CN114213979A - Electronic material glue solution and preparation method thereof - Google Patents
Electronic material glue solution and preparation method thereof Download PDFInfo
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- CN114213979A CN114213979A CN202111326497.2A CN202111326497A CN114213979A CN 114213979 A CN114213979 A CN 114213979A CN 202111326497 A CN202111326497 A CN 202111326497A CN 114213979 A CN114213979 A CN 114213979A
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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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- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to the technical field of electronic glue, in particular to electronic material glue and a preparation method thereof; comprises a component A and a curing agent according to the ratio of 100: (8-10), wherein the component A is prepared from the following raw materials in parts by weight: 80-90 parts of improved high-thermal-conductivity 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 dispersant and 1-2 parts of toughening agent. The electronic material glue solution prepared by the invention has moderate curing temperature and convenient operation, has the advantages of high heat-conducting property, high dielectric property, low viscosity and high filling amount after the epoxy glue solution is cured, has simple preparation process, has stronger protective capability when being applied to electronic packaging, accordingly prolongs the service life of electronic and electric appliances and has good practicability.
Description
Technical Field
The invention relates to the technical field of electronic glue, in particular to electronic material glue and a preparation method thereof.
Background
The heat-conducting adhesive is mainly used for bonding and packaging electronic and electrical components in electrical insulation occasions. With the development of integrated circuits and assembly techniques in the electronic industry, the volume of electronic components and logic circuits tends to be miniaturized, and the development of the electronic components and logic circuits towards multi-functionalization and integration tends to cause a great increase in heat generation, which puts high demands on the thermal conductivity of bonding and packaging materials, and thus, the improvement of thermal conductivity is an increasingly urgent issue.
There are two ways to improve the thermal conductivity of polymers: 1. synthesizing structural polymers with high heat conductivity coefficient, such as polyacetylene, polyaniline, polypyrrole and the like with good heat conductivity, and mainly realizing heat conduction through an electronic heat conduction mechanism, or polymers with complete crystallinity and realizing heat conduction through phonons; 2. and filling the polymer by adding a high-thermal-conductivity inorganic substance to prepare the polymer/inorganic substance thermal-conductivity composite material. Because organic polymers with good heat-conducting property are expensive, the method for filling heat-conducting inorganic fillers is widely adopted at present, and the adopted inorganic heat-conducting fillers mainly comprise aluminum oxide, boron nitride, aluminum nitride and the like.
Boron Nitride (BN) has extremely high thermal conductivity and breakdown strength, but because the BN density is small (2.25g/cm3), when the BN dosage exceeds 30 percent of the resin system, the viscosity of the resin is increased, the distribution is uneven, the glue mixing is very difficult, and the preparation process is complicated and the cost is too high.
Aluminum nitride (ALN) is used as a novel filler, the mass production is started in recent years in China, the product quality and stability need to be investigated, the price is high, and the cost is overhigh by using the ALN alone.
Non-spherical Alumina (AL)2O3) Good electric insulation performance, mature manufacturing process, low price and most common application. But the thermal conductivity is too low and high fill is required to increase the thermal conductivity. However, high filling can cause negative effects, such as severe increase in glue viscosity and reduced flowability, thereby affecting processability; in addition, the mechanical properties can also be influenced.
Therefore, the type, shape and usage amount of the inorganic filler are the key points for preparing the high-thermal-conductivity electronic pouring sealant. Therefore, by changing the types of the inorganic fillers, the invention designs the glue solution with high heat resistance, high heat conductivity, high dielectric property, low viscosity, high filling amount and simple preparation process, which is 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, and aims to solve the problems in the prior art.
In order to achieve the purpose, the technical scheme of the invention is as follows:
an electronic material glue solution is prepared from a component A and a curing agent according to the weight ratio of 100: (8-10), wherein the component A is prepared from the following raw materials in parts by weight: 80-90 parts of improved high-thermal-conductivity 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 dispersant and 1-2 parts of toughening agent.
Specifically, the curing agent is 650 low molecular weight polyamide resin.
Specifically, the preparation method of the improved high-thermal-conductivity component comprises the following steps:
s1: grinding non-spherical alumina in a ball mill to obtain fine alumina powder for later use;
s2: adding absolute ethyl alcohol: fine alumina powder: silicone resin: the weight ratio of welan gum to 30: 6: 1: 1, uniformly dispersing in a stirrer to prepare spray liquid;
s3: and (3) carrying out spray granulation on the spray liquid, and then carrying out drying, cooling, granule finishing and screening 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 μm.
Specifically, the spray liquid is filtered through 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 temperature of the spray granulation material is kept at 60-65 ℃.
Specifically, the drying temperature is 70-75 ℃, the drying time is 5-8 min, the temperature is cooled to be less than or equal to 30 ℃, then the false agglomerates are scattered through straightening, and the screening is carried out for later use.
Furthermore, the improved high-thermal-conductivity component is prepared from absolute ethyl alcohol, fine-particle alumina powder, silicon 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 microns, and on one hand, the non-spherical alumina with a smaller particle size is convenient for the whole particle size of the prepared improved high-thermal-conductivity component to be smaller in the subsequent granulation process, is convenient for subsequent dispersion in an electronic material glue solution, and has the advantage of high filling amount; on the other hand, the prepared improved high-heat-conductivity component is spherical in structure, and the whole structure is regular and 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-grained alumina powder is modified by using the silicone resin and the welan gum in a specific ratio, wherein the silicon resin is composed of a space network structure taking Si-O-Si as a main chain, has excellent high and low temperature resistance, atmospheric aging resistance, electrical insulation and elasticity, the high-thermal-conductivity electronic material glue solution is a cross-linking type semi-inorganic high-molecular polymer with organic groups connected to silicon atoms, is used as a template in an improved high-thermal-conductivity component system, fine-particle alumina powder is attached to a silicon resin net structure by utilizing Wenley glue, the thermal conductivity of the high-thermal-conductivity component in the electronic material glue solution is effectively adjusted and improved, the electronic material glue solution is guaranteed to have high thermal conductivity and high filling amount in the early stage of use, the fine-particle alumina powder can be slowly released in the later stage of use 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 a titanate coupling agent, the viscosity modifier is 1, 4-butanediol diglycidyl ether, the catalyst is dibutyltin 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 both the E-51 epoxy resin and the 650 low molecular weight polyamide resin are low-viscosity material components and are matched with the viscosity modifier for synergistic use, so that the viscosity of the whole system of the electronic material glue solution can be further improved.
Furthermore, the invention adopts titanate coupling agent, the inorganic functional group of which is a monofunctional group, namely Ti-OR' 2, the inorganic functional group and E-51 epoxy resin are subjected to bonding reaction under the action of 650 low molecular weight polyamide resin, the titanate coupling agent plays a role of an intermediate layer, and the titanate coupling agent contains a long soft bond segment to form a flexible interface layer which is beneficial to stress relaxation, so as to absorb and disperse impact energy, obtain the adhesive solution with good impact strength and toughness, and enable the electronic material adhesive solution to have better performances of medium resistance, water resistance and aging resistance.
Furthermore, the organic silicon oil is used as a 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 the 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.
A preparation method of electronic material glue solution comprises the following steps:
step 1: preparing an improved high thermal conductivity component;
step 2: placing the improved high-thermal-conductivity component, the coupling agent, the viscosity modifier, the dispersant and the toughening agent in corresponding parts by weight in a stirrer in sequence for dispersing, and fully stirring and mixing to obtain a mixture A;
and step 3: adding epoxy resin in corresponding weight parts into the obtained mixture A, and uniformly stirring to obtain a mixture B;
and 4, step 4: and (3) placing the mixture B, the catalyst and the curing agent in corresponding parts by weight in a stirrer for dispersing, fully stirring and mixing, and curing for 30-40 h at 25 ℃ or 5h at 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 invention has the beneficial effects that: the electronic material glue solution prepared by the invention has moderate curing temperature and convenient operation, has the advantages of high heat-conducting property, high dielectric property, low viscosity and high filling amount after the epoxy glue solution is cured, has simple preparation process, has stronger protective capability when being applied to electronic packaging, accordingly prolongs the service life of electronic and electric appliances and has good practicability.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
An electronic material glue solution is prepared from a component A and a curing agent according to the weight ratio of 100: 8, the component A is prepared by mixing the following raw materials in percentage by weight: 80 parts of improved high-thermal-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 dispersant 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-thermal-conductivity component comprises the following steps:
s1: grinding non-spherical alumina in a ball mill to obtain fine alumina powder for later use;
s2: adding absolute ethyl alcohol: fine alumina powder: silicone resin: the weight ratio of welan gum to 30: 6: 1: 1, uniformly dispersing in a stirrer to prepare spray liquid;
s3: and (3) carrying out spray granulation on the spray liquid, and then carrying out drying, cooling, granule finishing and screening 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 μm.
Specifically, the spray liquid is filtered through 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 temperature of the spray granulation material is kept at 60-65 ℃.
Specifically, the drying temperature is 70-75 ℃, the drying time is 5-8 min, the temperature is cooled to be less than or equal to 30 ℃, then the false agglomerates are scattered through straightening, and the screening is carried out for later use.
Specifically, the epoxy resin is E-51 epoxy resin, the coupling agent is a titanate coupling agent, the viscosity modifier is 1, 4-butanediol diglycidyl ether, the catalyst is dibutyltin dilaurate, the dispersing agent is organic silicone oil, and the toughening agent is dibutyl phthalate.
A preparation method of electronic material glue solution comprises the following steps:
step 1: preparing an improved high thermal conductivity component;
step 2: placing the improved high-thermal-conductivity component, the coupling agent, the viscosity modifier, the dispersant and the toughening agent in corresponding parts by weight in a stirrer in sequence for dispersing, and fully stirring and mixing to obtain a mixture A;
and step 3: adding epoxy resin in corresponding weight parts into the obtained mixture A, and uniformly stirring to obtain a mixture B;
and 4, step 4: and (3) placing the mixture B, the catalyst and the curing agent in corresponding parts by weight in a stirrer for dispersing, fully stirring and mixing, and curing for 30-40 h at 25 ℃ or 5h at 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 a component A and a curing agent according to the weight ratio of 100: 10, the component A is prepared from the following raw materials in parts by weight: 90 parts of improved high-thermal-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 dispersant 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-thermal-conductivity component comprises the following steps:
s1: grinding non-spherical alumina in a ball mill to obtain fine alumina powder for later use;
s2: adding absolute ethyl alcohol: fine alumina powder: silicone resin: the weight ratio of welan gum to 30: 6: 1: 1, uniformly dispersing in a stirrer to prepare spray liquid;
s3: and (3) carrying out spray granulation on the spray liquid, and then carrying out drying, cooling, granule finishing and screening 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 μm.
Specifically, the spray liquid is filtered through 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 temperature of the spray granulation material is kept at 60-65 ℃.
Specifically, the drying temperature is 70-75 ℃, the drying time is 5-8 min, the temperature is cooled to be less than or equal to 30 ℃, then the false agglomerates are scattered through straightening, and the screening is carried out for later use.
Specifically, the epoxy resin is E-51 epoxy resin, the coupling agent is a titanate coupling agent, the viscosity modifier is 1, 4-butanediol diglycidyl ether, the catalyst is dibutyltin dilaurate, the dispersing agent is organic silicone oil, and the toughening agent is dibutyl phthalate.
A preparation method of electronic material glue solution comprises the following steps:
step 1: preparing an improved high thermal conductivity component;
step 2: placing the improved high-thermal-conductivity component, the coupling agent, the viscosity modifier, the dispersant and the toughening agent in corresponding parts by weight in a stirrer in sequence for dispersing, and fully stirring and mixing to obtain a mixture A;
and step 3: adding epoxy resin in corresponding weight parts into the obtained mixture A, and uniformly stirring to obtain a mixture B;
and 4, step 4: and (3) placing the mixture B, the catalyst and the curing agent in corresponding parts by weight in a stirrer for dispersing, fully stirring and mixing, and curing for 30-40 h at 25 ℃ or 5h at 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 a component A and a curing agent according to the weight ratio of 100: 8.5, the component A is prepared by mixing the following raw materials in percentage by weight: 85 parts of improved high-thermal-conductivity 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 dispersant 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-thermal-conductivity component comprises the following steps:
s1: grinding non-spherical alumina in a ball mill to obtain fine alumina powder for later use;
s2: adding absolute ethyl alcohol: fine alumina powder: silicone resin: the weight ratio of welan gum to 30: 6: 1: 1, uniformly dispersing in a stirrer to prepare spray liquid;
s3: and (3) carrying out spray granulation on the spray liquid, and then carrying out drying, cooling, granule finishing and screening 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 μm.
Specifically, the spray liquid is filtered through 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 temperature of the spray granulation material is kept at 60-65 ℃.
Specifically, the drying temperature is 70-75 ℃, the drying time is 5-8 min, the temperature is cooled to be less than or equal to 30 ℃, then the false agglomerates are scattered through straightening, and the screening is carried out for later use.
Specifically, the epoxy resin is E-51 epoxy resin, the coupling agent is a titanate coupling agent, the viscosity modifier is 1, 4-butanediol diglycidyl ether, the catalyst is dibutyltin dilaurate, the dispersing agent is organic silicone oil, and the toughening agent is dibutyl phthalate.
A preparation method of electronic material glue solution comprises the following steps:
step 1: preparing an improved high thermal conductivity component;
step 2: placing the improved high-thermal-conductivity component, the coupling agent, the viscosity modifier, the dispersant and the toughening agent in corresponding parts by weight in a stirrer in sequence for dispersing, and fully stirring and mixing to obtain a mixture A;
and step 3: adding epoxy resin in corresponding weight parts into the obtained mixture A, and uniformly stirring to obtain a mixture B;
and 4, step 4: and (3) placing the mixture B, the catalyst and the curing agent in corresponding parts by weight in a stirrer for dispersing, fully stirring and mixing, and curing for 30-40 h at 25 ℃ or 5h at 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 a component A and a curing agent according to the weight ratio of 100: 9, the component A is prepared by mixing the following raw materials in percentage by weight: 88 parts of improved high-thermal-conductivity 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 dispersant 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-thermal-conductivity component comprises the following steps:
s1: grinding non-spherical alumina in a ball mill to obtain fine alumina powder for later use;
s2: adding absolute ethyl alcohol: fine alumina powder: silicone resin: the weight ratio of welan gum to 30: 6: 1: 1, uniformly dispersing in a stirrer to prepare spray liquid;
s3: and (3) carrying out spray granulation on the spray liquid, and then carrying out drying, cooling, granule finishing and screening 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 μm.
Specifically, the spray liquid is filtered through 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 temperature of the spray granulation material is kept at 60-65 ℃.
Specifically, the drying temperature is 70-75 ℃, the drying time is 5-8 min, the temperature is cooled to be less than or equal to 30 ℃, then the false agglomerates are scattered through straightening, and the screening is carried out for later use.
Specifically, the epoxy resin is E-51 epoxy resin, the coupling agent is a titanate coupling agent, the viscosity modifier is 1, 4-butanediol diglycidyl ether, the catalyst is dibutyltin dilaurate, the dispersing agent is organic silicone oil, and the toughening agent is dibutyl phthalate.
A preparation method of electronic material glue solution comprises the following steps:
step 1: preparing an improved high thermal conductivity component;
step 2: placing the improved high-thermal-conductivity component, the coupling agent, the viscosity modifier, the dispersant and the toughening agent in corresponding parts by weight in a stirrer in sequence for dispersing, and fully stirring and mixing to obtain a mixture A;
and step 3: adding epoxy resin in corresponding weight parts into the obtained mixture A, and uniformly stirring to obtain a mixture B;
and 4, step 4: and (3) placing the mixture B, the catalyst and the curing agent in corresponding parts by weight in a stirrer for dispersing, fully stirring and mixing, and curing for 30-40 h at 25 ℃ or 5h at 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, the component ratios and the preparation methods of the component a of the electronic material glue solution are the same as those in example 1, except that the electronic material glue solution of the comparative example is prepared from the component a and the curing agent according to a ratio of 100: 7 by weight ratio.
Comparative example 2
In the comparative example, the raw materials, the component ratios and the preparation methods of the component a of the electronic material glue solution are the same as those in example 1, except that the electronic material glue solution of the comparative example is prepared from the component a and the curing agent according to a ratio of 100: 11 by weight ratio.
Comparative example 3
In the comparative example, the raw materials, the component ratios and the preparation method of the electronic material glue solution are the same as those in example 1, except that the improved high thermal conductive component in the comparative example is directly prepared from non-spherical alumina.
Comparative example 4
In the comparative example, the raw materials, the component ratios and the preparation method of the electronic material glue solution are the same as those in example 1, except that the improved high-thermal-conductivity component in the comparative example is 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 glue solution is the same as that of example 1, except that the electronic material glue solution of this comparative example, 100: 8, the component A is prepared by mixing the following raw materials in percentage by weight: 75 parts of improved high-thermal-conductivity 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 dispersant and 0.8 part of toughening agent.
Comparative example 6
In this comparative example, the preparation method of the electronic material glue solution is the same as that of example 1, except that the electronic material glue solution of this comparative example, 100: 8, the component A is prepared by mixing the following raw materials in percentage by weight: 100 parts of improved high-thermal-conductivity component, 16 parts of epoxy resin, 4 parts of coupling agent, 4 parts of viscosity modifier, 0.13 part of catalyst, 2 parts of dispersant and 2.6 parts of toughening agent.
Performance testing
The samples prepared in examples 1-4 and the samples prepared in comparative examples 1-6 were measured for mechanical property, dielectric property, thermal property and adhesive property according to GB/T2794-1995, ASTM E1530 and IPC standard methods, and the test results are shown in Table 1.
TABLE 1 Property parameters of electronic Material glues
In conclusion, the glue solution for the electronic material disclosed by the invention is reasonable in composition and good in compatibility among components, so that the glue solution for the electronic material prepared by the method has the advantages of high heat-conducting property, high dielectric property, low viscosity and high filling amount, and meets the development and application requirements of the electronic material.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, 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 or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (10)
1. An electronic material glue solution is characterized by comprising a component A and a curing agent according to a ratio of 100: (8-10), wherein the component A is prepared from the following raw materials in parts by weight: 80-90 parts of improved high-thermal-conductivity 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 dispersant and 1-2 parts of toughening agent.
2. The electronic material glue solution of claim 1, wherein the curing agent is 650 low molecular weight polyamide resin.
3. The electronic material glue solution according to claim 1, wherein the preparation method of the improved high thermal conductive component comprises the following steps:
s1: grinding non-spherical alumina in a ball mill to obtain fine alumina powder for later use;
s2: adding absolute ethyl alcohol: fine alumina powder: silicone resin: the weight ratio of welan gum to 30: 6: 1: 1, uniformly dispersing in a stirrer to prepare spray liquid;
s3: and (3) carrying out spray granulation on the spray liquid, and then carrying out drying, cooling, granule finishing and screening to obtain the improved high-heat-conductivity component.
4. The electronic material glue solution of claim 3, wherein the median diameter of the fine alumina powder is less than or equal to 10 μm.
5. The electronic material glue solution according to claim 3, wherein the spray solution is filtered through 1250-mesh sieve and then subjected to spray granulation of S3.
6. The electronic material glue solution according to claim 3, wherein the speed of spray granulation is 1500 ml-1600 ml/min, and the temperature of the spray granulation material is kept at 60-65 ℃.
7. The electronic material glue solution according to claim 3, wherein 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 ℃, the false agglomerates are broken up through straightening, and the screen is screened for later use.
8. 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-based coupling agent, the viscosity modifier is 1, 4-butanediol diglycidyl ether, the catalyst is dibutyltin dilaurate, the dispersant is silicone oil, and the toughening agent is dibutyl phthalate.
9. The preparation method of the electronic material glue solution according to any one of claims 1 to 8, characterized by comprising the following steps:
step 1: preparing an improved high thermal conductivity component;
step 2: placing the improved high-thermal-conductivity component, the coupling agent, the viscosity modifier, the dispersant and the toughening agent in corresponding parts by weight in a stirrer in sequence for dispersing, and fully stirring and mixing to obtain a mixture A;
and step 3: adding epoxy resin in corresponding weight parts into the obtained mixture A, and uniformly stirring to obtain a mixture B;
and 4, step 4: and (3) placing the mixture B, the catalyst and the curing agent in corresponding parts by weight in a stirrer for dispersing, fully stirring and mixing, and curing for 30-40 h at 25 ℃ or 5h at 70 ℃.
10. The preparation method of the electronic material glue solution according to claim 9, 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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