CN109401732B - Low-oil-permeability heat-conducting silica gel gasket and preparation method thereof - Google Patents
Low-oil-permeability heat-conducting silica gel gasket and preparation method thereof Download PDFInfo
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- CN109401732B CN109401732B CN201811284008.XA CN201811284008A CN109401732B CN 109401732 B CN109401732 B CN 109401732B CN 201811284008 A CN201811284008 A CN 201811284008A CN 109401732 B CN109401732 B CN 109401732B
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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Abstract
The invention discloses a low-oil-permeability heat-conducting silica gel gasket which comprises the following components in parts by weight: 100 parts of vinyl silicone oil, 1-10 parts of hydrogen-containing silicone oil, 0.01-0.5 part of inhibitor, 0.1-0.5 part of catalyst and 700-1200 parts of alumina. The invention also discloses a method for preparing the low-oil-permeability heat-conducting silica gel gasket. The heat-conducting silica gel gasket prepared by the invention has low weight loss rate through aging test, does not have oil seepage phenomenon, and has stable heat-conducting property.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the application of thermal interface materials, in particular to a low-oil-permeability heat-conducting silica gel gasket with low oil permeability and stable heat conducting performance and a preparation method thereof.
[ background of the invention ]
In the heat dissipation design of the thermal interface material, because the thermal interface is not in sufficient contact to generate thermal contact resistance, the heat flow conduction is seriously hindered, and in order to solve the problem, a layer of thermal interface material needs to be arranged between the heating body and the heat dissipation body. Common heat dissipation materials include ceramics, heat-conducting silicone grease and heat-conducting silicone gaskets, wherein the ceramics have high heat conductivity but are brittle and difficult to fill micro gaps between thermal interfaces, and cannot be used as interface materials. The heat-conducting silicone grease can be coated on a very thin layer, so that the heat-conducting effect is good, but the requirements on operability, durability and the satisfaction of a certain tolerance size are difficult to achieve. On the premise that the heat-conducting silica gel gasket can ensure insulation, the heat-conducting silica gel gasket is fully filled in gaps between thermal interfaces by utilizing the characteristics of high elasticity and low-temperature processing molding of high polymers, exhausts air in the gaps generated by the unevenness of the thermal interfaces, has the effects of insulation, shock absorption, sealing and the like, meets the design requirements of equipment miniaturization and ultra-thinness, and is widely applied to electric motor controllers, power supplies, computers, automobile power supplies and the like as a main heat-conducting interface material. However, the conventional heat-conducting silica gel gasket often has an oil leakage phenomenon in a long-term use process, so that the heat-conducting performance of the heat-conducting silica gel gasket is changed, and even lenses, circuits and the like are polluted in serious cases, and the normal work of electronic devices is influenced.
[ summary of the invention ]
The invention aims to solve the problems and provides a low-oil-permeability heat-conducting silica gel gasket with low oil permeability and stable heat conducting performance and a preparation method thereof.
The invention also provides a method for preparing the low-oil-permeability heat-conducting silica gel gasket.
In order to realize the purpose of the invention, the invention provides a low-oil-permeability heat-conducting silica gel gasket which comprises the following components in parts by weight:
the weight percentage of vinyl in the vinyl silicone oil is 0.1-0.4%, and the viscosity of the vinyl silicone oil is 1000-100000mPa & s.
The hydrogen content of the hydrogen-containing silicone oil is 0.1-0.5 wt%.
The inhibitor is an acetylenic ketone inhibitor.
The catalyst is a vinyl-coordinated platinum catalyst.
The alumina is prepared by grading alumina with the particle size distribution of 0.2-300 microns.
The invention also provides a preparation method of the low-oil-permeability heat-conduction silica gel gasket, which comprises the following steps:
a. placing the vinyl silicone oil, the hydrogen-containing silicone oil and the inhibitor in parts by weight in a stirring device with the rotating speed of 60-120 revolutions per minute, and stirring for 10-50 minutes;
b. adding the aluminum oxide in parts by weight into a stirring device, adjusting the rotating speed to be 30-60 revolutions per minute, continuously stirring for 0.5-2 hours, adding the catalyst in parts by weight, stirring for 10-40 minutes at the rotating speed of 30-60 revolutions per minute, and vacuumizing to obtain a heat-conducting silica gel sizing material;
c. and c, rolling the heat-conducting silica gel material obtained in the step b into a sheet with the thickness of 1-5 mm, curing the sheet at the temperature of 100-150 ℃ for 5-30 minutes, and cutting the sheet into required sizes to obtain the low-oil-permeability heat-conducting silica gel gasket.
Preferably, in the step c, the heat-conducting silica gel material obtained in the step b is rolled into a sheet with the thickness of 2 mm, cured at the temperature of 120 ℃ for 10 minutes, and cut into the required size, so as to obtain the low-oil-permeability heat-conducting silica gel gasket.
The invention has the beneficial effects that: according to the invention, the crosslinking degree of the sizing material is regulated and controlled by adjusting the proper silicon-hydrogen ratio, so that the sizing material can fully react, the reactants remained completely due to non-reaction are reduced, the heat-conducting silicone grease gasket with low oil permeability is prepared, the prepared heat-conducting silicone grease gasket has low weight loss rate through aging test, the oil permeability phenomenon is not generated, and the heat-conducting performance is stable.
[ detailed description ] embodiments
The following examples are further illustrative and supplementary to the present invention and do not limit the present invention in any way.
Example 1
Adding 100 g of vinyl silicone oil, 4 g of hydrogen-containing silicone oil and 0.01 g of inhibitor into a stirring kettle with the rotation speed of 60 revolutions per minute, stirring for 30 minutes, then adding 700 g of alumina into the stirring kettle, stirring for 1 hour at the rotation speed of 30 revolutions per minute, then adding 0.2 g of catalyst into the stirring kettle, stirring for 20 minutes at the rotation speed of 60 revolutions per minute, and simultaneously vacuumizing to obtain the heat-conducting silica gel material.
The prepared heat-conducting silica gel sizing material is rolled into a sheet with the thickness of 2 mm, the sheet is cured for 10 minutes at the temperature of 120 ℃, then the sheet is cut into a target size to obtain a low-oil-permeability heat-conducting silica gel gasket, the heat conductivity coefficient of the heat-conducting silica gel gasket is tested by ASTM D5470, the heat-conducting silica gel gasket is used at the temperature of 150 ℃ for 240 hours, and the aging weight loss rate is tested, and the test results are shown in Table 1.
Example 2
Adding 100 g of vinyl silicone oil, 8 g of hydrogen-containing silicone oil and 0.01 g of inhibitor into a stirring kettle with the rotation speed of 120 revolutions per minute, stirring for 30 minutes, then adding 900 g of alumina into the stirring kettle, stirring for 1 hour at the rotation speed of 60 revolutions per minute, then adding 0.2 g of catalyst into the stirring kettle, stirring for 20 minutes at the rotation speed of 30 revolutions per minute, and simultaneously vacuumizing to obtain the heat-conducting silica gel material.
The prepared heat-conducting silica gel sizing material is rolled into a sheet with the thickness of 2 mm, the sheet is cured for 10 minutes at the temperature of 120 ℃, then the sheet is cut into a target size to obtain a low-oil-permeability heat-conducting silica gel gasket, the heat conductivity coefficient of the heat-conducting silica gel gasket is tested by ASTM D5470, the heat-conducting silica gel gasket is used at the temperature of 150 ℃ for 240 hours, and the aging weight loss rate is tested, and the test results are shown in Table 1.
Example 3
Adding 100 g of vinyl silicone oil, 10 g of hydrogen-containing silicone oil and 0.01 g of inhibitor into a stirring kettle with the rotation speed of 100 revolutions per minute, stirring for 10 minutes, then adding 1200 g of alumina into the stirring kettle, stirring for 0.5 hour at the rotation speed of 45 revolutions per minute, then adding 0.1 g of catalyst into the stirring kettle, stirring for 40 minutes at the rotation speed of 45 revolutions per minute, and simultaneously vacuumizing to obtain the heat-conducting silica gel material.
The prepared heat-conducting silica gel rubber material is rolled into a sheet with the thickness of 2 mm, is cured for 5 minutes at the temperature of 150 ℃, is cut into a target size to obtain a low-oil-permeability heat-conducting silica gel gasket, is used for testing the heat conductivity coefficient of the heat-conducting silica gel gasket by ASTM D5470 and is used for testing the aging weight loss rate for 240 hours at the temperature of 150 ℃, and the test results are shown in Table 1.
Example 4
Adding 100 g of vinyl silicone oil, 1 g of hydrogen-containing silicone oil and 0.01 g of inhibitor into a stirring kettle with the rotation speed of 80 revolutions per minute, stirring for 50 minutes, then adding 700 g of alumina into the stirring kettle, stirring for 2 hours at the rotation speed of 40 revolutions per minute, then adding 0.1 g of catalyst into the stirring kettle, stirring for 10 minutes at the rotation speed of 40 revolutions per minute, and simultaneously vacuumizing to obtain the heat-conducting silica gel material.
The prepared heat-conducting silica gel rubber material is rolled into a sheet with the thickness of 2 mm, the sheet is cured for 30 minutes at the temperature of 100 ℃, then the sheet is cut into a target size to obtain a low-oil-permeability heat-conducting silica gel gasket, the heat conductivity coefficient of the heat-conducting silica gel gasket is tested by ASTM D5470, the heat-conducting silica gel gasket is used at the temperature of 150 ℃ for 240 hours, and the aging weight loss rate is tested, and the test results are shown in Table 1.
Comparative example 1
Adding 100 g of vinyl silicone oil, 0.5 g of hydrogen-containing silicone oil and 0.01 g of inhibitor into a stirring kettle at the rotation speed of 80 revolutions per minute, stirring for 50 minutes, then adding 700 g of alumina into the stirring kettle, stirring for 2 hours at the rotation speed of 40 revolutions per minute, then adding 0.1 g of catalyst into the stirring kettle, stirring for 10 minutes at the rotation speed of 40 revolutions per minute, and simultaneously vacuumizing to obtain the heat-conducting silica gel material.
The prepared heat-conducting silica gel rubber material is rolled into a sheet with the thickness of 2 mm, the sheet is cured for 30 minutes at the temperature of 100 ℃, then the sheet is cut into a target size to obtain a low-oil-permeability heat-conducting silica gel gasket, the heat conductivity coefficient of the heat-conducting silica gel gasket is tested by ASTM D5470, the heat-conducting silica gel gasket is used at the temperature of 150 ℃ for 240 hours, and the aging weight loss rate is tested, and the test results are shown in Table 1.
Table 1 test results of low-permeability oil heat-conductive silicone gasket
As can be seen from table 1, the measurement results of the comparative examples and comparative examples show that the low-oil-permeability heat-conductive silicone gasket of the present invention has small change in heat conductivity coefficient before and after aging test, stable heat conductivity, low weight loss rate, and no occurrence of silicone oil exudation.
Although the present invention has been disclosed by the above embodiments, the protection scope of the present invention is not limited thereto, and several deductions, substitutions and the like of the above components are made within the scope of the claims of the present invention without departing from the concept of the present invention.
Claims (5)
1. The low-permeability oil heat-conducting silica gel gasket is characterized by comprising the following components in parts by weight:
vinyl silicone oil 100 parts
Hydrogen-containing silicone oil 4 parts
0.01 portion of inhibitor
Catalyst 0.2 part
700 parts of aluminum oxide;
wherein the weight percentage of hydrogen in the hydrogen-containing silicone oil is 0.1-0.5%; the heat-conducting alumina filler is prepared by grading alumina with the particle size distribution of 0.2-300 microns;
wherein the manufacturing process of the low-permeability oil heat-conducting silica gel gasket comprises the following steps:
adding 100 g of vinyl silicone oil, 4 g of hydrogen-containing silicone oil and 0.01 g of inhibitor into a stirring kettle at the rotating speed of 60 revolutions per minute, stirring for 30 minutes, then adding 700 g of alumina into the stirring kettle, stirring for 1 hour at the rotating speed of 30 revolutions per minute, then adding 0.2 g of catalyst into the stirring kettle, stirring for 20 minutes at the rotating speed of 60 revolutions per minute, and simultaneously vacuumizing to obtain a heat-conducting silica gel material;
and rolling the prepared heat-conducting silica gel glue stock into a sheet with the thickness of 2 mm, curing the sheet at the temperature of 120 ℃ for 10 minutes, and cutting the sheet into a target size to obtain the low-oil-permeability heat-conducting silica gel gasket.
2. The low-oil-permeability heat-conductive silicone gasket as claimed in claim 1, wherein the vinyl silicone oil contains 0.1-0.4% by weight of vinyl groups, and the viscosity of the vinyl silicone oil is 1000-.
3. The low-permeability oil-conducting silicone gasket as claimed in claim 1, wherein the inhibitor is an alkynol inhibitor.
4. The oil-permeable, heat-conductive silicone gasket of claim 1, wherein said catalyst is a vinyl-coordinated platinum catalyst.
5. A method of making the low oil permeability, thermally conductive silicone gasket of claim 1, comprising the steps of:
a. placing the vinyl silicone oil, the hydrogen-containing silicone oil and the inhibitor in parts by weight in a stirring device with the rotating speed of 60 revolutions per minute and stirring for 30 minutes;
b. adding the aluminum oxide in parts by weight into a stirring device, adjusting the rotating speed to be 30 revolutions per minute, continuously stirring for 1 hour, adding the catalyst in parts by weight, stirring for 20 minutes at the rotating speed of 60 revolutions per minute, and vacuumizing to obtain a heat-conducting silica gel sizing material;
c. and c, rolling the heat-conducting silica gel material obtained in the step b into a sheet with the thickness of 2 mm, curing the sheet at the temperature of 120 ℃ for 10 minutes, and cutting the sheet to obtain the low-oil-permeability heat-conducting silica gel gasket.
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| CN110982278A (en) * | 2019-12-24 | 2020-04-10 | 深圳德邦界面材料有限公司 | Low-volatilization heat-conducting gasket and preparation method thereof |
| CN114276688A (en) * | 2021-12-31 | 2022-04-05 | 四川天邑康和通信股份有限公司 | Flame-retardant high-elasticity heat-conducting gasket and preparation method thereof |
| CN114369369A (en) * | 2022-01-24 | 2022-04-19 | 福建美庆热传科技有限公司 | Low-volatility and low-oil-permeability heat conduction gasket and preparation method thereof |
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