CN116535863A - Heat-conducting silica gel and preparation method thereof - Google Patents
Heat-conducting silica gel and preparation method thereof Download PDFInfo
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Abstract
The invention provides a heat-conducting silica gel and a preparation method thereof, and relates to the technical field of heat-conducting materials. The method comprises the following steps: uniformly mixing vinyl silicone oil and a catalyst, adding hydrogen-containing silicone oil at the end, uniformly mixing, heating, adding various side hydrogen-containing silicone oils with different viscosities, and reacting to obtain matrix silicone resin; and adding a coupling agent into the matrix silicone resin, adding a heat-conducting filler, uniformly stirring, and vacuumizing to remove bubbles to obtain the heat-conducting silicone gel. The heat-conducting silica gel disclosed by the invention can not only avoid overlarge oil output, but also ensure that the silica gel has higher extrusion speed and extrusion quantity and ensure sizing speed.
Description
Technical Field
The invention relates to the technical field of heat conduction materials, in particular to a heat conduction silica gel and a preparation method thereof.
Background
Along with the rapid development of electronic components, the power is continuously increased, the requirement for heat dissipation is also continuously increased, and in order to ensure the normal operation of the devices, heat dissipation fins are generally arranged on the devices to remove redundant heat so as to maintain the working temperature of the devices. However, a gap inevitably occurs between the device and the heat sink, and the air in the gap blocks heat dissipation, so that the interface thermal resistance is increased, and the heat dissipation effect of the device is affected.
Most of the existing heat-conducting silica gel is a single-component pre-cured product, and the sizing flow rate is relatively low. The single-component high-heat-conductivity silicone gel which is cured after on-site sizing has higher sizing speed and higher reliability, but in order to ensure a certain sizing speed, namely a high extrusion rate, the gel itself is required to have lower viscosity. In the prior art, the low-viscosity matrix silicone resin and the heat-conducting filler with large particle size are used for compounding, but the low-molecular silicone oil is easy to phase separate in the long-time storage process, and is easy to exude and adsorb on a device after sizing or in the use process, so that the device is polluted, thereby causing the functional failure of part of the device and seriously influencing the service life of the device.
Disclosure of Invention
The invention aims to solve the problems that the existing single-component heat-conducting silicone gel adopts low-viscosity small molecular silicone oil as a matrix for meeting certain sizing speed, and fills large-particle-size heat-conducting filler to meet the heat-conducting property of the gel, but the silicone oil is easy to exude to pollute devices, thereby causing the function failure of the devices and the like.
In order to solve the above problems, the present invention provides a method for preparing a thermally conductive silicone gel, comprising:
uniformly mixing vinyl silicone oil and a catalyst, adding hydrogen-containing silicone oil at the end, uniformly mixing, heating, adding various side hydrogen-containing silicone oils with different viscosities, and reacting to obtain matrix silicone resin;
and adding a coupling agent into the matrix silicone resin, adding a heat-conducting filler, uniformly stirring, and vacuumizing to remove bubbles to obtain the heat-conducting silicone gel.
Preferably, the side hydrogen silicone oil comprises a first side hydrogen silicone oil with the viscosity of 100-600cp and a second side hydrogen silicone oil with the viscosity of 50-200cp; the addition sequence of the side hydrogen silicone oil is as follows: the side hydrogen silicone oil is added sequentially from the high viscosity to the low viscosity.
Preferably, the viscosity of the vinyl silicone oil is 30-200cp.
Preferably, the viscosity of the hydrogen-terminated silicone oil is 30-80cp.
Preferably, the heat conducting filler comprises fillers with the particle sizes of 80-100 mu m, 30-50 mu m, 0.5-1.5 mu m and 3-6 mu m, wherein the fillers with the particle sizes of 80-100 mu m account for 40-59% of the total amount of the heat conducting filler, the fillers with the particle sizes of 30-50 mu m account for 8-12% of the total amount of the heat conducting filler, the fillers with the particle sizes of 0.5-1.5 mu m account for 13-30% of the total amount of the heat conducting filler, and the fillers with the particle sizes of 3-6 mu m account for 14-35% of the total amount of the heat conducting filler.
Preferably, the heat conductive filler includes zinc oxide having particle diameters of 1 μm and 5 μm, and aluminum oxide having particle diameters of 1 μm, 5 μm, 40 μm and 90 μm.
Preferably, the content of each component is as follows in parts by weight: 3-5% of vinyl silicone oil, 0.07-0.2% of catalyst, 0.1-0.5% of terminal hydrogen silicone oil, 0.2-0.4% of first side hydrogen silicone oil, 0.5-1.5% of second side hydrogen silicone oil, 0.05-0.3% of coupling agent and 93-96% of heat conducting filler.
Preferably, the heating treatment is carried out under such conditions that the temperature is raised to 100-110 ℃ and the mixture is stirred for 1-1.5 hours.
Preferably, the coupling agent comprises triethylsilane, the catalyst is a latent catalyst prepared from vinyl silicone oil and a platinum catalyst, and the platinum content in the catalyst is 1000ppm.
The invention also provides a heat-conducting silica gel, which is prepared by adopting the preparation method of the heat-conducting silica gel.
Compared with the prior art, the preparation method of the heat-conducting silica gel has the advantages that:
according to the invention, through the cross-linking design among hydrogen-containing silicone oils with different structures and the control of the addition sequence of the hydrogen-containing silicone oils at the end and the hydrogen-containing silicone oils at the side, the hydrogen-containing silicone oils at the end are added first and then the hydrogen-containing silicone oils at the side are added to control the structure of the silicone resin, so that the matrix silicone resin with a dendritic structure is obtained, the low viscosity state of the silicone resin before solidification can be kept, the extrusion speed is ensured, meanwhile, the degree of concentration of cross-linking points is reduced by increasing the cross-linking degree of the solidified resin, so that silicone oil molecular chains are dendritic, the molecular chain distribution is more tortuous, the oil permeability is reduced, the low hardness of the matrix silicone resin is kept, and the heat-conducting silicone gel can avoid the excessive oil yield, ensure the high extrusion speed and extrusion quantity of the silicone gel, and ensure the sizing speed.
The advantages of the thermally conductive silicone gel of the present invention compared to the prior art are the same as those of the preparation method thereof compared to the prior art, and are not described in detail herein.
Drawings
Fig. 1 is a flowchart of a preparation method of a heat-conducting silicone gel according to an embodiment of the invention.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
The heat conduction silica gel comprises double-component heat conduction silica gel and single-component heat conduction silica gel, and the double-component heat conduction silica gel has heat absorption and heat release phenomena during solidification, so that the solidification shrinkage rate is high, and the bonding performance is poor. The single-component heat-conducting silica gel belongs to room-temperature-curing organic silicon rubber, takes organic silicon as a main body, is filled with high polymer materials such as heat-conducting materials, does not absorb heat or release heat during curing, has small shrinkage rate after curing, and has good adhesiveness to the materials. However, the single-component heat-conducting silica gel has higher heat resistance, the heat-conducting property is to be improved, and certain gluing speed is required to be ensured. Therefore, in the prior art, low viscosity silicones are generally selected as the matrix to ensure a high extrusion rate, thereby achieving a certain sizing speed. Meanwhile, a heat conducting filler with large particle size is selected to improve the heat conducting effect. However, the base material of the thermal conductive silica gel is organic silicon, and the thermal conductive silica gel is in a high-temperature environment for a long time, and the organic silicon is easy to generate low molecules such as siloxane and the like under the influence of high temperature, namely silicone oil, so that the phenomenon of oil seepage occurs.
In order to solve the above problems, as shown in fig. 1, an embodiment of the present invention provides a method for preparing a thermally conductive silicone gel, including:
uniformly mixing vinyl silicone oil and a catalyst, adding hydrogen-containing silicone oil at the end, uniformly mixing, heating, adding various side hydrogen-containing silicone oils with different viscosities, and reacting to obtain matrix silicone resin;
and adding a coupling agent into the matrix silicone resin, adding a heat-conducting filler, uniformly stirring, and vacuumizing to remove bubbles to obtain the heat-conducting silicone gel.
The present embodiment crosslinks vinyl silicone oils with a variety of hydrogen-containing silicone oils of different structures, wherein the hydrogen-containing silicone oils include terminal hydrogen-containing silicone oils and side hydrogen-containing silicone oils, and the side hydrogen-containing silicone oils include side hydrogen-containing silicone oils having different viscosities. Because the silicon-hydrogen bond (Si-H) contained in the silicone oil molecule is relatively active and is easy to generate a crosslinking reaction, the position of the silicon-hydrogen bond is changed by adding the terminal hydrogen-containing silicone oil and the side hydrogen-containing silicone oil, so that the position where the crosslinking reaction occurs is changed, the terminal hydrogen-containing addition is equivalent to the growth of a vinyl silicone oil chain and is similar to a trunk, and the side hydrogen-containing addition is equivalent to the branching of the vinyl silicone oil chain and is similar to a branch; the fundamental reasons for the different viscosities of the silicone oils are that the silicone oils have different molecular weights, molecular chain lengths and the like, so that the structures of the side hydrogen-containing silicone oils are also various, and therefore, in this embodiment, vinyl silicone oils with single viscosities are crosslinked with various hydrogen-containing silicone oils with different structures to obtain the matrix silicone resin with a dendritic structure. Illustratively, the structural formula of the side hydrogen silicone oil is as follows:
the structural formula of the terminal hydrogen-containing silicone oil is shown as follows:
wherein m, n is an integer greater than 0.
According to the embodiment, through the cross-linking design among hydrogen-containing silicone oils with different structures and the control of the addition sequence of the hydrogen-containing silicone oils at the end and the hydrogen-containing silicone oils at the side, the hydrogen-containing silicone oils at the end are added first and then the hydrogen-containing silicone oils at the side are added to control the structure of the silicone resin, so that the matrix silicone resin with a dendritic structure is obtained, on one hand, the low viscosity state of the silicone resin before solidification can be kept to ensure the extrusion speed, and on the other hand, the concentration degree of cross-linking points is reduced by increasing the cross-linking degree of the cured resin, so that the silicone oil molecular chains are dendritic, the molecular chain distribution is more tortuous, the oil permeability is reduced, the low hardness of the matrix silicone resin is kept, namely, the oil yield of the dendritic silicone resin is lower, and the cross-linking density is low due to the reduction of the concentration degree of the cross-linking points, so that the matrix silicone resin has good flexibility.
Compared with the condition that most single-component heat-conducting silica gel in the prior art is extremely easy to cause oil seepage by using vinyl silicone oil with single viscosity, in the embodiment, the vinyl silicone oil is crosslinked with hydrogen-containing silicone oil with different structures including terminal hydrogen-containing silicone oil, side hydrogen-containing silicone oil and the like to obtain a crosslinked structure with a dendritic structure, the terminal hydrogen-containing silicone oil is equal to a trunk, and is added firstly, the side hydrogen-containing silicone oil is equal to a branch, and is added later, so that the heat-conducting silica gel of the embodiment can avoid overlarge oil output, ensure that the silica gel has higher extrusion speed and extrusion quantity, and ensure the sizing speed.
In some embodiments, the multiple side hydrogen-containing silicone oils with different viscosities are added in order from large to small in viscosity, namely, the side hydrogen-containing silicone oil with larger molecular chain length is added first, and then the side hydrogen-containing silicone oil with smaller molecular chain length is added, so that the side hydrogen-containing silicone oils with different chain lengths are crosslinked again on the basis that the end hydrogen-containing silicone oil forms a backbone structure, and a dendritic crosslinked structure is formed.
In a preferred example, the side hydrogen silicone oil includes a first side hydrogen silicone oil having a viscosity of 100 to 600cp and a second side hydrogen silicone oil having a viscosity of 50 to 200cp; the viscosity of the vinyl silicone oil is 50-200cp; the viscosity of the hydrogen-containing silicone oil at the end is 30-80cp.
The addition sequence of the side hydrogen silicone oil is as follows: the viscosity of the side hydrogen silicone oil is added sequentially from large to small. In this embodiment, adding the side hydrogen silicone oil sequentially according to the order of the viscosity of the side hydrogen silicone oil includes: and adding the first side hydrogen-containing silicone oil and the second side hydrogen-containing silicone oil in sequence.
Further, the viscosity of the vinyl silicone oil is preferably 50cp, the viscosity of the terminal hydrogen silicone oil is preferably 30cp, the viscosity of the first side hydrogen silicone oil is preferably 500cp, and the viscosity of the second side hydrogen silicone oil is preferably 100cp.
In this example, vinyl silicone oil having a viscosity of 50cp was used, and three kinds of hydrogen-containing silicone oils, side chain hydrogen-containing silicone oil having a viscosity of 500cp and 100cp, and terminal hydrogen-containing silicone oil having a viscosity of 30cp were used, respectively. Through selecting the basic silicone oil (vinyl silicone oil) and the hydrogen-containing silicone oil with the structures, and controlling the adding sequence to add the hydrogen-containing silicone oil at the end into the basic silicone oil, the hydrogen-containing silicone oil at the end is subjected to cross-linking reaction with the basic silicone oil preferentially, and then the side hydrogen-containing silicone oil with larger chain length and smaller chain length is sequentially added, so that a 'small crotch' is further formed on a cross-linked structure forming a backbone structure, and finally, the dendritic structural matrix silicone resin is obtained, the matrix silicone resin can be kept to have lower hardness, so that extrusion is convenient, the sizing speed is kept, and meanwhile, the heat conducting filler is filled in the dendritic cross-linked structure, so that the heat conducting filler is uniformly distributed, and the silicon gel is ensured to have higher heat conductivity.
In some embodiments, the hydrogen content of the first side hydrogen silicone oil is preferably 0.5mmol/g and the hydrogen content of the second side hydrogen silicone oil is preferably 1.0mmol/g.
The hydrogen-containing silicone oil with the hydrogen content is selected, so that the basic silicone oil and the hydrogen-containing silicone oil can be subjected to sufficient crosslinking reaction, and meanwhile, the hydrogen content can not cause too dense crosslinking points, so that the heat-conducting silicone gel is ensured to have higher adhesive force.
In some embodiments, the heat conductive filler comprises a filler having a particle size of 80-100 μm, 30-50 μm, 0.5-1.5 μm,3-6 μm, wherein the filler having a particle size of 80-100 μm is 40-59% of the total amount of the heat conductive filler, the filler having a particle size of 30-50 μm is 8-12% of the total amount of the heat conductive filler, the filler having a particle size of 0.5-1.5 μm is 13-30% of the total amount of the heat conductive filler, and the filler having a particle size of 3-6 μm is 14-35% of the total amount of the heat conductive filler. In this example, the particle size of the filler means an average particle size.
When the same proportion of heat conducting filler is filled, the larger the particle size of the filler is, the higher the heat conductivity coefficient is, the higher the extrusion rate is, but the more serious the oil is discharged, while the smaller the particle size of the filler is, although the oil is less, the lower the heat conductivity coefficient is, the heat conducting performance is affected, the lower the extrusion speed is, and the sizing speed is also affected. Therefore, in this embodiment, filler powder with different particle sizes is used as the heat-conducting filler, the oil absorption value of the colloid is increased by using the filler with small particle sizes, the potentially-extravasated oil is locked, and the colloid is ensured to have a certain flow speed and heat conductivity coefficient by using the filler with large particle sizes, so that the heat-conducting gel is ensured to have a higher heat conductivity coefficient, a good extrusion rate and a small oil seepage rate. Specifically, the filler with the particle size of 80-100 mu m accounts for 40-59% of the total amount of the heat conducting filler, the filler with the particle size of 30-50 mu m accounts for 8-12% of the total amount of the heat conducting filler, the filler with the particle size of 0.5-1.5 mu m accounts for 13-30% of the total amount of the heat conducting filler, and the filler with the particle size of 3-6 mu m accounts for 14-35% of the total amount of the heat conducting filler.
In a preferred embodiment, the large particle size filler is 90 μm filler, the medium particle size filler is 40 μm filler, and the fine filler is preferably 1-5 μm filler, wherein 0.5-1.5 μm filler is preferably 1 μm filler and 3-6 μm filler is preferably 5 μm filler.
Wherein, small particles such as 1-5 mu m can be used for filling gaps among particles with large particle size, can be used as a ball effect during gel extrusion, is helpful for the fluidity of the gel under certain conditions, and the powder with small particle size can improve the oil yield of the gel; the particles with the particle size of 30-50 mu m are selected for powder grading, small-particle-size powder and large-particle-size powder are matched to finish the close packing of the powder, and the filling quantity is increased, so that the heat conductivity coefficient is improved; the powder with the particle size of 80-100 mu m is selected to improve the overall heat conducting property and the extrusion rate.
In some specific embodiments, the thermally conductive filler comprises zinc oxide having particle sizes of 1 μm and 5 μm, and aluminum oxide having particle sizes of 1 μm, 5 μm, 40 μm, and 90 μm.
In the embodiment, two heat conducting fillers of zinc oxide and aluminum oxide are selected, wherein the zinc oxide comprises two types, the particle sizes are respectively 1 mu m and 5 mu m, and the purities are more than or equal to 99 percent. The alumina is spherical alumina, and comprises four particle sizes of 1 mu m, 5 mu m, 40 mu m and 90 mu m, and the purity is more than or equal to 99 percent. In the embodiment, the oil absorption value of the colloid is increased through the zinc oxide and the aluminum oxide with small particle sizes, so that the possibly-extravasated oil is locked, and meanwhile, the spherical aluminum oxide with large particle sizes with a certain proportion is added to ensure a certain flowing speed of the colloid and the heat conductivity coefficient of the heat conducting gel.
In some embodiments, the thermal conductive filler is filled in a proportion of 93-96%. The filling proportion of the heat-conducting filler refers to the proportion of the heat filler in the whole body, and the whole body comprises base silicone oil, hydrogen-containing silicone oil, a catalyst, a coupling agent and the heat-conducting filler. By setting the filling proportion of the heat conducting filler in the above range, the prepared heat conducting gel not only has higher heat conducting property, but also can ensure certain extrusion speed and has good sizing speed.
In some specific embodiments, the thermally conductive silicone gel comprises the following components in parts by weight: 3-5% of vinyl silicone oil, 0.07-0.2% of catalyst, 0.1-0.5% of terminal hydrogen silicone oil, 0.2-0.4% of first side hydrogen silicone oil, 0.5-1.5% of second side hydrogen silicone oil, 0.05-0.3% of coupling agent and 93-96% of heat conducting filler. Wherein in the heat conducting filler, the filler with the particle size of 80-100 mu m accounts for 40-59% of the total amount of the heat conducting filler, the filler with the particle size of 30-50 mu m accounts for 8-12% of the total amount of the heat conducting filler, the filler with the particle size of 0.5-1.5 mu m accounts for 13-30% of the total amount of the heat conducting filler, and the filler with the particle size of 3-6 mu m accounts for 14-35% of the total amount of the heat conducting filler.
In some embodiments, the coupling agent comprises triethylsilane and the catalyst comprises a platinum catalyst. The heating treatment is carried out under the condition of heating to 100-110 ℃ and stirring for 1-1.5h.
In some embodiments, the method for preparing the thermally conductive silicone gel comprises the steps of:
uniformly mixing 5-5.5 parts by weight of vinyl silicone oil and 0.1 part by weight of catalyst, adding 0.2-0.4 part by weight of hydrogen-containing silicone oil at the end, uniformly mixing, heating to 100-110 ℃ and stirring for 1-1.5h, sequentially adding 0.4-0.6 part by weight of hydrogen-containing silicone oil at the first side with the viscosity of 500cp and 1.0-1.5 parts by weight of hydrogen-containing silicone oil at the second side with the viscosity of 100cp, and continuously heating and stirring for 1-1.5h to obtain matrix silicone resin;
0.1 part of coupling agent and 136 parts of heat conducting filler are added into the matrix silicone resin, wherein the specific steps are as follows: firstly adding 45 parts of zinc oxide with average particle size of 1 mu m and 5 mu m and aluminum oxide with average particle size of 1 mu m and 5 mu m, vacuumizing and stirring for 30min, then adding 10-15 parts of aluminum oxide with average particle size of 40 mu m, stirring for 20min, then adding 100 parts of aluminum oxide with average particle size of 90 mu m, uniformly stirring, vacuumizing and removing bubbles to obtain the heat-conducting silica gel.
The embodiment of the invention also provides the heat-conducting silica gel, which is prepared by adopting the preparation method of the heat-conducting silica gel.
The heat-conducting silica gel prepared by the method has oil seepage lower than 1mm, extrusion rate higher than 70g/min and hardness lower than 70 Shore hardness after solidification, namely hardness tested by Shore OO (high-precision digital display Shore hardness tester), which is also called Shore hardness.
The oil seepage test method is that 1mL of uncured gel is taken and placed on A4 paper, and a transparent PET film is used for pressing into a cake shape with the thickness of 1 mm. Standing at room temperature for 2 hours, baking at 100deg.C for 12 hours, and sucking free silicone oil away from paper at high temperature. And judging the oil output by observing the distance between the oil ring and the original gel position.
The extrusion rate was measured by loading the gel into a standard 30ccEFD tube, extruding for 1min at 90psi and weighing the mass of gel extruded over 1 min.
The invention is further illustrated by the following specific examples and comparative examples. The raw materials used in the following examples were: vinyl silicone oil (viscosity 50 cp), three hydrogen-containing silicone oils (two side chains contain 500cp and 100cp hydrogen, one end contains 30cp hydrogen-containing silicone oil), and a catalyst (3500 ppm latent platinum catalyst); and (3) a heat conducting filler: zinc oxide is two types: purity is more than or equal to 99%, average grain diameter is 1 μm and 5 μm; spherical alumina four types: the purity is more than or equal to 99 percent, the average grain diameter is 1 mu m, 5 mu m, 40 mu m and 90 mu m, and the coupling agent is triethylsilane.
Example 1
Taking 5.2 parts of 50cp vinyl silicone oil and 0.1 part of platinum catalyst, uniformly mixing, adding 0.3 part of 30cp end hydrogen-containing silicone oil, uniformly mixing, heating to 100 ℃ and stirring for 1h. 0.5 part of side hydrogen silicone oil with 500cp and hydrogen content of 0.5mmol/g and 1.3 parts of side hydrogen silicone oil with 100cp and hydrogen content of 1.0mmol/g are added, and stirring is continued for 1h, so that the vinyl and the hydrogen silicone oil react completely.
0.1 part of triethylsilane was added to increase the affinity between the heat conductive powder and the silicone oil. 8 parts of 1 mu m zinc oxide, 20 parts of 5 mu m zinc oxide, 10 parts of 1 mu m aluminum oxide and 17 parts of 5 mu m aluminum oxide are added, the mixture is vacuumized and stirred for 30min, then 11 parts of 40 mu m aluminum oxide is added, the mixture is stirred for 20min, then 70 parts of 90 mu m aluminum oxide is added, and after uniform stirring, the mixture is vacuumized and bubble is removed, so that the heat-conducting silica gel is obtained.
The thermal conductive silicone gel prepared in this example was tested to have an extrusion rate of 75g/min, oil bleed <1mm, shore hardness 63, and thermal conductivity of 6.5W/m.K.
Example 2
Taking 5.2 parts of 50cp vinyl silicone oil and 0.1 part of platinum catalyst, uniformly mixing, adding 0.3 part of 30cp end hydrogen-containing silicone oil, uniformly mixing, heating to 100 ℃ and stirring for 1h. 0.5 part of side hydrogen silicone oil with 500cp and hydrogen content of 0.5mmol/g and 1.3 parts of side hydrogen silicone oil with 100cp and hydrogen content of 1.0mmol/g are added, and stirring is continued for 1h, so that the vinyl and the hydrogen silicone oil react completely.
0.1 part of triethylsilane was added to increase the affinity between the heat conductive powder and the silicone oil. 8 parts of 1 mu m zinc oxide, 12 parts of 1 mu m aluminum oxide and 40 parts of 5 mu m aluminum oxide are added, the mixture is vacuumized and stirred for 30min, 16 parts of 40 mu m aluminum oxide is added, the mixture is stirred for 20min, 60 parts of 90 mu m aluminum oxide is added, and the mixture is uniformly stirred, vacuumized and bubble-removed to obtain the heat-conducting silica gel.
The thermal conductive silicone gel prepared in this example was tested to have an extrusion rate of 71g/min, oil bleed <1mm, shore hardness 62, and thermal conductivity of 6.0W/m.K.
Example 3
Taking 5.2 parts of 50cp vinyl silicone oil and 0.1 part of platinum catalyst, uniformly mixing, adding 0.3 part of 30cp end hydrogen-containing silicone oil, uniformly mixing, heating to 100 ℃ and stirring for 1h. 0.5 part of side hydrogen silicone oil with 500cp and hydrogen content of 0.5mmol/g and 1.3 parts of side hydrogen silicone oil with 100cp and hydrogen content of 1.0mmol/g are added, and stirring is continued for 1h, so that the vinyl and the hydrogen silicone oil react completely.
0.1 part of triethylsilane was added to increase the affinity between the heat conductive powder and the silicone oil. 10 parts of 1 mu m zinc oxide, 20 parts of 1 mu m aluminum oxide and 30 parts of 5 mu m aluminum oxide are added, the mixture is vacuumized and stirred for 30min, 16 parts of 40 mu m aluminum oxide is added, the mixture is stirred for 20min, 60 parts of 90 mu m aluminum oxide is added, and the mixture is uniformly stirred, vacuumized and bubble-removed to obtain the heat-conducting silica gel.
The heat-conducting silicone gel prepared in this example was tested to have an extrusion rate of 70g/min, oil bleed <1mm, shore hardness 68, and a thermal conductivity of 6.2W/m.K.
Example 4
Taking 5.2 parts of 50cp vinyl silicone oil and 0.1 part of platinum catalyst, uniformly mixing, adding 0.3 part of 30cp end hydrogen-containing silicone oil, uniformly mixing, heating to 100 ℃ and stirring for 1h. 0.5 part of side hydrogen silicone oil with 500cp and hydrogen content of 0.5mmol/g and 1.3 parts of side hydrogen silicone oil with 100cp and hydrogen content of 1.0mmol/g are added, and stirring is continued for 1h, so that the vinyl and the hydrogen silicone oil react completely.
0.1 part of triethylsilane was added to increase the affinity between the heat conductive powder and the silicone oil. 10 parts of 0.7 mu m zinc oxide, 5 parts of 0.3 mu m aluminum oxide, 15 parts of 1 mu m aluminum oxide and 30 parts of 5 mu m aluminum oxide are added, the mixture is vacuumized and stirred for 30min, 16 parts of 40 mu m aluminum oxide is then added, the mixture is stirred for 20min, 60 parts of 90 mu m aluminum oxide is then added, and the mixture is uniformly stirred and vacuumized to remove bubbles, so that the heat-conducting silica gel is obtained.
The heat-conducting silicone gel prepared in the example was tested, and the extrusion rate was 80g/min, oil bleed <1mm, shore hardness 60, and thermal conductivity 6.3W/m.K.
Comparative example 1
Taking 5.2 parts of 50cp vinyl silicone oil and 0.1 part of platinum catalyst, uniformly mixing, adding 0.1 part of 30cp end hydrogen-containing silicone oil, uniformly mixing, heating to 100 ℃ and stirring for 1h. 0.6 part of side hydrogen silicone oil with 500cp and hydrogen content of 0.5mmol/g and 1.4 parts of side hydrogen silicone oil with 100cp and hydrogen content of 1.0mmol/g are added, and stirring is continued for 1h, so that the vinyl and the hydrogen silicone oil react completely.
0.1 part of triethylsilane was added to increase the affinity between the heat conductive powder and the silicone oil. 8 parts of 1 mu m zinc oxide, 12 parts of 1 mu m aluminum oxide and 40 parts of 5 mu m aluminum oxide are added, the mixture is vacuumized and stirred for 30min, 16 parts of 40 mu m aluminum oxide is added, the mixture is stirred for 20min, 60 parts of 90 mu m aluminum oxide is added, and the mixture is uniformly stirred, vacuumized and bubble-removed to obtain the heat-conducting silica gel.
The prepared heat-conducting silica gel is tested, and the extrusion rate is 35g/min, oil seepage is more than 1mm, the Shore hardness is 62, and the heat conductivity is 6.0W/m.K. The amount of side hydrogen silicone oil was increased and the amount of end hydrogen silicone oil was decreased compared to example 2, resulting in a sharp decrease in the extrusion amount.
Comparative example 2
Taking 5.2 parts of 50cp vinyl silicone oil and 0.1 part of platinum catalyst, uniformly mixing, adding 0.3 part of 30cp end hydrogen-containing silicone oil, uniformly mixing, heating to 100 ℃ and stirring for 1h. 0.5 part of side hydrogen silicone oil with 500cp and hydrogen content of 0.5mmol/g and 1.3 parts of side hydrogen silicone oil with 100cp and hydrogen content of 1.0mmol/g are added, and stirring is continued for 1h, so that the vinyl and the hydrogen silicone oil react completely.
0.1 part of triethylsilane was added to increase the affinity between the heat conductive powder and the silicone oil. 7 parts of 0.7 mu m zinc oxide, 5 parts of 0.3 mu m aluminum oxide, 8 parts of 1 mu m aluminum oxide and 20 parts of 5 mu m aluminum oxide are added, the mixture is vacuumized and stirred for 30min, 16 parts of 40 mu m aluminum oxide is then added, the mixture is stirred for 20min, 80 parts of 90 mu m aluminum oxide is then added, and the mixture is uniformly stirred and vacuumized to remove bubbles, so that the heat-conducting silica gel is obtained.
The prepared heat-conducting silica gel is tested, and the extrusion rate is 55g/min, oil seepage is more than 1mm, the Shore hardness is 55, and the heat conductivity is 6.7W/m.K. In this comparative example, too much coarse powder in the heat conductive filler, although the heat conductivity was increased, resulted in a lower extrusion rate and a larger amount of oil.
Comparative example 3
Taking 5.2 parts of 50cp vinyl silicone oil and 0.1 part of platinum catalyst, uniformly mixing, adding 0.3 part of 30cp end hydrogen-containing silicone oil, uniformly mixing, heating to 100 ℃ and stirring for 1h. 0.5 part of side hydrogen silicone oil with 500cp and hydrogen content of 0.5mmol/g and 1.3 parts of side hydrogen silicone oil with 100cp and hydrogen content of 1.0mmol/g are added, and stirring is continued for 1h, so that the vinyl and the hydrogen silicone oil react completely.
0.1 part of triethylsilane was added to increase the affinity between the heat conductive powder and the silicone oil. 15 parts of 0.7 mu m zinc oxide, 10 parts of 0.3 mu m aluminum oxide, 20 parts of 1 mu m aluminum oxide and 30 parts of 5 mu m aluminum oxide are added, the mixture is vacuumized and stirred for 30min, 16 parts of 40 mu m aluminum oxide is then added, the mixture is stirred for 20min, 45 parts of 90 mu m aluminum oxide is then added, and the mixture is uniformly stirred and vacuumized to remove bubbles, so that the heat-conducting silica gel is obtained.
The prepared heat-conducting silica gel is tested, and the extrusion rate is 40g/min, oil seepage is less than 1mm, the Shore hardness is 64, and the heat conductivity is 5.8W/m.K. In this comparative example, the heat conductive filler had less coarse powder and too much fine powder, and although the oil permeation amount was low, the heat conductivity was also low, and the extrusion rate was drastically lowered.
Comparative example 4
Taking 5.0 parts of 50cp vinyl silicone oil and 0.1 part of platinum catalyst, uniformly mixing, adding 0.5 part of 30cp end hydrogen-containing silicone oil, uniformly mixing, heating to 100 ℃ and stirring for 1h. 0.2 part of side hydrogen silicone oil with 500cp and hydrogen content of 0.5mmol/g and 1.3 parts of side hydrogen silicone oil with 100cp and hydrogen content of 1.0mmol/g are added, and stirring is continued for 1h, so that the vinyl and the hydrogen silicone oil react completely.
0.1 part of triethylsilane was added to increase the affinity between the heat conductive powder and the silicone oil. 8 parts of 1 mu m zinc oxide, 12 parts of 1 mu m aluminum oxide and 40 parts of 5 mu m aluminum oxide are added, the mixture is vacuumized and stirred for 30min, 16 parts of 40 mu m aluminum oxide is added, the mixture is stirred for 20min, 60 parts of 90 mu m aluminum oxide is added, and the mixture is uniformly stirred, vacuumized and bubble-removed to obtain the heat-conducting silica gel.
The prepared heat-conducting silica gel is tested, and the extrusion rate is 45g/min, oil seepage is more than 1mm, the Shore hardness is 62, and the heat conductivity is 6.0W/m.K. In this comparative example, the terminal hydrogen silicone oil was added in a larger amount, resulting in a larger oil output.
Examples 1 to 4 and comparative examples 1 to 4 were prepared by using the raw materials and the amounts shown in tables 1 and 2, and the results of testing the thermally conductive silicone gel prepared therefrom are shown in table 3. The data in tables 1 and 2 are parts by weight.
Table 1:
table 2:
remarks: in the table "/" indicates no addition.
Table 3:
| extrusion rate | Oil seepage | Shore hardness | Thermal conductivity | |
| Example 1 | 75g/min | <1mm | 63 | 6.5W/m.K |
| Example 2 | 71g/min | <1mm | 62 | 6.0W/m.K |
| Example 3 | 70g/min | <1mm | 68 | 6.2W/m.K |
| Example 4 | 80g/min | <1mm | 60 | 6.3W/m.K |
| Comparative example 1 | 35g/min | ＞1mm | 62 | 6.0W/m.K |
| Comparative example 2 | 55g/min | ＞1mm | 55 | 6.7W/m.K |
| Comparative example 3 | 40g/min | <1mm | 64 | 5.8W/m.K |
| Comparative example 4 | 45g/min | ＞1mm | 62 | 6.0W/m.K |
From tables 1 and 3, it is understood that the proportions of the vinyl silicone oil, the terminal hydrogen silicone oil and the side hydrogen silicone oil should be controlled within a certain range to obtain a specific silicone resin dendritic structure. When the end hydrogen silicone oil is larger, the trunk is too long, which easily leads to larger oil output of the heat conduction silicone gel (comparative example 4), when the end hydrogen silicone oil is smaller, and the side hydrogen silicone oil is larger, the trunk is too short, and the branches are more, which easily leads to lower extrusion quantity under the same collocation of heat conduction filler powder (comparative example 1).
From tables 2 and 3, it is found that by incorporating zinc oxide and aluminum oxide particles having extremely small particle diameters (1 to 5 μm), silicone oil possibly exuding from the raw material is blocked, and by alumina particles having large particle diameters (. Gtoreq.70 μm), the heat conductive property and extrusion rate of the gel are ensured. However, too much or too little of the coarse powder and the fine powder in the heat conductive filler have disadvantages in terms of oil bleeding amount, extrusion rate, heat conductivity, etc., for example, too little of the coarse powder content and too much of the fine powder (comparative example 3) result in poor heat conductivity (5.8W/m.K) and also a significant decrease in extrusion rate (40 g/min). On the other hand, too much coarse powder content, for example, 90 μm alumina in comparative example 2, greatly increased, resulting in a lower extrusion rate and a larger oil yield.
In summary, according to the embodiment, through selecting vinyl silicone oil with proper viscosity and hydrogen-containing silicone oil with various structures, and according to the addition sequence of adding hydrogen-containing silicone oil at the end and then adding hydrogen-containing silicone oil at the side, the silicone resin with a dendritic structure is obtained under proper component content, so that the problem that silicone oil is easy to exude and the sizing speed cannot be balanced is solved, meanwhile, through grading of different particle sizes of the heat conducting filler, the finally obtained heat conducting silicone gel can balance various indexes such as heat conducting effect, extrusion rate and oil seepage amount, so that the heat conducting silicone gel has high heat conductivity, a certain extrusion rate can be ensured, and the oil yield is low.
Although the present disclosure is described above, the scope of protection of the present disclosure is not limited thereto. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the disclosure, and these changes and modifications will fall within the scope of the invention.
Claims (10)
1. A method for preparing a thermally conductive silicone gel, comprising:
uniformly mixing vinyl silicone oil and a catalyst, adding hydrogen-containing silicone oil at the end, uniformly mixing, heating, adding various side hydrogen-containing silicone oils with different viscosities, and reacting to obtain matrix silicone resin;
and adding a coupling agent into the matrix silicone resin, adding a heat-conducting filler, uniformly stirring, and vacuumizing to remove bubbles to obtain the heat-conducting silicone gel.
2. The method of preparing a thermally conductive silicone gel as set forth in claim 1, wherein said side hydrogen-containing silicone oil comprises a first side hydrogen-containing silicone oil having a viscosity of 100-600cp and a second side hydrogen-containing silicone oil having a viscosity of 50-200cp; the addition sequence of the side hydrogen silicone oil is as follows: the side hydrogen silicone oil is added sequentially from the high viscosity to the low viscosity.
3. The method for preparing a thermally conductive silicone gel as set forth in claim 2, wherein the vinyl silicone oil has a viscosity of 30 to 200cp.
4. The method for preparing a thermally conductive silicone gel according to claim 2, wherein the hydrogen-terminated silicone oil has a viscosity of 30 to 80cp.
5. The method for preparing a thermally conductive silicone gel according to claim 1, wherein the thermally conductive filler comprises a filler having a particle size of 80 to 100 μm, 30 to 50 μm, 0.5 to 1.5 μm,3 to 6 μm, wherein the filler having a particle size of 80 to 100 μm accounts for 40 to 59% of the total amount of the thermally conductive filler, the filler having a particle size of 30 to 50 μm accounts for 8 to 12% of the total amount of the thermally conductive filler, the filler having a particle size of 0.5 to 1.5 μm accounts for 13 to 30% of the total amount of the thermally conductive filler, and the filler having a particle size of 3 to 6 μm accounts for 14 to 35% of the total amount of the thermally conductive filler.
6. The method of preparing a thermally conductive silicone gel as set forth in claim 1, wherein the thermally conductive filler comprises zinc oxide having particle diameters of 1 μm and 5 μm, and aluminum oxide having particle diameters of 1 μm, 5 μm, 40 μm and 90 μm.
7. The method for preparing a thermally conductive silicone gel as set forth in claim 2, wherein the contents of the respective components in parts by weight are: 3-5% of vinyl silicone oil, 0.07-0.2% of catalyst, 0.1-0.5% of terminal hydrogen silicone oil, 0.2-0.4% of first side hydrogen silicone oil, 0.5-1.5% of second side hydrogen silicone oil, 0.05-0.3% of coupling agent and 93-96% of heat conducting filler.
8. The method for preparing a thermally conductive silicone gel as set forth in claim 1, wherein the heating treatment is performed under a condition of heating to 100 to 110 ℃ and stirring for 1 to 1.5 hours.
9. The method for preparing a thermally conductive silicone gel according to claim 1, wherein the coupling agent comprises triethylsilane, the catalyst is a latent catalyst prepared from vinyl silicone oil and a platinum catalyst, and the platinum content of the catalyst is 1000ppm.
10. A thermally conductive silicone gel prepared by the method of any one of claims 1 to 9.
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