CN113999617A - Method for preparing inorganic heat-conducting glue by using etched diamond micro powder as filler - Google Patents
Method for preparing inorganic heat-conducting glue by using etched diamond micro powder as filler Download PDFInfo
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- CN113999617A CN113999617A CN202111381018.7A CN202111381018A CN113999617A CN 113999617 A CN113999617 A CN 113999617A CN 202111381018 A CN202111381018 A CN 202111381018A CN 113999617 A CN113999617 A CN 113999617A
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 117
- 239000010432 diamond Substances 0.000 title claims abstract description 117
- 239000000843 powder Substances 0.000 title claims abstract description 92
- 239000003292 glue Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000000945 filler Substances 0.000 title claims abstract description 15
- 239000011159 matrix material Substances 0.000 claims abstract description 37
- 238000012986 modification Methods 0.000 claims abstract description 22
- 230000004048 modification Effects 0.000 claims abstract description 22
- 238000005530 etching Methods 0.000 claims abstract description 13
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 10
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 2
- 230000003247 decreasing effect Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000032683 aging Effects 0.000 abstract description 8
- 239000000853 adhesive Substances 0.000 abstract description 7
- 230000001070 adhesive effect Effects 0.000 abstract description 7
- 238000011049 filling Methods 0.000 abstract description 4
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 5
- 230000018109 developmental process Effects 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 238000007605 air drying Methods 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002113 nanodiamond Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Classifications
-
- 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
- C09J1/02—Adhesives based on inorganic constituents containing water-soluble alkali silicates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
-
- 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
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
Abstract
The invention discloses a method for preparing heat-conducting glue by using etched diamond micro powder as a filler and sodium silicate as a matrix, belonging to the field of diamond functionalized application. The main process comprises four parts of etching of diamond micropowder, impurity removal of the etched diamond micropowder, surface modification treatment of the etched diamond micropowder, and combination of the modified diamond micropowder serving as a filler and a heat-conducting adhesive matrix. The invention has simple operation, improved heat conductivity, good corrosion resistance and good aging resistance. The etched diamond micro powder can be combined with the matrix more firmly, and the mechanical property of the heat-conducting glue can be ensured under the condition of high diamond micro powder filling amount. The heat conductivity coefficient of the heat-conducting glue can be further improved by adopting the etched diamond micro powder. The inorganic matrix with more excellent ageing resistance can improve the ageing resistance of the heat-conducting glue, so that the service life of the heat-conducting glue is prolonged.
Description
Technical Field
The invention relates to the field of diamond application, in particular to a preparation method for preparing inorganic heat-conducting glue by using etched diamond micro powder as a filler.
Background
The diamond micro powder has higher specific surface area and better dispersibility than nano diamond, so the micron-level diamond micro powder is widely applied in recent years to prepare various composite materials. Because diamond has excellent performances such as high thermal conductivity, the application of diamond micropowder in the field of heat conduction attracts many students.
At present, in order to meet the development requirements of microelectronic technology, the volume of electronic devices is continuously reduced, the integration level is continuously improved, and the power consumption of integrated circuits is also increased, so that the heat flux density of electronic equipment is higher and higher. The problem of heat dissipation of electronic components is one of the important factors that restrict the integration development of electronic devices. With the development of 5G mobile networks, the requirement for effective heat conduction inside electronic devices is more prominent. Due to the presence of surface roughness, the contact between an electronic component, such as a chip, and a heat sink is not perfectly matched. There may be air between the contact surfaces so that heat transfer is impeded. Therefore, it is necessary to fill a thermal interface material between the electronic component and the heat dissipation device, and to exhaust air so that heat can be better conducted to the outside.
In the field of heat-conducting glue applied to electronic products, the diamond micro powder has good heat conductivity, so that the diamond micro powder can be used as a filler to prepare the heat-conducting glue for heat dissipation of the electronic products. At present, many scholars take epoxy resin as a matrix of the heat-conducting adhesive, but the organic matrix of the heat-conducting adhesive has poor high-temperature resistance, is easy to age, has high curing temperature, and has problems of cracks, peeling phenomena and the like caused by stress generated by thermal expansion, and the problems are yet to be overcome. If an inorganic matrix with better ageing resistance is used and the surface of the diamond micro powder is modified, such as etching, the service life of the heat-conducting adhesive is prolonged.
Disclosure of Invention
The invention aims to: etching the diamond micro powder by adopting Ni powder, and removing Ni and oxides thereof by using an acid washing and ultrasonic oscillation method. So that the surface of the diamond micro powder generates an etching pit, the specific surface area of the diamond micro powder can be further improved, and the diamond micro powder can be better combined with a heat-conducting glue matrix. When the diamond micro powder filling amount reaches a certain value, due to the increase of the content of the diamond micro powder, the diamond micro powder forms a heat conduction network in the heat conduction glue, so that the heat conduction coefficient of the heat conduction glue is greatly improved. But at the same time, the mechanical properties of the heat-conducting adhesive, such as tensile strength, etc., are reduced because the diamond micro-powders are contacted with each other. If the etched diamond micro powder is used as a filler, the diamond micro powder is not simply contacted with each other, and the heat-conducting resin base exists in an etching pit on the surface of the diamond micro powder to play a role in increasing the binding force between the diamond micro powder. The filling amount of the diamond micro powder can be improved under the same mechanical property of the heat-conducting glue, so that the heat conductivity coefficient of the heat-conducting glue can be improved. In order to improve the ageing resistance of the heat-conducting adhesive, inorganic matrix sodium silicate with higher ageing resistance is adopted as a matrix of the heat-conducting adhesive.
Technical scheme
In order to realize the purpose of the invention, the following technical scheme is adopted for realizing the purpose:
a. the diamond micro powder etching comprises the following specific processes: uniformly mixing diamond micro powder and Ni powder according to the proportion of 1:5, and placing the mixture into a crucible to etch in a tubular furnace. The temperature and time parameters are that the temperature is raised from room temperature to 600 ℃ at the speed of 10 ℃/min to 20 ℃/min, the temperature is raised from 600 ℃ to 900 ℃ at the speed of 5 ℃/min to 10 ℃/min, the temperature is kept at 900 ℃ for 60min to 80min, then the temperature is lowered to 300 ℃ at the speed of 10 ℃/min to 20 ℃/min, and the temperature is naturally cooled to room temperature.
b. Removing impurities from the etched diamond micro powder, and the specific process comprises the following steps: putting the etched diamond micro powder into a beaker, adding a nitric acid solution, heating in a water bath kettle at 80 ℃, carrying out ultrasonic oscillation, filtering, washing with distilled water until the solution is neutral, putting into a blast drying oven, carrying out drying treatment at 110 ℃, and taking out for later use.
c. The surface modification treatment of the etched diamond micropowder comprises the following specific processes: and taking the etched diamond micro powder, carrying out surface modification on the diamond micro powder by using sodium dodecyl benzene sulfonate, and drying. The diamond micropowder with the modified surface is ready for use. The dispersion uniformity of the diamond micropowder subjected to surface modification in the heat-conducting glue matrix is improved.
d. The modified diamond micropowder is used as a filler and is combined with a heat-conducting glue matrix, and the specific process comprises the following steps: liquid sodium silicate is selected as an inorganic matrix, etched and modified diamond micro powder is added, and the modified diamond micro powder with the particle size of 60 micrometers and the modified diamond micro powder with the particle size of 30 micrometers are proportioned. Stirring for 1h to uniformly distribute the diamond micropowder in the matrix. Then adding MgO as a curing agent, continuously stirring for a period of time, and packaging.
In the invention, the etched diamond micro powder in the step b is subjected to impurity removal, and the preferable process is as follows: putting the etched diamond micro powder into a beaker, adding a nitric acid solution with the concentration of 50-70%, heating in a water bath at 80 ℃ for 30-50 min in a water bath, then oscillating for 40-60 min by ultrasonic waves, filtering, washing with distilled water until the solution is neutral, putting the solution into a blast drying oven, drying at 110 ℃ for 2-3 h, and taking out for later use.
In the invention, the modified diamond micropowder in the step d is used as a filler to be combined with a heat-conducting glue matrix, and the preferred process is as follows: 5g to 7g of liquid sodium silicate is selected as an inorganic matrix, the diamond micro powder after etching modification is added, and the modified diamond micro powder with the particle size of 60 mu m and the modified diamond micro powder with the particle size of 30 mu m are adopted, wherein the mass ratio is 3:1,2:1 and 3:2 respectively. Stirring for 1h to uniformly distribute the diamond micropowder in the matrix. Then adding 1 to 1.4g of MgO as a curing agent, continuously stirring for 30 to 40min, and packaging.
The invention has the beneficial effects that:
1. the Ni powder is adopted to etch the diamond micro powder, so that the bonding capacity of the diamond micro powder and a matrix can be increased, the filling amount of the diamond micro powder can be increased, and the heat conductivity coefficient of the heat-conducting glue is further increased.
2. The surface modification of the etched diamond micro powder by the sodium dodecyl benzene sulfonate can improve the dispersion uniformity of the diamond micro powder in the heat-conducting glue matrix, so that the diamond micro powder filler can form a better heat-conducting network in the heat-conducting glue.
3. The sodium silicate has excellent performances of strong bonding force, higher strength, good heat resistance, good ageing resistance and the like, can improve the ageing resistance of the heat-conducting glue as a heat-conducting glue matrix, and prolongs the service life of the heat-conducting glue.
Detailed Description
The invention is further described below with reference to specific examples:
example 1:
a. uniformly mixing diamond micro powder and Ni powder according to the proportion of 1:5, and placing the mixture into a crucible to etch in a tubular furnace. The temperature and time parameters are that the temperature is raised from room temperature to 600 ℃ at the speed of 10 ℃, the temperature is raised from 600 ℃ to 900 ℃ at the speed of 5 ℃/min, the temperature is preserved for 60min at 900 ℃, then the temperature is lowered to 300 ℃ at the speed of 10 ℃/min, and finally the temperature is naturally cooled to room temperature.
b. Removing impurities from the etched diamond micro powder, and the specific process comprises the following steps: putting the etched diamond micro powder into a beaker, adding a nitric acid solution with the concentration of 50%, heating in a water bath at 80 ℃ for 30min in a water bath, oscillating for 40min by ultrasonic waves, filtering, washing with distilled water until the solution is neutral, putting into a blast drying oven, drying at 110 ℃ for 2h, and taking out for later use.
c. The surface modification treatment of the etched diamond micropowder comprises the following specific processes: and taking the etched diamond micro powder, carrying out surface modification on the diamond micro powder by using sodium dodecyl benzene sulfonate, and drying. The diamond micropowder with the modified surface is ready for use. The dispersion uniformity of the diamond micropowder subjected to surface modification in the heat-conducting glue matrix is improved.
d. The modified diamond micropowder is used as a filler and is combined with a heat-conducting glue matrix, and the specific process comprises the following steps: 5g of liquid sodium silicate is selected as an inorganic matrix, and etching modified diamond micro powder is added, wherein the weight ratio of the modified diamond micro powder with the particle size of 60 mu m to 1g of the modified diamond micro powder with the particle size of 30 mu m is 3: 1. Stirring for 1h to uniformly distribute the diamond micropowder in the matrix. Then 1g of MgO is added as a curing agent, the mixture is continuously stirred for 30min, and the packaging treatment is carried out.
Example 2:
a. uniformly mixing diamond micro powder and Ni powder according to the proportion of 1:5, and placing the mixture into a crucible to etch in a tubular furnace. The temperature and time parameters are that the temperature is raised from room temperature to 600 ℃ at the speed of 15 ℃/min, the temperature is raised from 600 ℃ to 900 ℃ at the speed of 7 ℃/min, the temperature is preserved for 70min at 900 ℃, then the temperature is lowered to 300 ℃ at the speed of 15 ℃/min, and finally the temperature is naturally cooled to room temperature.
b. Removing impurities from the etched diamond micro powder, and the specific process comprises the following steps: putting the etched diamond micro powder into a beaker, adding a nitric acid solution with the concentration of 60%, heating in a water bath kettle at the temperature of 80 ℃ for 40min in a water bath manner, then oscillating for 50min by ultrasonic waves, filtering, washing with distilled water until the solution is neutral, putting into a forced air drying oven, drying at the temperature of 110 ℃ for 2.5h, and taking out for later use.
c. The surface modification treatment of the etched diamond micropowder comprises the following specific processes: and taking the etched diamond micro powder, carrying out surface modification on the diamond micro powder by using sodium dodecyl benzene sulfonate, and drying. The diamond micropowder with the modified surface is ready for use. The dispersion uniformity of the diamond micropowder subjected to surface modification in the heat-conducting glue matrix is improved.
d. The modified diamond micropowder is used as a filler and is combined with a heat-conducting glue matrix, and the specific process comprises the following steps: 6g of liquid sodium silicate is selected as an inorganic matrix, and etching modified diamond micro powder is added, wherein the amount of the modified diamond micro powder with the particle size of 60 mu m is 3g, the amount of the modified diamond micro powder with the particle size of 30 mu m is 1.5g, and the mass ratio is 2: 1. Stirring for 1h to uniformly distribute the diamond micropowder in the matrix. Then 1.2g MgO is added as curing agent, and the mixture is continuously stirred for 35min and packaged.
Example 3:
a. uniformly mixing diamond micro powder and Ni powder according to the proportion of 1:5, and placing the mixture into a crucible to etch in a tubular furnace. The temperature and time parameters are that the temperature is raised from room temperature to 600 ℃ at the speed of 20 ℃/min, the temperature is raised from 600 ℃ to 900 ℃ at the speed of 10 ℃/min, the temperature is preserved for 80min at 900 ℃, then the temperature is lowered to 300 ℃ at the speed of 20 ℃/min, and finally the temperature is naturally cooled to room temperature.
b. Removing impurities from the etched diamond micro powder, and the specific process comprises the following steps: putting the etched diamond micro powder into a beaker, adding a nitric acid solution with the concentration of 70%, heating in a water bath at 80 ℃ for 50min in a water bath, oscillating for 60min by ultrasonic waves, filtering, washing with distilled water until the solution is neutral, putting into a forced air drying oven, drying at 110 ℃ for 3h, and taking out for later use.
c. The surface modification treatment of the etched diamond micropowder comprises the following specific processes: and taking the etched diamond micro powder, carrying out surface modification on the diamond micro powder by using sodium dodecyl benzene sulfonate, and drying. The diamond micropowder with the modified surface is ready for use. The dispersion uniformity of the diamond micropowder subjected to surface modification in the heat-conducting glue matrix is improved.
d. The modified diamond micropowder is used as a filler and is combined with a heat-conducting glue matrix, and the specific process comprises the following steps: 7g of liquid sodium silicate is used as an inorganic matrix, and the diamond micro powder after etching modification is added, wherein the diamond micro powder after modification with the particle size of 60 mu m is 3g, the diamond micro powder after modification with the particle size of 30 mu m is 2g, and the mass ratio is 3: 2. Stirring for 1h to uniformly distribute the diamond micropowder in the matrix. Then 1.4g MgO is added as curing agent, and the mixture is stirred for 40min and packaged.
Claims (2)
1. A preparation method of heat-conducting glue by using etched diamond micro powder as a filler and inorganic gel sodium silicate as a matrix is characterized by comprising the following steps:
a. the diamond micro powder etching comprises the following specific processes: uniformly mixing diamond micro powder and Ni powder according to the ratio of 1:5, placing the mixture into a crucible, and etching the mixture in a tubular furnace, wherein the temperature and the time parameters are that the temperature is increased to 600 ℃ from room temperature at the speed of 10 ℃/min to 20 ℃/min, the temperature is increased to 900 ℃ from 600 ℃ at the speed of 5 ℃/min to 10 ℃/min, the temperature is maintained at 900 ℃ for 60min to 80min, then the temperature is decreased to 300 ℃ at the speed of 10 ℃/min to 20 ℃/min, and the mixture is naturally cooled to room temperature;
b. removing impurities from the etched diamond micro powder, and the specific process comprises the following steps: putting the etched diamond micro powder into a beaker, adding a nitric acid solution, heating in a water bath kettle at 80 ℃, carrying out ultrasonic oscillation, filtering, washing with distilled water until the solution is neutral, putting into a blast drying oven, drying at 110 ℃, and taking out for later use;
c. the surface modification treatment of the etched diamond micropowder comprises the following specific processes: taking the etched diamond micro powder, carrying out surface modification on the diamond micro powder by using sodium dodecyl benzene sulfonate, and drying the diamond micro powder, wherein the diamond micro powder after surface modification is reserved;
d. the modified diamond micropowder is used as a filler and is combined with a heat-conducting glue matrix, and the specific process comprises the following steps: selecting liquid sodium silicate as an inorganic matrix, adding etched and modified diamond micro powder, matching 60 mu m of modified diamond micro powder and 30 mu m of modified diamond micro powder, stirring for 1h to uniformly distribute the diamond micro powder in the matrix, adding MgO as a curing agent, continuously stirring for a period of time, and packaging.
2. The production method according to claim 1, characterized in that: putting the etched diamond micro powder into a beaker, adding a nitric acid solution with the concentration of 50-70%, heating in a water bath at 80 ℃ for 30-50 min in a water bath, then carrying out ultrasonic oscillation for 40-60 min, then filtering, washing with distilled water until the solution is neutral, putting the solution into a blast drying oven, carrying out drying treatment at 110 ℃ for 2-3 h, and taking out for later use; in the step d, the mass ratio of the diamond micro powder after etching modification with the thickness of 60 microns and 30 microns is 3:1,2:1 and 3:2, stirring is carried out for 1h to ensure that the diamond micro powder is uniformly distributed in the matrix, then MgO is added as a curing agent, stirring is carried out continuously for 30min to 40min, and packaging treatment is carried out.
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---|---|---|---|---|
CN115322687A (en) * | 2022-09-23 | 2022-11-11 | 哈尔滨工业大学 | High-thermal-conductivity phosphate-based inorganic insulating adhesive and bonding method thereof |
CN115322687B (en) * | 2022-09-23 | 2023-06-09 | 哈尔滨工业大学 | High-heat-conductivity phosphate-based inorganic insulating adhesive and bonding method thereof |
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