CN111029309A - Preparation method of compact combined type composite material for electronic packaging - Google Patents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/28—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection
- H01L23/29—Encapsulations, e.g. encapsulating layers, coatings, e.g. for protection characterised by the material, e.g. carbon
- H01L23/298—Semiconductor material, e.g. amorphous silicon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
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Abstract
The invention relates to a preparation method of a compact combined type composite material for electronic packaging, belonging to the technical field of electronic packaging materials. In the technical scheme of the invention, through acid modification and alkali modification treatment on the surface of the diamond material, a plurality of discontinuous old-shaped lock holes are formed on the surface of the powder under the action of strong acid, the lock holes are favorable for adsorption of metal copper particles in the lock holes and effective combination of the surface of an interface sol material, and through effective modification on the surface of the material, the material has excellent combination strength and the compact combination performance of the composite material is improved.
Description
Technical Field
The invention relates to a preparation method of a compact combined type composite material for electronic packaging, belonging to the technical field of electronic packaging materials.
Background
The electronic packaging material is a sealing body of an integrated circuit, has mechanical support and environmental protection effects on a chip, and avoids pollution and corrosion of water vapor, impurities and various chemical atmospheres in the atmosphere, so that the integrated circuit chip can stably play a normal electrical function, and the packaging material plays a very important role in thermal performance and even reliability of electronic devices and circuits. The electrical packaging material industry is now an important branch of the semiconductor industry, and it has been widely related to various disciplines such as chemistry, electricity, thermodynamics, mechanics and process equipment.
As a reinforcement of the metal matrix composite, the SiC particles have the advantages of high modulus, high hardness, low thermal expansion, high thermal conductivity, wide sources, low cost and the like. The Al alloy has the advantages of low density, high thermal conductivity (170-220W/m.K), low price, easy hot working and the like. By combining the above factors and considering the characteristics of the electronic packaging material such as low Coefficient of Thermal Expansion (CTE) matched with the substrate, high thermal conductivity, high rigidity, low density, low cost and the like, after the electronic packaging material is compounded into the particle reinforced aluminum-based composite material, the material has the advantages of Al and SiC and almost represents all performance requirements of an ideal packaging material, so that the SiC/Al composite material becomes the most spotlighted and potentially widely applied composite material in the metal-based composite material for electronic packaging.
Graphene is the strongest material in the world (Young modulus 1.7TPa), has a theoretical specific surface area of 2630m2/g, and has good thermal conductivity (5000W/(m.k)) and high-speed electron mobility at room temperature (200000cm 2/(V.s)). Meanwhile, the unique structure of the high-power-density semiconductor laser enables the high-power-density semiconductor laser to have special properties such as a perfect quantum Hall effect, a unique quantum tunneling effect and a bipolar electric field effect. Due to the excellent performance of graphene, the specific surface area is extremely large and the production cost is low (relative to carbon nanotubes); the connection between each carbon atom of graphene is very flexible, and when an external mechanical force is applied, the surface of each carbon atom can be bent and deformed to adapt to the external force without rearranging the carbon atoms, so that the stability of the structure is maintained. Based on the excellent performances of graphene, if the graphene is added into metal aluminum or copper to prepare an electronic packaging material, the conductivity of the material is greatly improved; the density of the graphene is small, and the density of the obtained composite material is lower than that of a metal matrix; the thermal expansion coefficient is small; meanwhile, the problem of interface wetting in the electronic packaging composite material is solved, and the reduction of interface thermal resistance is facilitated; the processing is easy. Therefore, the graphene metal matrix composite material has a wide application prospect in the field of electronic packaging.
Chinese patent (CN201210165260.5) discloses a non-pressure soaking methodThe process for preparing the SiC/Al electronic packaging material comprises the steps of taking silicon carbide as a reinforcing phase and Al-Mg-Si alloy as a matrix phase, uniformly mixing silicon carbide particles, a binder, a plasticizer, a lubricant and a solvent, performing compression molding, preheating treatment and sintering, and then soaking in an Al-Mg-Si alloy melt. The electronic packaging material has a thermal conductivity of (140--6The electronic packaging material has poor cutting processing performance, the high melting point of the silicon carbide causes poor welding performance of the electronic packaging material, and the thermal expansion coefficient and the thermal conductivity of the electronic packaging material need to be further improved.
Chinese patent (201610418417.9) discloses a method for preparing a 3D-SiC/Al composite material with a three-dimensional interpenetrating structure, which comprises the steps of preparing a 3D-SiC prefabricated part and preparing the 3D-SiC/Al composite material through subsequent pressureless infiltration. Wherein, the 3D-SiC prefabricated part is applied to the subsequent pressureless infiltration of the 3D-SiC/Al composite material. It may or may not be subjected to an oxidation pretreatment depending on the composition of the aluminum alloy used. The thermal conductivity of the composite material can reach 232W/m ℃, and the density of the composite material can reach 2.9-3.1g/cm2The bending strength can reach 330 MPa. But the preparation process is complicated, the use amount of the organic solvent is large, and certain pollution is caused to the environment.
The doctor thesis of Beijing university of science and technology "preparation and performance research of short graphite fiber/aluminum electronic packaging material" P8-P42; the authors: the Liuting is Ting; the short graphite fiber/aluminum composite material is prepared by modifying the fiber surface through chemical plating and salt bath plating and adopting vacuum hot-pressing sintering and vacuum pressure infiltration technologies. Although the interface effect of the short graphite fiber and aluminum can be effectively solved, the method is complex, the preparation cost is high, and the prepared material has poor radiation resistance.
The existing SiC/Al composite material electronic packaging material is mainly manufactured by an infiltration method, has problems in heat conduction performance, manufacturing process and welding performance, is particularly difficult to weld by the existing packaging welding in China, limits the application of the material, and needs a novel packaging material to make up the defects of the traditional material.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems that the existing SiC/Al composite material electronic packaging material is mainly manufactured by an infiltration method and has defects in heat-conducting property, manufacturing process and welding property, the preparation method of the compact combined type composite material for electronic packaging is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
(1) respectively weighing 45-50 parts by weight of deionized water, 30-50 parts by weight of 10% copper nitrate solution, 15-20 parts by weight of absolute ethyl alcohol and 10-15 parts by weight of ethyl orthosilicate in a three-neck flask, stirring, mixing and placing at room temperature to obtain mixed base fluid, dropwise adding ammonia water into the mixed base fluid according to the mass ratio of 1:15, stirring, mixing and placing in a water bath kettle after dropwise adding is completed, and performing water bath reaction to obtain matrix gel fluid;
(2) respectively weighing 45-50 parts by weight of deionized water, 10-15 parts by weight of absolute ethyl alcohol and 3-5 parts by weight of ethyl orthosilicate, stirring, mixing and adjusting the pH to 2.5, carrying out heat preservation and reflux to obtain a mixed solution, adding boric acid into the mixed solution in a stirring state according to a mass ratio of 1:15, stirring after the addition is finished, carrying out heat preservation and reflux to obtain a modified sol solution;
(3) stirring and mixing the matrix gel liquid and the modified sol liquid according to the mass ratio of 1:1, preserving heat and aging, collecting the aged sol liquid, taking the single crystal diamond and stirring and mixing the single crystal diamond and the sodium hydroxide solution according to the mass ratio of 1:10, heating and boiling, filtering, collecting a filter cake, and washing to obtain washed diamond particles;
(4) respectively weighing 45-50 parts by weight of deionized water, 3-5 parts by weight of sodium chloride, 1-2 parts by weight of urea and 0.1-0.2 part by weight of resorcinol, placing the materials into a beaker, stirring and mixing the materials, dropwise adding a sodium stannate hydrochloric acid solution, and stirring and mixing the materials to obtain a modified solution; respectively weighing 45-50 parts by weight of deionized water, 3-5 parts by weight of 5% hydrochloric acid, 0.1-0.2 part by weight of palladium chloride and 3-5 parts by weight of stannous oxide in a triangular flask, stirring, mixing and ultrasonically dispersing to obtain a dispersion liquid, dripping the modified liquid into the dispersion liquid according to the mass ratio of 1:2, stirring, mixing, keeping the temperature and curing at 45-50 ℃ to obtain an activated liquid;
(5) adding the washed diamond particles into an activating solution, performing activation treatment to obtain activated modified diamond particles, respectively weighing 45-50 parts by weight of nano copper powder, 10-15 parts by weight of activated modified diamond particles and 6-8 parts by weight of aged sol solution, placing the obtained mixture into a mold, performing pressure maintaining treatment to obtain a cold-pressed blank, placing the cold-pressed blank into a muffle furnace, heating and performing heat preservation calcination, performing compression molding, standing and cooling to room temperature, and demolding to obtain the compact combined type composite material for electronic packaging.
The dropping speed of the ammonia water is 2 mL/min.
The water bath reaction is carried out by heating to 40-45 ℃ at a speed of 1 ℃/min, carrying out heat preservation reaction for 3-5 h, then heating to 85-95 ℃ at a speed of 3 ℃/min, and carrying out heat preservation water bath reaction for 1-2 h.
The boric acid is added at a stirring speed of 250-300 r/min.
And the washing treatment is to wash the mixture for 3-5 times by using nitric acid with the mass fraction of 15%, and then wash the mixture by using deionized water until the washing liquid is neutral.
The sodium stannate hydrochloric acid solution is a sodium stannate hydrochloric acid solution with the same mass percentage of 1% of sodium chloride.
The pressure maintaining pressure of the cold-pressed blank is 450-500 MPa.
The heating and heat preservation calcining is carried out at the temperature of 1100-1200 ℃ at the speed of 8 ℃/min, and the heat preservation reaction is carried out for 35-45 min.
The compression molding pressure is 45-50 MPa.
Compared with other methods, the method has the beneficial technical effects that:
(1) the technical scheme of the invention adopts a sol-gel method to prepare copper-based composite sol solution and composite sol prepared by doping boric acid in a pure silica sol system, physical or chemical modification is carried out by doping other components in the sol forming stage, so that the sol system has amphiphilic properties of metal copper and diamond, and an interface material structure is formed between the composite sol and the material, generally, the diamond/copper-based composite material has low interface thermal conductivity and large thermal resistance, and the heat is blocked at the interface and can not effectively transfer the heat, so that the temperature gradient change at the interface position is large, but the technical scheme of the invention is tighter and denser along with the interface combination, the combination coefficient is gradually increased, the heat flow density near particles is increased, the heat flow vectors of adjacent diamond particles are linked and even overlapped, and a heat conduction channel is generated, the heat conduction channels are increased, the interaction between the diamond particles obviously improves the heat conduction performance of the composite material, the increase of the heat conduction channels shortens the transmission path of heat flow, the heat flow can be quickly transmitted through the heat conduction networks, namely the heat conductivity of the composite material is quickly increased, and the heat conduction efficiency and the compactness of the material are effectively improved;
(2) in the technical scheme of the invention, through acid modification and alkali modification treatment on the surface of the diamond material, a plurality of discontinuous 'old' shaped locking holes are formed on the surface of the powder under the action of strong acid, the shaped locking holes are beneficial to the adsorption of metal copper particles in the locking holes and the effective combination of the surface of an interface sol material, and the surface of the material is effectively modified, so that the material has excellent combination strength and the compact combination performance of a composite material is improved, meanwhile, boron and a compound nano structure thereof are introduced on the surface of the diamond particles, on one hand, because the solubility of element boron and metal copper is higher than the solubility of element carbon and copper by orders of magnitude, the interface chemical property of diamond and copper is improved, on the other hand, boron nanowires are grown on the surface of the diamond particles, so that the boron nanowires are contacted with the metal copper, and the contact area of the diamond and the copper is improved, and a heat transfer channel is added, so that the high-heat-conductivity composite material can be obtained, the compact bonding strength of the material is further improved, and the heat-conducting property of the material is improved.
Detailed Description
Respectively weighing 45-50 parts by weight of deionized water, 30-50 parts by weight of 10% copper nitrate solution, 15-20 parts by weight of absolute ethyl alcohol and 10-15 parts by weight of ethyl orthosilicate, placing the mixture in a three-neck flask, stirring, mixing and placing the mixture at room temperature to obtain a mixed base fluid, dropwise adding 10% by weight of ammonia water into the mixed base fluid according to the mass ratio of 1:15, controlling the dropwise adding rate to be 2mL/min, stirring, mixing, placing the mixture in a water bath, heating to 40-45 ℃ at 1 ℃/min, carrying out heat preservation reaction for 3-5 h, heating to 85-95 ℃ at 3 ℃/min, carrying out heat preservation water bath reaction for 1-2 h, and collecting a base gel fluid; respectively weighing 45-50 parts by weight of deionized water, 10-15 parts by weight of absolute ethyl alcohol and 3-5 parts by weight of ethyl orthosilicate, stirring and mixing, adjusting the pH to 2.5 by using 0.5mol/L hydrochloric acid, carrying out heat preservation and reflux at 65-75 ℃ for 2-3 hours to obtain a mixed solution, adding boric acid into the mixed solution according to the mass ratio of 1:15, controlling the stirring speed to be 250-300 r/min, and carrying out heat preservation and reflux at 65-75 ℃ for 2-3 hours after stirring is completed, so as to obtain a modified sol solution; stirring and mixing the matrix gel liquid and the modified sol liquid according to the mass ratio of 1:1, preserving heat and aging at 45-50 ℃ for 3-5 h, and collecting the aged sol liquid; taking single crystal diamond, stirring and mixing the diamond and a sodium hydroxide solution with the mass fraction of 10% according to the mass ratio of 1:10, heating and boiling, filtering and collecting a filter cake, washing the filter cake for 3-5 times by using nitric acid with the mass fraction of 15%, and washing the filter cake by using deionized water until a washing solution is neutral to obtain washed diamond particles; respectively weighing 45-50 parts by weight of deionized water, 3-5 parts by weight of sodium chloride, 1-2 parts by weight of urea and 0.1-0.2 part by weight of resorcinol, placing the materials into a beaker, stirring and mixing the materials, dropwise adding a sodium stannate hydrochloric acid solution with the same mass fraction as that of the sodium chloride, and stirring and mixing the materials to obtain a modified solution; respectively weighing 45-50 parts by weight of deionized water, 3-5 parts by weight of 5% hydrochloric acid, 0.1-0.2 part by weight of palladium chloride and 3-5 parts by weight of stannous oxide in a triangular flask, stirring, mixing and ultrasonically dispersing to obtain a dispersion, dropwise adding a modification solution into the dispersion according to a mass ratio of 1:2, stirring, mixing, keeping the temperature and curing at 45-50 ℃ for 3-5 hours to obtain an activation solution, adding the washed diamond particles into the activation solution according to a mass ratio of 1:10, performing activation treatment to obtain activated modified diamond particles, respectively weighing 45-50 parts by weight of nano copper powder, 10-15 parts by weight of activated modified diamond particles and 6-8 parts by weight of aged sol solution in a mold, performing pressure-maintaining treatment at 450-550 MPa for 1-2 minutes to obtain a cold-pressed blank, placing the cold-pressed blank in a muffle furnace, heating to 1100-1200 ℃ at 8 ℃/min, performing heat-maintaining reaction for 35-45 minutes, and pressing for 3-5 min under 45-50 MPa, standing, cooling to room temperature, and demolding to obtain the compact combined type composite material for electronic packaging.
Example 1
Respectively weighing 45 parts by weight of deionized water, 30 parts by weight of 10% copper nitrate solution, 15 parts by weight of anhydrous ethanol and 10 parts by weight of ethyl orthosilicate, placing the deionized water, the 30 parts by weight of 10% copper nitrate solution, the 15 parts by weight of anhydrous ethanol and the 10 parts by weight of ethyl orthosilicate into a three-neck flask, stirring and mixing the mixture and placing the mixture at room temperature to obtain mixed base fluid, dropwise adding 10% by weight of ammonia water into the mixed base fluid according to the mass ratio of 1:15, controlling the dropwise adding rate to be 2mL/min, stirring and mixing the mixture after the dropwise adding is finished, placing the mixture in a water bath, heating the mixture to 40 ℃ according to 1 ℃/min, carrying out heat preservation reaction for 3h, heating the mixture to 85 ℃; respectively weighing 45 parts by weight of deionized water, 10 parts by weight of absolute ethyl alcohol and 3 parts by weight of ethyl orthosilicate, stirring and mixing, adjusting the pH to 2.5 by using 0.5mol/L hydrochloric acid, preserving heat and refluxing at 65 ℃ for 2 hours to obtain a mixed solution, adding boric acid into the mixed solution according to a mass ratio of 1:15, controlling the stirring rate to be 250r/min, and preserving heat and refluxing at 65 ℃ for 2 hours after stirring is completed, so as to obtain a modified sol solution; stirring and mixing the matrix gel liquid and the modified sol liquid according to the mass ratio of 1:1, preserving heat and aging at 45 ℃ for 3 hours, and collecting aged sol liquid; taking single crystal diamond, stirring and mixing the diamond and a sodium hydroxide solution with the mass fraction of 10% according to the mass ratio of 1:10, heating and boiling, filtering and collecting a filter cake, washing for 3 times by using nitric acid with the mass fraction of 15%, and washing by using deionized water until a washing solution is neutral to obtain washed diamond particles; respectively weighing 45 parts of deionized water, 3 parts of sodium chloride, 1 part of urea and 0.1 part of resorcinol according to parts by weight, placing the deionized water, the sodium chloride, the urea and the resorcinol in a beaker, stirring and mixing, dropwise adding a sodium stannate hydrochloric acid solution with the same mass fraction as that of the sodium chloride, and stirring and mixing to obtain a modified solution; respectively weighing 45 parts of deionized water, 3 parts of hydrochloric acid with the mass fraction of 5%, 0.1 part of palladium chloride and 3 parts of stannous oxide in parts by weight, placing the materials in a triangular flask, stirring, mixing and ultrasonically dispersing to obtain dispersion, dripping the modified solution into the dispersion according to the mass ratio of 1:2, stirring, mixing, keeping the temperature at 45 ℃, curing for 3 hours to obtain an activation solution, adding the washed diamond particles into the activation solution according to the mass ratio of 1:10, after the activation treatment, obtaining activated modified diamond particles, respectively weighing 45 parts of nano copper powder, 10 parts of activated modified diamond particles and 6 parts of aged sol solution in parts by weight, placing the nano copper powder, the activated modified diamond particles and the aged sol solution in a mold, maintaining the pressure at 450MPa for 1min to obtain cold-pressed blank, placing in a muffle furnace, heating to 1100 deg.C at 8 deg.C/min, reacting for 35min, and pressing for 3min under 45MPa, standing, cooling to room temperature, and demolding to obtain the compact combined type composite material for electronic packaging.
Example 2
Respectively weighing 47 parts by weight of deionized water, 40 parts by weight of 10% copper nitrate solution, 17 parts by weight of anhydrous ethanol and 13 parts by weight of ethyl orthosilicate, placing the mixture in a three-neck flask, stirring and mixing the mixture and placing the mixture at room temperature to obtain mixed base fluid, dropwise adding 10% by weight of ammonia water into the mixed base fluid according to the mass ratio of 1:15, controlling the dropwise adding rate to be 2mL/min, stirring and mixing the mixture after the dropwise adding is finished, placing the mixture in a water bath, heating the mixture to 43 ℃ according to 1 ℃/min, carrying out heat preservation reaction for 4 hours, heating the mixture to 90 ℃ according to 3 ℃/min, carrying out heat preservation water bath reaction for 1.5 hours, and collecting the base gel fluid; respectively weighing 47 parts by weight of deionized water, 13 parts by weight of absolute ethyl alcohol and 4 parts by weight of ethyl orthosilicate, stirring and mixing, adjusting the pH to 2.5 by using 0.5mol/L hydrochloric acid, carrying out heat preservation and reflux at 70 ℃ for 2.5 hours to obtain a mixed solution, adding boric acid into the mixed solution according to the mass ratio of 1:15, controlling the stirring speed to be 275r/min, carrying out heat preservation and reflux at 70 ℃ for 2.5 hours after the addition is finished and stirring for 27 minutes to obtain a modified sol solution; stirring and mixing the matrix gel liquid and the modified sol liquid according to the mass ratio of 1:1, preserving heat and aging at 47 ℃ for 4 hours, and collecting aged sol liquid; taking single crystal diamond, stirring and mixing the diamond and a sodium hydroxide solution with the mass fraction of 10% according to the mass ratio of 1:10, heating and boiling, filtering and collecting a filter cake, washing the filter cake for 4 times by using nitric acid with the mass fraction of 15%, and washing the filter cake by using deionized water until a washing solution is neutral to obtain washed diamond particles; respectively weighing 47 parts of deionized water, 4 parts of sodium chloride, 1.5 parts of urea and 0.15 part of resorcinol in parts by weight, placing the materials into a beaker, stirring and mixing the materials, dropwise adding a sodium stannate hydrochloric acid solution with the same mass fraction as that of the sodium chloride, and stirring and mixing the materials to obtain a modified solution; respectively weighing 47 parts by weight of deionized water, 4 parts by weight of 5% hydrochloric acid, 0.15 part by weight of palladium chloride and 4 parts by weight of stannous oxide, placing the materials in a triangular flask, stirring, mixing and ultrasonically dispersing to obtain dispersion, dripping the modified solution into the dispersion according to the mass ratio of 1:2, stirring, mixing, keeping the temperature and curing at 47 ℃ for 4h to obtain an activation solution, adding the washed diamond particles into the activation solution according to the mass ratio of 1:10, after the activation treatment, activated modified diamond particles are obtained, 47 parts of nano copper powder, 13 parts of activated modified diamond particles and 7 parts of aged sol solution are respectively weighed according to parts by weight and placed in a mould, maintaining the pressure at 500MPa for 1.5min to obtain cold-pressed blank, placing the cold-pressed blank in a muffle furnace, heating to 1150 ℃ at the speed of 8 ℃/min, keeping the temperature for reaction for 40min, then pressing for 4min under the pressure of 47MPa, standing, cooling to room temperature, and demolding to obtain the compact combined type composite material for electronic packaging.
Example 3
Respectively weighing 50 parts by weight of deionized water, 50 parts by weight of 10% copper nitrate solution, 20 parts by weight of anhydrous ethanol and 15 parts by weight of ethyl orthosilicate, placing the deionized water, the 50 parts by weight of 10% copper nitrate solution, the 20 parts by weight of anhydrous ethanol and the 15 parts by weight of ethyl orthosilicate into a three-neck flask, stirring and mixing the mixture and placing the mixture at room temperature to obtain a mixed base fluid, dropwise adding 10% by weight of ammonia water into the mixed base fluid according to the mass ratio of 1:15, controlling the dropwise adding rate to be 2mL/min, stirring and mixing the mixture after the dropwise adding is finished, placing the mixture in a water bath, heating the mixture to 45 ℃ according to the speed of 1 ℃/min, carrying out heat preservation reaction for 5 hours, heating the; respectively weighing 50 parts by weight of deionized water, 15 parts by weight of absolute ethyl alcohol and 5 parts by weight of ethyl orthosilicate, stirring and mixing, adjusting the pH to 2.5 by using 0.5mol/L hydrochloric acid, preserving heat and refluxing at 75 ℃ for 3 hours to obtain a mixed solution, adding boric acid into the mixed solution according to the mass ratio of 1:15, controlling the stirring speed to be 300r/min, and preserving heat and refluxing at 75 ℃ for 3 hours after stirring is completed, so as to obtain a modified sol solution; stirring and mixing the matrix gel liquid and the modified sol liquid according to the mass ratio of 1:1, preserving heat at 50 ℃ and aging for 5 hours, and collecting the aged sol liquid; taking single crystal diamond, stirring and mixing the diamond and a sodium hydroxide solution with the mass fraction of 10% according to the mass ratio of 1:10, heating and boiling, filtering and collecting a filter cake, washing the filter cake for 5 times by using nitric acid with the mass fraction of 15%, and washing the filter cake by using deionized water until a washing solution is neutral to obtain washed diamond particles; respectively weighing 50 parts by weight of deionized water, 5 parts by weight of sodium chloride, 2 parts by weight of urea and 0.2 part by weight of resorcinol, placing the deionized water, the sodium chloride, the urea and the resorcinol into a beaker, stirring and mixing the deionized water, the sodium chloride, the urea and the resorcinol, the sodium stannate and the hydrochloric acid with the same mass fraction as that of the sodium chloride, and stirring and mixing the solution to obtain a modified solution; respectively weighing 50 parts of deionized water, 5 parts of hydrochloric acid with the mass fraction of 5%, 0.2 part of palladium chloride and 5 parts of stannous oxide in parts by weight, placing the materials in a triangular flask, stirring, mixing and ultrasonically dispersing to obtain dispersion, dripping the modified solution into the dispersion according to the mass ratio of 1:2, stirring, mixing, keeping the temperature and curing at 50 ℃ for 5h to obtain an activation solution, adding the washed diamond particles into the activation solution according to the mass ratio of 1:10, after the activation treatment, activated modified diamond particles are obtained, 50 parts of nano copper powder, 15 parts of activated modified diamond particles and 8 parts of aged sol solution are respectively weighed in parts by weight and placed in a mould, maintaining the pressure at 550MPa for 2min to obtain cold-pressed blank, placing in a muffle furnace, heating to 1200 deg.C at 8 deg.C/min, reacting for 45min, and pressing for 5min under 50MPa, standing, cooling to room temperature, and demolding to obtain the compact combined type composite material for electronic packaging.
The composite material for compact combined electronic packaging prepared by the invention and the existing SiC/Al composite material electronic packaging material are subjected to performance detection, and specific detection results are shown in the following table 1.
The test method comprises the following steps:
1. thermal conductivity test
According to the national standard GB11108-89, the thermal conductivity of the electronic packaging material is measured by a Denshi NETZSCHJR3 thermal conductivity tester.
The experiment tests the thermal conductivity of the electronic packaging material at normal temperature, and the preparation process of the sample is as follows: cutting the prepared electronic packaging material into rectangular blocks of 10mm multiplied by 2mm, and polishing the surfaces of the rectangular blocks to be flat and parallel; and sequentially putting the sample into acetone and alcohol for ultrasonic cleaning, and airing to finish the preparation of the thermal conductivity sample.
Coefficient of thermal expansion
The test was carried out using a Delhi Dil402PC thermal expansion tester. The experiment tests the thermal expansion coefficient of the electronic packaging material within the range of 20-500 ℃, the size of a sample is 5 multiplied by 20mm, and the heating rate is 10 ℃/min. In order to ensure the temperature uniformity during the test and prevent the sample from being oxidized, the experiment is carried out under the protection of nitrogen atmosphere, and the nitrogen flow is 20 ml/min.
TABLE 1 characterization of composite Material for dense combination electronic packaging
As can be seen from Table 1, the composite material for dense bonding electronic packaging prepared by the invention has high thermal conductivity and stable and controllable thermal expansion coefficient.
Claims (9)
1. A preparation method of a compact combined type composite material for electronic packaging is characterized by comprising the following specific preparation steps:
(1) respectively weighing 45-50 parts by weight of deionized water, 30-50 parts by weight of 10% copper nitrate solution, 15-20 parts by weight of absolute ethyl alcohol and 10-15 parts by weight of ethyl orthosilicate in a three-neck flask, stirring, mixing and placing at room temperature to obtain mixed base fluid, dropwise adding ammonia water into the mixed base fluid according to the mass ratio of 1:15, stirring, mixing and placing in a water bath kettle after dropwise adding is completed, and performing water bath reaction to obtain matrix gel fluid;
(2) respectively weighing 45-50 parts by weight of deionized water, 10-15 parts by weight of absolute ethyl alcohol and 3-5 parts by weight of ethyl orthosilicate, stirring, mixing and adjusting the pH to 2.5, carrying out heat preservation and reflux to obtain a mixed solution, adding boric acid into the mixed solution in a stirring state according to a mass ratio of 1:15, stirring after the addition is finished, carrying out heat preservation and reflux to obtain a modified sol solution;
(3) stirring and mixing the matrix gel liquid and the modified sol liquid according to the mass ratio of 1:1, preserving heat and aging, collecting the aged sol liquid, taking the single crystal diamond and stirring and mixing the single crystal diamond and the sodium hydroxide solution according to the mass ratio of 1:10, heating and boiling, filtering, collecting a filter cake, and washing to obtain washed diamond particles;
(4) respectively weighing 45-50 parts by weight of deionized water, 3-5 parts by weight of sodium chloride, 1-2 parts by weight of urea and 0.1-0.2 part by weight of resorcinol, placing the materials into a beaker, stirring and mixing the materials, dropwise adding a sodium stannate hydrochloric acid solution, and stirring and mixing the materials to obtain a modified solution; respectively weighing 45-50 parts by weight of deionized water, 3-5 parts by weight of 5% hydrochloric acid, 0.1-0.2 part by weight of palladium chloride and 3-5 parts by weight of stannous oxide in a triangular flask, stirring, mixing and ultrasonically dispersing to obtain a dispersion liquid, dripping the modified liquid into the dispersion liquid according to the mass ratio of 1:2, stirring, mixing, keeping the temperature and curing at 45-50 ℃ to obtain an activated liquid;
(5) adding the washed diamond particles into an activating solution, performing activation treatment to obtain activated modified diamond particles, respectively weighing 45-50 parts by weight of nano copper powder, 10-15 parts by weight of activated modified diamond particles and 6-8 parts by weight of aged sol solution, placing the obtained mixture into a mold, performing pressure maintaining treatment to obtain a cold-pressed blank, placing the cold-pressed blank into a muffle furnace, heating and performing heat preservation calcination, performing compression molding, standing and cooling to room temperature, and demolding to obtain the compact combined type composite material for electronic packaging.
2. The method for preparing the composite material for dense bonding electronic packaging according to claim 1, wherein: the dropping speed of the ammonia water is 2 mL/min.
3. The method for preparing the composite material for dense bonding electronic packaging according to claim 1, wherein: the water bath reaction is carried out by heating to 40-45 ℃ at a speed of 1 ℃/min, carrying out heat preservation reaction for 3-5 h, then heating to 85-95 ℃ at a speed of 3 ℃/min, and carrying out heat preservation water bath reaction for 1-2 h.
4. The method for preparing the composite material for dense bonding electronic packaging according to claim 1, wherein: the boric acid is added at a stirring speed of 250-300 r/min.
5. The method for preparing the composite material for dense bonding electronic packaging according to claim 1, wherein: and the washing treatment is to wash the mixture for 3-5 times by using nitric acid with the mass fraction of 15%, and then wash the mixture by using deionized water until the washing liquid is neutral.
6. The method for preparing the composite material for dense bonding electronic packaging according to claim 1, wherein: the sodium stannate hydrochloric acid solution is a sodium stannate hydrochloric acid solution with the same mass percentage of 1% of sodium chloride.
7. The method for preparing the composite material for dense bonding electronic packaging according to claim 1, wherein: the pressure maintaining pressure of the cold-pressed blank is 450-500 MPa.
8. The method for preparing the composite material for dense bonding electronic packaging according to claim 1, wherein: the heating and heat preservation calcining is carried out at the temperature of 1100-1200 ℃ at the speed of 8 ℃/min, and the heat preservation reaction is carried out for 35-45 min.
9. The method for preparing the composite material for dense bonding electronic packaging according to claim 1, wherein: the compression molding pressure is 45-50 MPa.
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| CN113308617A (en) * | 2021-05-26 | 2021-08-27 | 河南工业大学 | Preparation method of diamond/Al composite material with interpenetrating structure |
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