performance, high dielectric property, low viscosity and high filling quantity, and the preparation process is simple, so that the epoxy glue solution has stronger protective capability when being applied to electronic packaging, thereby correspondingly prolonging the service life of electronic appliances and having good practicability.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
An electronic material glue solution is prepared from component A and a curing agent according to the proportion of 100:8, wherein the component A is prepared by mixing the following raw materials in parts by weight: 80 parts of improved high-heat-conductivity component, 10 parts of epoxy resin, 1 part of coupling agent, 2 parts of viscosity modifier, 0.05 part of catalyst, 1 part of dispersing agent and 1 part of toughening agent.
Specifically, the curing agent is 650 low molecular weight polyamide resin.
Specifically, the preparation method of the improved high-heat-conductivity component comprises the following steps:
s1: grinding the non-spherical alumina in a ball mill to obtain fine-particle alumina powder for later use;
s2: absolute ethanol: fine-grained alumina powder: silicone resin: the welan gum is prepared from the following components: 6:1:1 are placed in a stirrer to be uniformly dispersed to prepare spray liquid;
s3: and (3) carrying out spray granulation on the spray liquid, and then drying, cooling, granulating and sieving to obtain the improved high-heat-conductivity component.
Specifically, the median diameter of the fine-particle alumina powder is less than or equal to 10 mu m.
Specifically, the spray liquid is filtered by a 1250-mesh sieve and then is subjected to spray granulation of S3.
Specifically, the speed of spray granulation is 1500 ml-1600 ml/min, and the material temperature of spray granulation is kept at 60-65 ℃.
Specifically, the drying temperature is 70-75 ℃, the drying time is 5-8 min, the material temperature is cooled to be less than or equal to 30 ℃, then the pseudo-caking is broken up through the whole grain, and the powder is screened for later use.
Specifically, the epoxy resin is E-51 epoxy resin, the coupling agent is titanate coupling agent, the viscosity modifier is 1, 4-butanediol diglycidyl ether, the catalyst is dibutyl tin dilaurate, the dispersing agent is organic silicone oil, and the toughening agent is dibutyl phthalate.
The preparation method of the electronic material glue solution comprises the following steps:
step 1: preparing an improved high thermal conductivity component;
step 2: sequentially placing the improved high-heat-conductivity component, the coupling agent, the viscosity modifier, the dispersing agent and the toughening agent in a stirrer for dispersing, and fully stirring and mixing to obtain a mixture A;
step 3: adding epoxy resin with corresponding weight parts into the obtained mixture A, and uniformly stirring to obtain a mixture B;
step 4: and (3) dispersing the mixture B, the catalyst and the curing agent in the corresponding parts by weight in a stirrer, fully stirring and mixing, and curing for 30-40 h at the room temperature of 25 ℃ or 5h at the temperature of 70 ℃.
Specifically, the rotating speed in the step 2 is 2000-2300 r/min, and the stirring time is 10-20 min; the rotating speed in the step 3 is 2500-2700 r/min, the stirring time is 20-30 min, the rotating speed in the step 4 is 1200-1500 r/min, and the stirring time is 30-40 min.
Example 2
An electronic material glue solution is prepared from component A and a curing agent according to the proportion of 100:10, wherein the component A consists of the following raw materials in percentage by weight: 90 parts of improved high-heat-conductivity component, 15 parts of epoxy resin, 3 parts of coupling agent, 3 parts of viscosity modifier, 0.1 part of catalyst, 1.5 parts of dispersing agent and 2 parts of toughening agent.
Specifically, the curing agent is 650 low molecular weight polyamide resin.
Specifically, the preparation method of the improved high-heat-conductivity component comprises the following steps:
s1: grinding the non-spherical alumina in a ball mill to obtain fine-particle alumina powder for later use;
s2: absolute ethanol: fine-grained alumina powder: silicone resin: the welan gum is prepared from the following components: 6:1:1 are placed in a stirrer to be uniformly dispersed to prepare spray liquid;
s3: and (3) carrying out spray granulation on the spray liquid, and then drying, cooling, granulating and sieving to obtain the improved high-heat-conductivity component.
Specifically, the median diameter of the fine-particle alumina powder is less than or equal to 10 mu m.
Specifically, the spray liquid is filtered by a 1250-mesh sieve and then is subjected to spray granulation of S3.
Specifically, the speed of spray granulation is 1500 ml-1600 ml/min, and the material temperature of spray granulation is kept at 60-65 ℃.
Specifically, the drying temperature is 70-75 ℃, the drying time is 5-8 min, the material temperature is cooled to be less than or equal to 30 ℃, then the pseudo-caking is broken up through the whole grain, and the powder is screened for later use.
Specifically, the epoxy resin is E-51 epoxy resin, the coupling agent is titanate coupling agent, the viscosity modifier is 1, 4-butanediol diglycidyl ether, the catalyst is dibutyl tin dilaurate, the dispersing agent is organic silicone oil, and the toughening agent is dibutyl phthalate.
The preparation method of the electronic material glue solution comprises the following steps:
step 1: preparing an improved high thermal conductivity component;
step 2: sequentially placing the improved high-heat-conductivity component, the coupling agent, the viscosity modifier, the dispersing agent and the toughening agent in a stirrer for dispersing, and fully stirring and mixing to obtain a mixture A;
step 3: adding epoxy resin with corresponding weight parts into the obtained mixture A, and uniformly stirring to obtain a mixture B;
step 4: and (3) dispersing the mixture B, the catalyst and the curing agent in the corresponding parts by weight in a stirrer, fully stirring and mixing, and curing for 30-40 h at the room temperature of 25 ℃ or 5h at the temperature of 70 ℃.
Specifically, the rotating speed in the step 2 is 2000-2300 r/min, and the stirring time is 10-20 min; the rotating speed in the step 3 is 2500-2700 r/min, the stirring time is 20-30 min, the rotating speed in the step 4 is 1200-1500 r/min, and the stirring time is 30-40 min.
Example 3
An electronic material glue solution is prepared from component A and a curing agent according to the proportion of 100:8.5, wherein the component A consists of the following raw materials in percentage by weight: 85 parts of modified high heat conduction component, 12 parts of epoxy resin, 1.5 parts of coupling agent, 2.3 parts of viscosity modifier, 0.07 part of catalyst, 1.3 parts of dispersing agent and 1.3 parts of toughening agent.
Specifically, the curing agent is 650 low molecular weight polyamide resin.
Specifically, the preparation method of the improved high-heat-conductivity component comprises the following steps:
s1: grinding the non-spherical alumina in a ball mill to obtain fine-particle alumina powder for later use;
s2: absolute ethanol: fine-grained alumina powder: silicone resin: the welan gum is prepared from the following components: 6:1:1 are placed in a stirrer to be uniformly dispersed to prepare spray liquid;
s3: and (3) carrying out spray granulation on the spray liquid, and then drying, cooling, granulating and sieving to obtain the improved high-heat-conductivity component.
Specifically, the median diameter of the fine-particle alumina powder is less than or equal to 10 mu m.
Specifically, the spray liquid is filtered by a 1250-mesh sieve and then is subjected to spray granulation of S3.
Specifically, the speed of spray granulation is 1500 ml-1600 ml/min, and the material temperature of spray granulation is kept at 60-65 ℃.
Specifically, the drying temperature is 70-75 ℃, the drying time is 5-8 min, the material temperature is cooled to be less than or equal to 30 ℃, then the pseudo-caking is broken up through the whole grain, and the powder is screened for later use.
Specifically, the epoxy resin is E-51 epoxy resin, the coupling agent is titanate coupling agent, the viscosity modifier is 1, 4-butanediol diglycidyl ether, the catalyst is dibutyl tin dilaurate, the dispersing agent is organic silicone oil, and the toughening agent is dibutyl phthalate.
The preparation method of the electronic material glue solution comprises the following steps:
step 1: preparing an improved high thermal conductivity component;
step 2: sequentially placing the improved high-heat-conductivity component, the coupling agent, the viscosity modifier, the dispersing agent and the toughening agent in a stirrer for dispersing, and fully stirring and mixing to obtain a mixture A;
step 3: adding epoxy resin with corresponding weight parts into the obtained mixture A, and uniformly stirring to obtain a mixture B;
step 4: and (3) dispersing the mixture B, the catalyst and the curing agent in the corresponding parts by weight in a stirrer, fully stirring and mixing, and curing for 30-40 h at the room temperature of 25 ℃ or 5h at the temperature of 70 ℃.
Specifically, the rotating speed in the step 2 is 2000-2300 r/min, and the stirring time is 10-20 min; the rotating speed in the step 3 is 2500-2700 r/min, the stirring time is 20-30 min, the rotating speed in the step 4 is 1200-1500 r/min, and the stirring time is 30-40 min.
Example 4
An electronic material glue solution is prepared from component A and a curing agent according to the proportion of 100:9, wherein the component A is prepared by mixing the following raw materials in parts by weight: 88 parts of modified high heat conduction component, 14 parts of epoxy resin, 2.6 parts of coupling agent, 2.5 parts of viscosity modifier, 0.09 part of catalyst, 1.3 parts of dispersing agent and 1.9 parts of toughening agent.
Specifically, the curing agent is 650 low molecular weight polyamide resin.
Specifically, the preparation method of the improved high-heat-conductivity component comprises the following steps:
s1: grinding the non-spherical alumina in a ball mill to obtain fine-particle alumina powder for later use;
s2: absolute ethanol: fine-grained alumina powder: silicone resin: the welan gum is prepared from the following components: 6:1:1 are placed in a stirrer to be uniformly dispersed to prepare spray liquid;
s3: and (3) carrying out spray granulation on the spray liquid, and then drying, cooling, granulating and sieving to obtain the improved high-heat-conductivity component.
Specifically, the median diameter of the fine-particle alumina powder is less than or equal to 10 mu m.
Specifically, the spray liquid is filtered by a 1250-mesh sieve and then is subjected to spray granulation of S3.
Specifically, the speed of spray granulation is 1500 ml-1600 ml/min, and the material temperature of spray granulation is kept at 60-65 ℃.
Specifically, the drying temperature is 70-75 ℃, the drying time is 5-8 min, the material temperature is cooled to be less than or equal to 30 ℃, then the pseudo-caking is broken up through the whole grain, and the powder is screened for later use.
Specifically, the epoxy resin is E-51 epoxy resin, the coupling agent is titanate coupling agent, the viscosity modifier is 1, 4-butanediol diglycidyl ether, the catalyst is dibutyl tin dilaurate, the dispersing agent is organic silicone oil, and the toughening agent is dibutyl phthalate.
The preparation method of the electronic material glue solution comprises the following steps:
step 1: preparing an improved high thermal conductivity component;
step 2: sequentially placing the improved high-heat-conductivity component, the coupling agent, the viscosity modifier, the dispersing agent and the toughening agent in a stirrer for dispersing, and fully stirring and mixing to obtain a mixture A;
step 3: adding epoxy resin with corresponding weight parts into the obtained mixture A, and uniformly stirring to obtain a mixture B;
step 4: and (3) dispersing the mixture B, the catalyst and the curing agent in the corresponding parts by weight in a stirrer, fully stirring and mixing, and curing for 30-40 h at the room temperature of 25 ℃ or 5h at the temperature of 70 ℃.
Specifically, the rotating speed in the step 2 is 2000-2300 r/min, and the stirring time is 10-20 min; the rotating speed in the step 3 is 2500-2700 r/min, the stirring time is 20-30 min, the rotating speed in the step 4 is 1200-1500 r/min, and the stirring time is 30-40 min.
Comparative example 1
In the comparative example, the raw materials of the component A, the component proportion and the preparation method of the electronic material glue solution are the same as those of the example 1, except that the electronic material glue solution of the comparative example comprises the component A and a curing agent according to the proportion of 100:7 weight ratio.
Comparative example 2
In the comparative example, the raw materials of the component A, the component proportion and the preparation method of the electronic material glue solution are the same as those of the example 1, except that the electronic material glue solution of the comparative example comprises the component A and a curing agent according to the proportion of 100:11 weight ratio.
Comparative example 3
In this comparative example, the raw materials, the component proportions, and the preparation methods of the electronic material dope were the same as those of example 1, except that the modified high heat conductive component in this comparative example was directly prepared using non-spherical alumina.
Comparative example 4
In this comparative example, the raw materials, the component proportions and the preparation methods of the electronic material dope were the same as those of example 1, except that the modified high heat conductive component in this comparative example was prepared by grinding non-spherical alumina in a ball mill to obtain fine-particle alumina powder.
Comparative example 5
In this comparative example, the preparation method of the electronic material dope was the same as in example 1, except that the electronic material dope of this comparative example, 100:8, wherein the component A is prepared by mixing the following raw materials in parts by weight: 75 parts of modified high heat conduction component, 6 parts of epoxy resin, 0.5 part of coupling agent, 1 part of viscosity modifier, 0.04 part of catalyst, 0.9 part of dispersing agent and 0.8 part of toughening agent.
Comparative example 6
In this comparative example, the preparation method of the electronic material dope was the same as in example 1, except that the electronic material dope of this comparative example, 100:8, wherein the component A is prepared by mixing the following raw materials in parts by weight: 100 parts of modified high heat conduction component, 16 parts of epoxy resin, 4 parts of coupling agent, 4 parts of viscosity modifier, 0.13 part of catalyst, 2 parts of dispersing agent and 2.6 parts of toughening agent.
Performance testing
The mechanical properties, dielectric properties, thermal properties and adhesion properties of the samples prepared in examples 1 to 4 and the samples prepared in comparative examples 1 to 6 were measured according to GB/T2794-1995, ASTM E1530 and IPC standard methods, and the measurement results are shown in Table 1.
TABLE 1 Performance parameters of electronic Material glue
In conclusion, the glue solution for the electronic material disclosed by the invention has reasonable composition and good compatibility among all components, so that the glue solution for the electronic material is prepared, has the advantages of high heat conduction performance, high dielectric property, low viscosity and high filling quantity, and meets the development and application of the electronic material.
Finally, it is noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention.
Claims (9)
1. The electronic material glue solution is characterized by comprising a component A and a curing agent according to the weight ratio of 100: the component A is formed by mixing the following raw materials in parts by weight: 80-90 parts of improved high heat conduction component, 10-15 parts of epoxy resin, 1-3 parts of coupling agent, 2-3 parts of viscosity modifier, 0.05-0.1 part of catalyst, 1-1.5 parts of dispersing agent and 1-2 parts of toughening agent, wherein the preparation method of the improved high heat conduction component comprises the following steps:
s1: grinding the non-spherical alumina in a ball mill to obtain fine-particle alumina powder for later use;
s2: absolute ethanol: fine-grained alumina powder: silicone resin: the welan gum is prepared from the following components: 6:1:1 are placed in a stirrer to be uniformly dispersed to prepare spray liquid;
s3: and (3) carrying out spray granulation on the spray liquid, and then drying, cooling, granulating and sieving to obtain the improved high-heat-conductivity component.
2. The electronic material glue of claim 1, wherein the curing agent is 650 low molecular weight polyamide resin.
3. An electronic material glue solution according to claim 2, wherein the median diameter of the fine-grained alumina powder is less than or equal to 10 μm.
4. An electronic material glue according to claim 2, wherein the spray solution is filtered through a 1250 mesh sieve and then subjected to spray granulation of S3.
5. An electronic material glue solution according to claim 2, wherein the speed of spray granulation is 1500 ml-1600 ml/min, and the material temperature of spray granulation is kept at 60-65 ℃.
6. The electronic material glue solution according to claim 2, wherein the drying temperature is 70-75 ℃, the drying time is 5-8 min, the cooling temperature is less than or equal to 30 ℃, and the pseudo-caking is broken up by the granule finishing and is screened for later use.
7. The electronic material glue solution according to claim 1, wherein the epoxy resin is an E-51 epoxy resin, the coupling agent is a titanate coupling agent, the viscosity modifier is 1, 4-butanediol diglycidyl ether, the catalyst is dibutyl tin dilaurate, the dispersant is silicone oil, and the toughening agent is dibutyl phthalate.
8. The method for preparing an electronic material glue solution according to any one of claims 1 to 7, comprising the steps of:
step 1: preparing an improved high thermal conductivity component;
step 2: sequentially placing the improved high-heat-conductivity component, the coupling agent, the viscosity modifier, the dispersing agent and the toughening agent in a stirrer for dispersing, and fully stirring and mixing to obtain a mixture A;
step 3: adding epoxy resin with corresponding weight parts into the obtained mixture A, and uniformly stirring to obtain a mixture B;
step 4: and (3) dispersing the mixture B, the catalyst and the curing agent in the corresponding parts by weight in a stirrer, fully stirring and mixing, and curing for 30-40 h at the room temperature of 25 ℃ or 5h at the temperature of 70 ℃.
9. The method for preparing an electronic material glue solution according to claim 8, wherein the rotation speed in the step 2 is 2000-2300 r/min, and the stirring time is 10-20 min; the rotating speed in the step 3 is 2500-2700 r/min, the stirring time is 20-30 min, the rotating speed in the step 4 is 1200-1500 r/min, and the stirring time is 30-40 min.
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| CN202111326497.2A CN114213979B (en) | 2021-11-10 | 2021-11-10 | Electronic material glue solution and preparation method thereof |
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| CN202111326497.2A CN114213979B (en) | 2021-11-10 | 2021-11-10 | Electronic material glue solution and preparation method thereof |
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