CN109659281B - High-thermal-conductivity electronic packaging composite material and preparation method thereof - Google Patents
High-thermal-conductivity electronic packaging composite material and preparation method thereof Download PDFInfo
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- CN109659281B CN109659281B CN201910087278.XA CN201910087278A CN109659281B CN 109659281 B CN109659281 B CN 109659281B CN 201910087278 A CN201910087278 A CN 201910087278A CN 109659281 B CN109659281 B CN 109659281B
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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
- H01L23/293—Organic, e.g. plastic
- H01L23/295—Organic, e.g. plastic containing a filler
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01L23/34—Arrangements for cooling, heating, ventilating or temperature compensation ; Temperature sensing arrangements
- H01L23/36—Selection of materials, or shaping, to facilitate cooling or heating, e.g. heatsinks
- H01L23/373—Cooling facilitated by selection of materials for the device or materials for thermal expansion adaptation, e.g. carbon
- H01L23/3737—Organic materials with or without a thermoconductive filler
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/73—Means for bonding being of different types provided for in two or more of groups H01L2224/10, H01L2224/18, H01L2224/26, H01L2224/34, H01L2224/42, H01L2224/50, H01L2224/63, H01L2224/71
- H01L2224/732—Location after the connecting process
- H01L2224/73201—Location after the connecting process on the same surface
- H01L2224/73203—Bump and layer connectors
- H01L2224/73204—Bump and layer connectors the bump connector being embedded into the layer connector
Abstract
The invention provides a high-thermal-conductivity electronic packaging composite material and a preparation method thereof, wherein the composite material consists of insulating nano particles and a polymer, and the volume ratio of the insulating nano particles to the polymer is 0.1-0.3; the insulating nano-particles are nano-copper particles coated with a silicon dioxide insulating layer, the thickness of the silicon dioxide insulating layer is 10-100nm, and the particle size of the nano-copper particles is 50-500 nm. The preparation method comprises the steps of preparing insulating nano copper particles, and mixing the insulating nano copper particles with a polymer to prepare the high-thermal-conductivity electronic packaging composite material. The composite material provided by the invention can meet the requirements of packaging insulation and packaging filling on heat conductivity and fluidity, and can remarkably improve the heat dissipation performance of a device, reduce the thermal expansion coefficient, improve the vitrification temperature and greatly improve the electromigration failure time by carrying out nano-composite filling on the composite material.
Description
Technical Field
The invention relates to the technical field of electronic packaging materials, in particular to a high-thermal-conductivity electronic packaging composite material and a preparation method thereof.
Background
Moore's law has been directing the world semiconductor industry to lower cost, higher integration and greater economic efficiency since it was proposed by gorden moore in 1965. With microelectronic chipThe characteristic dimensions of the fabrication gradually approach the physical limits and moore's law no longer applies. However, this does not mean the end of the progress, and the multi-chip three-dimensional integrated package that does not rely on the characteristic size reduction has advantages of shortened interconnections, improved integration, additional more new functions, and rapid market entry, with an increase in processing speed, transmission rate, storage capacity, etc. by 103By-fold, volume reduction to 1/1000, three-dimensional integration will be an important direction of development in the 'post-molar' era.
The multi-chip three-dimensional integrated device which is connected with each other through the micro-bump flip chip performs more and larger calculation in the same space, and the heat of the multi-chip integration is further superposed along with the stacking of the chips while the power density of a single chip is increased; the reduction of the size of the micro bump, the reduction of the filling gap between chips, the thinning of the chip thickness and other changes of the space size lead to large thermal gradient, and the generation of 'hot spots' on the temperature distribution. Existing inter-multichip fill materials are not able to effectively handle the increasing number of hot spots, which ultimately limits their effectiveness, range of implementation, or overall feasibility. The inter-chip fill material will release more heat and stress and new materials are now needed to meet these stringent thermal management challenges than ever before.
Non-metallic materials such as oxide and nitride ceramics have a much lower thermal conductivity, and it is necessary to increase the amount of filler added as much as possible in order to increase the thermal conductivity. Chinese patent CN201610377344.3 discloses an organosilicon ternary packaging material and a preparation method thereof, in the embodiment, the thermal conductivity coefficient of the prepared packaging material with different silica contents is analyzed, and the overall thermal conductivity coefficient is gradually improved along with the improvement of the content of doped silica. However, an increase in the amount of addition inevitably leads to a decrease in the flowability of the encapsulating material.
Therefore, it is necessary to provide an encapsulating material having high thermal conductivity, high insulation properties, and satisfactory flowability of the encapsulating filling.
Disclosure of Invention
The invention aims to provide a high-thermal-conductivity electronic packaging composite material and a preparation method thereof, so that the composite material has high thermal conductivity and insulativity and meets the requirement of packaging filling fluidity.
In order to achieve the purpose, the invention provides the following technical scheme:
a high thermal conductivity electronic packaging composite material is composed of insulating nanoparticles and a polymer, wherein the volume ratio of the insulating nanoparticles to the polymer is 0.1-0.3;
the insulating nano-particles are nano-copper particles coated with a silicon dioxide insulating layer, the thickness of the silicon dioxide insulating layer is 10-100nm, and the particle size of the nano-copper particles is 50-500 nm.
Preferably, the polymer comprises an epoxy, acrylate or phenolic resin.
The invention also provides a preparation method of the high-thermal-conductivity electronic packaging composite material, which comprises the following steps:
the method comprises the following steps: adding polyvinylpyrrolidone and sodium borohydride into the cupric oxalate solution, and stirring to obtain a mixture; wherein the molar ratio of copper oxalate, polyvinylpyrrolidone and sodium borohydride is 2 (1.0-1.2) to 1.2-1.4;
step two: heating and filtering the mixture obtained in the step one to obtain filter residue A, and cleaning the obtained filter residue A to obtain an intermediate product A;
step three: dissolving and dispersing the intermediate product A obtained in the step two to obtain a mixed solution, adding ammonia water and tetraethoxysilane into the mixed solution, stirring and filtering to obtain a filter residue B, and cleaning and drying the filter residue B to obtain powder B;
step four: sintering the powder B obtained in the step three in a mixed gas of argon and hydrogen to obtain insulated nano-copper particles;
step five: and mixing the insulated nano copper particles obtained in the step four with a polymer according to the volume ratio of 0.1-0.3, and stirring to obtain the high-thermal-conductivity electronic packaging composite material.
Preferably, the solvent of the copper oxalate solution is N, N-dimethylformamide.
Preferably, the concentration of the copper oxalate solution is 0.6-1.0 mol/L.
Preferably, the molar ratio of the copper oxalate to the ethyl orthosilicate is 2: 0.2-0.3.
Preferably, the heating is carried out by keeping the mixture at 80-90 ℃ for 3-5 min.
Preferably, the mass percentage concentration of the ammonia water is 25-28%; the volume ratio of the mixed solution to the ammonia water is 100: 1-2.
Preferably, the dissolving and dispersing are to dissolve and disperse the intermediate product a in a mixed solution of ethanol and water; wherein the volume ratio of the ethanol to the water is 1: 1-2.
Preferably, the sintering treatment is specifically to heat the powder B from room temperature to 550-700 ℃ and then preserve the temperature for 1-2 h; wherein the heating rate is 4-6 ℃/min.
The invention firstly utilizes the chemical reaction principle to regulate and control the reaction process to prepare the nano-copper particles, generates a layer of silicon dioxide film on the surface of the nano-copper particles by a chemical method to realize the insulating property of the nano-copper, and adopts the sintering process to densify the film. Mixing the prepared insulating nano copper particles with a polymer, and forming a uniformly distributed composite material by ultrasonic stirring to obtain the microelectronic packaging filling composite material consisting of the polymer-insulating layer-copper particles.
Since copper powder has a relatively low surface energy, silica is difficult to deposit on the surface of copper powder by any means, and the prior art refers to the property of particles in this form as being silica-poor, and having this property also metallic palladium, nickel, etc. Most of silicon dioxide coated copper adopts a method of directly coating elemental copper, and the method needs to adopt a silane coupling agent for surface treatment, so that the binding capacity of the nano copper powder and the silicon dioxide is improved. However, this method of modification by directly adding an active agent requires addition of a large amount of a modifying agent, making the reaction step cumbersome and complicated.
The method comprises the steps of firstly synthesizing cuprous oxide nano copper balls, then coating silicon dioxide, and then carrying out heat treatment to obtain the composite material. The simple and rapid method avoids a large amount of surfactants and complicated steps introduced by solving the problem of silicon-starving behavior, so that the nano copper ball has controllable size and uniform appearance.
The scheme of the invention has the following beneficial effects:
the preparation method of the high-thermal-conductivity electronic packaging composite material provided by the invention is simple in process, low in cost and strong in operability, the size of the prepared nano copper ball is controllable, the shape of the prepared nano copper ball is uniform, and the obtained high-thermal-conductivity electronic packaging composite material is excellent in performance.
The high-thermal-conductivity electronic packaging composite material provided by the invention is a composite material formed by mixing silicon dioxide coated nano copper particles and a polymer. The composite material can meet the requirements of packaging insulation, and simultaneously, the heat dissipation performance of the three-dimensional integrated device is greatly improved by utilizing the heat conduction characteristic of metal, and the requirement of packaging filling on fluidity can also be met.
The high-thermal-conductivity electronic packaging composite material provided by the invention enables the heat dissipation mode of the filling material to be converted from single amorphous phonon heat transfer into phonon and electron heat transfer together, the heat transfer performance of metal crystal electrons is one order of magnitude higher than that of amorphous phonons, and the metal particles form a heat dissipation driving source in a composite body, so that the filling and packaging of the composite material can efficiently release heat energy generated by the service of a three-dimensional integrated device, and the service life of a high-end electronic component is greatly prolonged.
The high-thermal-conductivity electronic packaging composite material provided by the invention is used for nano composite filling, so that the heat dissipation performance of a device can be obviously improved, the thermal expansion coefficient can be reduced, the glass transition temperature can be increased, and the electromigration failure time can be greatly prolonged.
The thermal conductivity of the composite material provided by the embodiment is improved to 3.0W/mK from 0.6-0.8W/mK of the pure silicon dioxide composite material, the thermal expansion coefficient is reduced compared with the pure silicon dioxide composite material, and the electrical resistivity is improved compared with the pure silicon dioxide composite material. Reliability tests of chips filled with the composite material with 40 micron gaps showed that the electromigration failure lifetime of the chips increased from 6 hours for pure silicon dioxide composites to over 17 hours.
Drawings
Fig. 1 is a schematic view of a high thermal conductivity electronic packaging composite material according to the present invention.
Description of the drawings: 1. nano-copper particles; 2. a silicon dioxide layer; 3. a polymer; 4. a chip; 5. a substrate; 6. and (4) micro convex points.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
Example 1
The high-thermal-conductivity electronic packaging composite material provided by the invention is used for packaging and filling a microelectronic chip, and as shown in figure 1, the outer surface of a nano copper particle 1 is coated with a silicon dioxide layer 2; the silicon dioxide layer 2 is used as an insulating layer and has the thickness of 10-100 nm; the particle size of the nano-copper particles is 50-500 nm. Mixing the nano copper particles wrapped with the silicon dioxide layer 2 with a polymer 3 to form a high-thermal-conductivity electronic packaging composite material; wherein the volume ratio of the insulating nanoparticles to the polymer is 0.1-0.3. The polymer comprises an epoxy resin, an acrylate or a phenolic resin.
The high-thermal-conductivity electronic packaging composite material is filled between the chip 4 and the substrate 5, the chip 4 and the substrate 5 further comprise micro bumps 6, and the micro bumps 6 are used for I/O connection between the chip 4 and the substrate 5 to form filling packaging between the chip and the substrate. The high-thermal-conductivity electronic packaging composite material can be filled between the chips to form filling packaging between the chips.
In order to meet the requirements of packaging and filling of microelectronic chips, tests such as insulativity, thermal conductivity and flowability of composite materials with different particle specific weights are carried out. In order to meet the requirement of package filling fluidity, the volume proportion of the particles should be less than or equal to 30 percent, otherwise, the package can not realize filling due to high viscosity. The resistivity of the composite body decreases with increasing particles, and the lowest resistivity is 1012The omega cm can meet the requirement of insulativity, and the thermal conductivity is improved by one order of magnitude compared with the compounding of polymers and pure nano silicon dioxide.
Example 2
The method comprises the following steps: weighing 2mmol of copper oxalate and dissolving the copper oxalate in 25ml of N, N-dimethylformamide solution;
step two: adding 1mmol of polyvinylpyrrolidone and 1.3mmol of sodium borohydride into the solution in the first step;
step three: stirring for five minutes, heating the mixture to 85 ℃, preserving heat for 3 minutes, then filtering to obtain orange precipitate called filter residue A, and washing the filter residue A with alcohol for a plurality of times to obtain an intermediate product A;
step four: dissolving and dispersing the intermediate product A obtained in the third step into a mixed solution of 60ml of water and 40ml of ethanol to obtain a mixed solution;
step five: adding 1mL of concentrated ammonia water into the mixed solution obtained in the fourth step, and then adding 0.24mmol of tetraethoxysilane; wherein the mass percentage concentration of the ammonia water is 28%;
step six: stirring for 6 hours at room temperature, filtering to obtain filter residue B, washing the filter residue B with water and ethanol for a plurality of times, and drying to obtain powder B;
step seven: placing the powder B obtained in the sixth step into a magnetic boat, heating to 630 ℃ at room temperature at a speed of 5 ℃/min in an argon/hydrogen mixed gas, and preserving heat for 1.5h to obtain insulating nano copper particles;
step eight: and mixing the insulating nano copper particles obtained in the sixth step with epoxy resin according to the volume ratio of 0.2 to obtain the high-thermal-conductivity electronic packaging composite material.
The high thermal conductivity electronic packaging composite material obtained in example 2 was subjected to thermal conductivity and insulation performance tests, and was filled between chips to perform reliability tests, and the results are shown in table 1.
TABLE 1 results of performance testing of the composite obtained in example 2 with pure silica polymer materials
Example 3
The method comprises the following steps: weighing 3mmol of copper oxalate and dissolving in 50ml of N, N-dimethylformamide solution;
step two: adding 1.6mmol of polyvinylpyrrolidone and 1.8mmol of sodium borohydride into the solution in the first step;
step three: stirring for five minutes, heating the mixture to 90 ℃, preserving heat for 4 minutes, then filtering to obtain orange precipitate called filter residue A, and washing the filter residue A with alcohol for a plurality of times to obtain an intermediate product A;
step four: dissolving and dispersing the intermediate product A obtained in the third step into a mixed solution of 75ml of water and 75ml of ethanol to obtain a mixed solution;
step five: adding 3mL of concentrated ammonia water into the mixed solution obtained in the fourth step, and then adding 0.3mmol of tetraethoxysilane; wherein the mass percentage concentration of the ammonia water is 26%;
step six: stirring for 7 hours at room temperature, filtering to obtain filter residue B, washing the filter residue B with water and ethanol for a plurality of times, and drying to obtain powder B;
step seven: placing the powder B obtained in the sixth step into a magnetic boat, heating to 550 ℃ at room temperature at a rate of 4 ℃/min in an argon/hydrogen mixed gas, and then preserving heat for 2 hours to obtain insulating nano copper particles;
step eight: and mixing the insulated nano copper particles obtained in the step six with phenolic resin according to the volume ratio of 0.1 to obtain the high-thermal-conductivity electronic packaging composite material.
Example 4
The method comprises the following steps: weighing 2.5mmol of copper oxalate and dissolving in 25ml of N, N-dimethylformamide solution;
step two: adding 1.6mmol of polyvinylpyrrolidone and 1.75mmol of sodium borohydride into the solution in the first step;
step three: stirring for five minutes, heating the mixture to 80 ℃, preserving heat for 5 minutes, then filtering to obtain orange precipitate called filter residue A, and washing the filter residue A with alcohol for a plurality of times to obtain an intermediate product A;
step four: dissolving and dispersing the intermediate product A obtained in the third step into a mixed solution of 80ml of water and 40ml of ethanol to obtain a mixed solution;
step five: adding 2ml of concentrated ammonia water into the mixed solution obtained in the fourth step, and then adding 0.38mmol of ethyl orthosilicate; wherein the mass percentage concentration of the ammonia water is 25%;
step six: stirring for 8 hours at room temperature, filtering to obtain filter residue B, washing the filter residue B with water and ethanol for a plurality of times, and drying to obtain powder B;
step seven: placing the powder B obtained in the sixth step into a magnetic boat, heating to 700 ℃ at the temperature of 30 ℃ at the speed of 6 ℃/min in an argon/hydrogen mixed gas, and then preserving heat for 1h to obtain insulating nano copper particles;
step eight: and mixing the insulating nano copper particles obtained in the step six with acrylic ester according to the volume ratio of 0.3 to obtain the high-thermal-conductivity electronic packaging composite material.
According to the size of the filling gap between the chips, the diameter of the nano particles is designed, the smaller the filling gap is, the smaller the diameter of the designed particles is, and even quantum dots and the quantum dots wrapped by the quantum dots can be adopted. Through adjustment and optimization of chemical process parameters, insulating nano-copper particles with different particle sizes and different film thicknesses are prepared, and composite filling materials with different requirements can be configured.
And carrying out three-dimensional integrated package filling and curing on the multiple chips to form insulating high-heat-conductivity package protection. Finally, reliability test and evaluation of the nano composite packaging device are carried out, and as can be seen from table 1, compared with a pure silicon dioxide polymer filling material, the high-thermal-conductivity electronic packaging composite material prepared by the embodiment of the application can be used for filling, so that the heat dissipation performance of the device can be obviously improved, the thermal expansion coefficient can be reduced, the resistivity and the glass transition temperature can be improved, and the electromigration failure time can be greatly prolonged.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. The preparation method of the high-thermal-conductivity electronic packaging composite material is characterized by comprising the following steps of:
the method comprises the following steps: adding polyvinylpyrrolidone and sodium borohydride into the cupric oxalate solution, and stirring to obtain a mixture; wherein the molar ratio of copper oxalate, polyvinylpyrrolidone and sodium borohydride is 2 (1.0-1.2) to 1.2-1.4;
step two: heating and filtering the mixture obtained in the step one to obtain filter residue A, and cleaning the obtained filter residue A to obtain an intermediate product A;
step three: dissolving and dispersing the intermediate product A obtained in the step two to obtain a mixed solution, adding ammonia water and tetraethoxysilane into the mixed solution, stirring and filtering to obtain a filter residue B, and cleaning and drying the filter residue B to obtain powder B;
step four: sintering the powder B obtained in the step three in a mixed gas of argon and hydrogen to obtain insulated nano-copper particles;
step five: and mixing the insulated nano copper particles obtained in the step four with a polymer according to the volume ratio of 0.1-0.3, and stirring to obtain the high-thermal-conductivity electronic packaging composite material.
2. The method according to claim 1, wherein the solvent of the copper oxalate solution is N, N-dimethylformamide.
3. The method according to claim 1, wherein the concentration of the copper oxalate solution is 0.6 to 1.0 mol/L.
4. The method according to claim 1, wherein the molar ratio of copper oxalate to ethyl orthosilicate is 2: 0.2-0.3.
5. The method according to claim 1, wherein the heating is carried out by incubating the mixture at 80-90 ℃ for 3-5 min.
6. The preparation method of claim 1, wherein the mass percentage concentration of the ammonia water is 25-28%; the volume ratio of the mixed solution to the ammonia water is 100: 1-2.
7. The preparation method according to claim 1, wherein the dissolving and dispersing is specifically to dissolve and disperse the intermediate product a in a mixed solution of ethanol and water; wherein the volume ratio of the ethanol to the water is 1: 1-2.
8. The method as claimed in claim 1, wherein the sintering treatment in step four comprises raising the temperature of the powder B from room temperature to 550-700 ℃ and then maintaining the temperature for 1-2 h; wherein the heating rate is 4-6 ℃/min.
9. The high-thermal-conductivity electronic packaging composite material prepared by the method of any one of claims 1 to 8, wherein the composite material is composed of insulating nanoparticles and a polymer, and the volume ratio of the insulating nanoparticles to the polymer is 0.1-0.3;
the insulating nano particles are nano copper particles coated with a silicon dioxide insulating layer, the thickness of the silicon dioxide insulating layer is 10-100nm, and the particle size of the nano copper particles is 50-500 nm;
the polymer comprises an epoxy resin, an acrylate or a phenolic resin.
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