CN110172249B - Heat-conducting silica gel sheet and preparation method and application thereof, heat-conducting heating silica gel sheet and preparation method and application thereof - Google Patents
Heat-conducting silica gel sheet and preparation method and application thereof, heat-conducting heating silica gel sheet and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the field of silica gel sheets, and particularly provides a heat-conducting silica gel sheet, a preparation method and application thereof, a heat-conducting heating silica gel sheet, a preparation method and application thereof. The heat-conducting silica gel sheet is prepared from the following raw materials in parts by mass: 10-100 parts of silicon rubber, 300-1900 parts of heat-conducting agent, 0.5-100 parts of flame retardant, 0.3-6 parts of reinforcing agent and 3-50 parts of cross-linking agent; the weight average molecular weight of the silicon rubber is 70-90 ten thousand. The heat-conducting silica gel sheet has the advantages of high heat conductivity coefficient, reasonable hardness and good high-temperature resistance, the heat conductivity coefficient can reach 1-5W/(m.K), the hardness Shore OO is 40-80, and the application range is wider.
Description
Technical Field
The invention relates to the field of silica gel sheets, in particular to a heat-conducting silica gel sheet, a preparation method and application thereof, a heat-conducting heating silica gel sheet, a preparation method and application thereof.
Background
The heat-conducting silica gel sheet is a heat-conducting medium material synthesized by a special process by taking silica gel as a base material and adding various auxiliary materials such as metal oxides and the like, is also called a heat-conducting silica gel pad, a heat-conducting silica gel sheet, a soft heat-conducting pad, a heat-conducting silica gel gasket and the like in the industry, is specially designed for transferring heat by utilizing a gap, is used for reducing contact thermal resistance generated between the surface of a heat source and a contact surface of a heat dissipation device, can fill the gap, completes heat transfer between a heating part and a heat dissipation part, simultaneously has the effects of insulation, shock absorption, sealing and the like, can meet the design requirements of miniaturization and ultra-thinness of equipment, has manufacturability and usability, and has wide thickness application range, and is particularly widely applied to electronic products.
The main heat conduction mechanism of the heat conduction silica gel sheet is carried out through heat conduction, and the heat conduction coefficient of the currently adopted heat conduction silica gel sheet is low, and the high temperature resistance and the hardness are poor, so that the application of the heat conduction silica gel sheet is limited.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a heat-conducting silica gel sheet, which has a high heat conductivity coefficient, good high-temperature resistance and reasonable hardness, wherein the heat conductivity coefficient can reach 1-5W/(m.K), and the application range is wider.
The second objective of the present invention is to provide a method for preparing the above heat conductive silica gel sheet.
The third purpose of the invention is to provide a heat-conducting heating silica gel sheet, which has the functions of heat conduction and heating, can meet the use requirements under different working conditions, and has a wider application range.
The fourth purpose of the invention is to provide a preparation method of the heat-conducting heating silica gel sheet.
The fifth objective of the present invention is to provide an application of the above heat conductive silicone sheet or the above heat conductive heating silicone sheet in an electronic product.
A sixth object of the present invention is to provide a semiconductor device, a relay, a circuit board, or a battery pack.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
in a first aspect, the invention provides a heat-conducting silica gel sheet which is mainly prepared from the following raw materials in parts by mass: 10-100 parts of silicon rubber, 300-1900 parts of heat-conducting agent, 0.5-100 parts of flame retardant, 0.3-6 parts of reinforcing agent and 3-50 parts of cross-linking agent; the weight average molecular weight of the silicone rubber is 70-90 ten thousand.
As a further preferred technical scheme, the heat-conducting silica gel sheet is mainly prepared from the following raw materials in parts by mass: 20-80 parts of silicon rubber, 500-1700 parts of heat-conducting agent, 10-80 parts of flame retardant, 1-6 parts of reinforcing agent and 5-45 parts of cross-linking agent;
preferably, the heat-conducting silica gel sheet is mainly prepared from the following raw materials in parts by mass: 35-70 parts of silicon rubber, 800-1500 parts of heat-conducting agent, 30-70 parts of flame retardant, 2-5 parts of reinforcing agent and 10-40 parts of cross-linking agent.
As a further preferable technical scheme, the weight average molecular weight of the silicon rubber is 70-85 ten thousand;
preferably, the heat conductive agent includes aluminum oxide and boron nitride;
preferably, the mass ratio of the aluminum oxide to the boron nitride is (10-15): (1-5), more preferably 12: (1-2);
preferably, the flame retardant comprises aluminium oxide and/or magnesium oxide;
preferably, the reinforcing agent comprises talc and/or titanium dioxide;
preferably, the cross-linking agent comprises bis-tetra and/or bis-di-penta;
preferably, the thickness of heat conduction silica gel piece is 0.5-2 mm.
In a second aspect, the invention provides a preparation method of the heat-conducting silica gel sheet, which comprises the following steps: and uniformly mixing the raw materials, and curing and forming to obtain the heat-conducting silica gel sheet.
As a further preferable technical solution, the curing molding includes pressure curing molding;
preferably, the curing molding pressure is more than 250kgfcm, and the curing molding time is 20-30 seconds;
preferably, the curing and molding temperature is 150-.
In a third aspect, the present invention provides a heat conducting heating silica gel sheet, including: the heating assembly and the heat-conducting silica gel sheet are arranged on at least one side of the heating assembly.
As a further preferred technical scheme, the heat-conducting silica gel sheets are respectively arranged on two sides of the heating component;
preferably, the heat generating component includes a metal material and/or a carbon material;
preferably, the metallic material comprises a pure metal or an alloy;
preferably, the pure metal comprises one of copper, aluminum, manganese or silver;
preferably, the alloy comprises at least one of nichrome, nichrome alloy, stainless steel, constantan resistance alloy, neoconstantan resistance alloy, or copper-manganese alloy;
preferably, the carbon material comprises carbon pulp and/or carbon fibers;
preferably, the thickness of the heat generating component is 0.03-0.5 mm.
In a fourth aspect, the invention provides a preparation method of the heat-conducting heating silica gel sheet, which comprises the following steps:
(a) uniformly mixing the raw materials of the heat-conducting silica gel sheet, and performing to obtain an uncured heat-conducting silica gel sheet;
(b) and arranging the uncured heat-conducting silica gel sheet on at least one side of the heating assembly, and curing and molding to obtain the heat-conducting heating silica gel sheet.
As a further preferable technical solution, the curing molding includes pressure curing molding;
preferably, the curing molding pressure is more than 250kgfcm, and the curing molding time is 20-30 seconds;
preferably, the curing molding temperature is 150-200 ℃.
In a fifth aspect, the invention provides an application of the heat conductive silicone sheet or the heat conductive heating silicone sheet in an electronic product.
In a sixth aspect, the invention provides a security video monitoring product, a semiconductor device, a relay, a circuit board or a battery pack, which includes the above heat-conducting silica gel sheet or the above heat-conducting heating silica gel sheet.
Compared with the prior art, the invention has the following beneficial effects:
the heat-conducting silica gel sheet provided by the invention is prepared from specific silicon rubber, a heat-conducting agent, a flame retardant, a reinforcing agent and a crosslinking agent with specific contents, wherein the silicon rubber is specific silicon rubber with the weight-average molecular weight of 70-90 ten thousand, the heat-conducting silica gel sheet has a scientific formula, the heat-conducting silica gel sheet has a high heat conductivity coefficient and good high-temperature resistance due to the cooperation of the silicon rubber, the heat-conducting adhesive and the flame retardant, the heat-conducting silica gel sheet has reasonable hardness due to the cooperation of the silicon rubber, the reinforcing agent and the crosslinking agent, the heat conductivity coefficient can reach 1-5W/(m.K), the hardness Shore OO is 40-80, the product stability is high, and the application range is wider.
The heat-conducting heating silica gel sheet provided by the invention has the functions of heat conduction and heating, plays a role of heating when being electrified, can work under the voltage of 1-380V when being electrified, and has higher heating power; the heat conducting heating silica gel sheet can meet the use requirements under different working conditions, and has a wider application range.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer.
It should be noted that:
in the present invention, all embodiments and preferred methods mentioned herein can be combined with each other to form a new technical solution, if not specifically stated.
In the present invention, all the technical features mentioned herein and preferred features may be combined with each other to form a new technical solution, if not specifically stated.
In the present invention, the components referred to or the preferred components thereof may be combined with each other to form a novel embodiment, unless otherwise specified.
In the present invention, unless otherwise stated, the numerical range "a-b" represents a shorthand representation of any combination of real numbers between a and b, where a and b are both real numbers. For example, a numerical range of "10 to 100" indicates that all real numbers between "10 to 100" have been listed herein, and "10 to 100" is only an abbreviated representation of the combination of these numbers.
In the present invention, unless otherwise specified, the individual operation steps may be performed sequentially or may not be performed in sequence. Preferably, the steps of the operations herein are performed sequentially.
Unless otherwise defined, technical and scientific terms used herein have the same meaning as is familiar to those skilled in the art. In addition, any methods or materials similar or equivalent to those described herein can also be used in the present invention.
According to one aspect of the invention, in at least one embodiment, the heat-conducting silica gel sheet is prepared by adopting the following raw materials in parts by mass: 10-100 parts of silicon rubber, 300-1900 parts of heat-conducting agent, 0.5-100 parts of flame retardant, 0.3-6 parts of reinforcing agent and 3-50 parts of cross-linking agent; the weight average molecular weight of the silicone rubber is 70-90 ten thousand.
The heat-conducting silica gel sheet is prepared from specific silicon rubber, a heat-conducting agent, a flame retardant, a reinforcing agent and a crosslinking agent with specific contents, wherein the silicon rubber is specific silicon rubber with the weight-average molecular weight of 70-90 ten thousand, the heat-conducting silica gel sheet is scientific in formula, the heat-conducting silica gel sheet has high heat conductivity and good high-temperature resistance due to the cooperation of the silicon rubber, the heat-conducting adhesive and the flame retardant, the heat-conducting silica gel sheet has reasonable hardness due to the cooperation of the silicon rubber, the reinforcing agent and the crosslinking agent, the heat conductivity can reach 1-5W/(m.K), the hardness Shore OO is 40-80, the product stability is high, and the application range is wider.
It should be noted that:
silicone rubber refers to rubber having a backbone composed of alternating silicon and oxygen atoms, with the silicon atoms typically having two organic groups attached. The weight average molecular weight of the above silicone rubber is typically, but not limited to, 70 ten thousand, 71 ten thousand, 72 ten thousand, 73 ten thousand, 74 ten thousand, 75 ten thousand, 76 ten thousand, 77 ten thousand, 78 ten thousand, 79 ten thousand, 80 ten thousand, 81 ten thousand, 82 ten thousand, 83 ten thousand, 84 ten thousand, 85 ten thousand, 86 ten thousand, 87 ten thousand, 88 ten thousand, 89 ten thousand or 90 ten thousand.
The main effect of the heat conducting agent is to improve the heat conducting property of the silica gel sheet, and different heat conducting agents have different influences on the heat conducting property of the silica gel sheet. The heat conducting agent comprises at least one of aluminum nitride, boron nitride, aluminum oxide, aluminum hydroxide, zinc oxide or silicon carbide, including but not limited to the following: aluminum nitride, boron nitride, aluminum oxide, aluminum hydroxide, zinc oxide, silicon carbide, a combination of aluminum nitride and boron nitride, a combination of boron nitride and aluminum oxide, a combination of aluminum hydroxide and zinc oxide, or a combination of aluminum hydroxide, zinc oxide and silicon carbide, or the like.
The fire retardant mainly has the effects of improving the high temperature resistance and the flame retardant effect of the silica gel sheet and preventing the silica gel sheet from being burnt and damaged when being heated by strong heat. The flame retardant comprises at least one of aluminum hydroxide, aluminum oxide and magnesium oxide, and includes but is not limited to the following components: aluminum hydroxide, aluminum oxide, magnesium oxide, a combination of aluminum hydroxide and aluminum oxide, a combination of aluminum oxide and magnesium oxide, a combination of aluminum hydroxide, aluminum oxide and magnesium oxide, or the like.
The reinforcing agent mainly has the function of increasing the mechanical strength, such as toughness and the like, of the silica gel sheet. The reinforcing agent includes at least one of talc, silica or titanium dioxide, including but not limited to talc, silica, titanium dioxide, a combination of talc and silica, a combination of silica and titanium dioxide, a combination of talc and titanium dioxide, or a combination of talc, silica and titanium dioxide, and the like.
The main function of the cross-linking agent is to form a bridge bond between polymer molecular chains and change the polymer molecular chains into a three-dimensional network structure, and the elasticity and the toughness of the silica gel sheet are better under the action of the cross-linking agent. The cross-linking agent includes at least one of bis-tetra, bis-penta, hydrogen-containing silicone oil or platinum-based catalyst, including but not limited to bis-tetra, bis-penta, hydrogen-containing silicone oil, platinum-based catalyst, a combination of bis-tetra and bis-penta, a combination of hydrogen-containing silicone oil and platinum-based catalyst, or a combination of bis-tetra, bis-penta and hydrogen-containing silicone oil, etc.
In a preferred embodiment, the heat-conducting silica gel sheet is mainly prepared from the following raw materials in parts by mass: 20-80 parts of silicon rubber, 500-1700 parts of heat-conducting agent, 10-80 parts of flame retardant, 1-6 parts of reinforcing agent and 5-45 parts of cross-linking agent.
Preferably, the heat-conducting silica gel sheet is mainly prepared from the following raw materials in parts by mass: 35-70 parts of silicon rubber, 800-1500 parts of heat-conducting agent, 30-70 parts of flame retardant, 2-5 parts of reinforcing agent and 10-40 parts of cross-linking agent.
In the preferred embodiment, the content of each raw material is further preferred, so that the proportion of each raw material is more reasonable, the heat conductivity coefficient of the heat-conducting silica gel sheet is further improved, and the heat resistance of the heat-conducting silica gel sheet is further reduced.
In a preferred embodiment, the silicone rubber has a weight average molecular weight of from 70 to 85 ten thousand. By further optimizing the weight average molecular weight of the silicone rubber, the porosity inside the heat-conductive silicone rubber sheet is further reduced, and the heat conductivity is improved.
In a preferred embodiment, the thermal conductor comprises aluminum oxide and boron nitride. Alumina and boron nitride all have good heat conduction effect, and wherein the heat conduction effect of boron nitride is better, but its price is higher, chooses for use alumina and boron nitride to act as the heat-conducting agent jointly and can improve coefficient of heat conductivity, reduces the cost of heat conduction silica gel piece as far as possible.
Preferably, the mass ratio of the aluminum oxide to the boron nitride is (10-15): (1-5), more preferably 12: (1-2).
Preferably, the flame retardant comprises aluminium oxide and/or magnesium oxide. Such flame retardants include, but are not limited to, aluminum oxide, magnesium oxide, or a combination of aluminum oxide and magnesium oxide. The specific flame retardant has good flame retardant effect, higher compatibility with other raw materials and lower price.
Preferably, the reinforcing agent comprises talc and/or titanium dioxide. Such reinforcing agents include, but are not limited to, talc, titanium dioxide, or a combination of talc and titanium dioxide. The talcum powder has good reinforcement and fire resistance, stable chemical property and can effectively enhance the toughness and chemical stability of the silica gel sheet. The titanium dioxide has strong adhesive capacity and stable chemical property, and has good reinforcing effect when being used for silica gel sheets.
Preferably, the cross-linking agent comprises bis-di-tetra and/or bis-di-penta. Such cross-linking agents include, but are not limited to, bis-bistetra, bis-dipenta, or a combination of bis-bistetra and bis-dipenta. Bis-di-tetra-is bis (2, 4-dichlorobenzoyl) peroxide, which has low decomposition temperature and high decomposition speed. The dipenta refers to 2, 5-dimethyl-2, 5 di-tert-butyl hexane peroxide, the decomposition temperature is high, the scorch performance is good, and when the dipenta is adopted, the compression deformation of vulcanized rubber is low, and the elongation is high. The strength, hardness and the like of the product can be improved by the aid of the double-two-four and the double-two-five.
Preferably, the thickness of the heat-conducting silica gel sheet is 0.5-2 mm. The thickness of the thermally conductive silicone rubber sheet is typically, but not limited to, 0.5mm, 1mm, 1.5mm, or 2 mm. When the thickness of the heat conduction silica gel sheet is within the range, the toughness of the heat conduction silica gel sheet can be ensured, the thermal resistance can be reduced, and a good heat conduction effect is ensured. The thickness is too high, so that the thermal resistance is increased, and the heat conduction effect is poor; the thickness is too small, the toughness is poor, and the service life is short.
According to another aspect of the present invention, a preparation method of the above heat conductive silicone sheet is provided, which includes the following steps: and uniformly mixing the raw materials, and curing and forming to obtain the heat-conducting silica gel sheet. The method has simple process, is suitable for mass production, and the prepared heat-conducting silica gel sheet has good heat-conducting property and wide application range.
Preferably, the curing molding comprises pressure curing molding. The production efficiency of pressure curing molding is high, the internal stress of the obtained product is small, the mechanical property is stable, the size precision of the product is high, and the product consistency is good.
Preferably, the curing molding pressure is greater than 250kgfcm 2 The curing and molding time is 20-30 seconds. The curing molding pressure is typically, but not limited to, 275kgfcm, 300kgfcm, 350kgfcm, 400kgfcm, or the like. The above-mentioned curing molding time is typically, but not limited to, 20 seconds, 21 seconds, 22 seconds, 23 seconds, 24 seconds, 25 seconds, 26 seconds, 27 seconds, 28 seconds, 29 seconds, or 30 seconds. Under the curing molding pressure and the curing molding time, the obtained heat-conducting silica gel sheet has better flexibility and smaller thermal resistance. If the pressure is too high or the time is too long, the hardness of the silica gel sheet can be increased, so that the flexibility of the silica gel sheet is reduced, the capability of the silica gel sheet for filling gaps is reduced, the fitting degree is poor, the thermal resistance is increased, and the heat conduction effect is influenced; if the pressure is too low or the time is too short, the hardness is too low, the mechanical strength is too low, and the case of deformation, failure of adhesion, and the like is likely to occur during the use.
Preferably, the curing molding temperature is 150-200 ℃. The curing temperature is typically, but not limited to, 150 deg.C, 160 deg.C, 170 deg.C, 180 deg.C, 190 deg.C, or 200 deg.C.
According to another aspect of the present invention, there is provided a heat conductive heating silicone sheet, including: the heating assembly and the heat-conducting silica gel sheet are arranged on at least one side of the heating assembly. The heat-conducting heating silica gel sheet has the functions of heat conduction and heating, plays a role of heating when electrified, can work under the voltage of 1-380V when electrified, and has higher heating power; the heat conducting function is exerted when the power is not on, the heat conducting coefficient can reach 1-5W/(m.K), the heat conducting and heating silica gel sheet can meet the use requirements under different working conditions, and the application range is wider.
Preferably, the two sides of the heating component are respectively provided with the heat-conducting silica gel sheets.
Preferably, the heat generating component includes a metal material and/or a carbon material. The metal material and/or the carbon material have good heating effect, and the heating efficiency of the heat conduction heating silica gel sheet can be improved. The heat generating component includes, but is not limited to, a metallic material, a carbon material, or a combination of a metallic material and a carbon material.
Preferably, the metallic material comprises a pure metal or an alloy.
Preferably, the pure metal comprises one of copper, aluminum, manganese or silver. The pure metal has good heating performance and excellent heat conducting performance.
Preferably, the alloy includes at least one of nichrome, nichrome alloy, stainless steel, constantan resistance alloy, neoconstantan resistance alloy, or copper-manganese alloy. Such alloys include, but are not limited to, nickel-chromium alloys, nickel-chromium-aluminum alloys, stainless steel, constantan resistance alloys, neoconstantan resistance alloys, copper-manganese alloys, combinations of nickel-chromium alloys and nickel-chromium-aluminum alloys, stainless steel and constantan resistance alloys, neoconstantan resistance alloys and copper-manganese alloys, or combinations of nickel-chromium-aluminum alloys, stainless steel, and constantan resistance alloys, and the like.
Preferably, the carbon material comprises carbon pulp and/or carbon fibers. Such carbon materials include, but are not limited to, carbon pulp, carbon fibers, or a combination of carbon pulp and carbon fibers, and the like.
It should be noted that the heating component may be a resistor sheet or a resistance wire.
Preferably, the thickness of the heat generating component is 0.03-0.5 mm. The thickness of the above-described heat generating component is typically, but not limited to, 0.03mm, 0.1mm, 0.15mm, 0.2mm, 0.25mm, 0.3mm, 0.35mm, 0.4mm, 0.45mm, or 0.5 mm. The heating component is reasonable in thickness, can bear large current and voltage, and is high in heating power.
It should be understood that, the heat-conducting heating silicone sheet further includes a conducting wire connected to the heating component, and may be any one of a teflon wire, a silicone wire (tinned copper wire), a silicone braided wire, a silicone high-temperature wire (tinned copper wire), or a high-pressure silicone wire (tinned copper wire), and the type of the heat-conducting heating silicone sheet is selected according to the carrying current and the length of the wire, which is not particularly limited in the present invention.
According to another aspect of the present invention, a preparation method of the above heat conduction heating silica gel sheet is provided, which includes the following steps:
(a) uniformly mixing the raw materials of the heat-conducting silica gel sheet, and performing to obtain an uncured heat-conducting silica gel sheet;
(b) and arranging an uncured heat conduction silica gel sheet on at least one side of the heating assembly, and curing and molding to obtain the heat conduction heating silica gel sheet.
The method has scientific and reasonable process steps, is suitable for industrial production, the prepared heat-conducting heating silica gel sheet has the functions of heat conduction and heating, can work under the voltage of 1-380V when electrified, has higher heating power and heat conductivity coefficient of 1-5W/(m.K), can meet the use requirements under different working conditions, and has wider application range.
Preferably, the curing molding comprises pressure curing molding.
Preferably, the curing molding pressure is more than 250kgfcm, and the curing molding time is 20-30 seconds. The curing molding pressure is typically, but not limited to, 275kgfcm, 300kgfcm, 350kgfcm, 400kgfcm, or the like. The above-mentioned curing molding time is typically, but not limited to, 20 seconds, 21 seconds, 22 seconds, 23 seconds, 24 seconds, 25 seconds, 26 seconds, 27 seconds, 28 seconds, 29 seconds, or 30 seconds. Under the curing and forming pressure and the curing and forming time, the obtained heat-conducting silica gel sheet has better flexibility and smaller thermal resistance. If the pressure is too high or the time is too long, the hardness of the silicon sheet can be increased, so that the flexibility of the silicon sheet is reduced, the capability of the silicon sheet for filling gaps is reduced, the fitting degree is poor, the thermal resistance is increased, and the heat conduction effect is influenced; if the pressure is too low or the time is too short, the hardness is too low, the mechanical strength is too low, and the conditions of deformation, incapability of sticking and the like are easy to occur in the using process.
Preferably, the curing molding temperature is 150-200 ℃. The curing temperature is typically, but not limited to, 150 deg.C, 160 deg.C, 170 deg.C, 180 deg.C, 190 deg.C or 200 deg.C.
It should be noted that the "pre-form" described above can be molded at a temperature below 40 ℃ to a thickness of 0.5 to 5mm to obtain an uncured thermally conductive silicone sheet.
According to another aspect of the present invention, an application of the above heat conductive silicone sheet or the heat conductive heating silicone sheet in an electronic product is provided.
The electronic products include but are not limited to security video monitoring products, semiconductor devices, relays, circuit boards or battery packs and the like.
According to another aspect of the present invention, there is provided a security video monitoring product, a semiconductor device, a relay, a circuit board or a battery pack, including the above-mentioned heat conductive silicone sheet or the above-mentioned heat conductive heating silicone sheet.
The present invention will be described in further detail with reference to examples and comparative examples.
Example 1
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by mass: 10 parts of silicon rubber, 300 parts of aluminum oxide, 0.5 part of aluminum hydroxide, 0.3 part of silicon dioxide and 3 parts of hydrogen-containing silicone oil; the weight average molecular weight of the silicon rubber is 70 ten thousand; the thickness of heat conduction silica gel piece is 1.0 mm.
Example 2
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by mass: 100 parts of silicon rubber, 1000 parts of silicon carbide, 100 parts of aluminum oxide, 6 parts of talcum powder and 50 parts of platinum-based catalyst; the weight average molecular weight of the silicone rubber is 90 ten thousand; the thickness of heat conduction silica gel piece is 2.5 mm.
Example 3
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by mass: 35 parts of silicon rubber, 1500 parts of zinc oxide, 30 parts of aluminum hydroxide, 2 parts of talcum powder and 40 parts of bis-di-five; the weight average molecular weight of the silicon rubber is 88 ten thousand; the thickness of heat conduction silica gel piece is 1.0 mm.
Example 4
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by mass: 70 parts of silicon rubber, 800 parts of aluminum hydroxide, 70 parts of aluminum oxide, 5 parts of titanium dioxide and 10 parts of bis-di-tetra-n; the weight average molecular weight of the silicon rubber is 90 ten thousand; the thickness of heat conduction silica gel piece is 3 mm.
Example 5
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by mass: 50 parts of silicon rubber, 1200 parts of silicon carbide, 45 parts of aluminum hydroxide, 4 parts of silicon dioxide and 30 parts of hydrogen-containing silicone oil; the weight average molecular weight of the silicone rubber is 90 ten thousand; the thickness of heat conduction silica gel piece is 0.3 mm.
Examples 6 to 8
A thermally conductive silicone rubber sheet, differing from example 5 in that the weight average molecular weights of the silicone rubbers in examples 6 to 8 were 70 ten thousand, 80 ten thousand, and 85 ten thousand, respectively.
The weight average molecular weight of the silicone rubber in examples 6-8 is within the preferred range of the present invention.
Examples 9 to 13
A thermally conductive silicone rubber sheet, differing from example 7 in that silicon carbide was replaced with aluminum oxide and boron nitride in examples 9 to 13, the mass ratio of aluminum oxide to boron nitride being 18: 1. 15: 1. 10: 1. 12: 1 and 12: 1.5.
the preferred thermal conductive agent of the present invention is used in examples 9 to 13, wherein the mass ratio of alumina to boron nitride in examples 10 to 13 is within the preferred range of the present invention, and the mass ratio of alumina to boron nitride in examples 12 to 13 is within the further preferred range of the present invention.
Examples 14 to 16
A thermally conductive silicone rubber sheet differs from that of example 13 in that in examples 14 to 16, aluminum hydroxide was replaced with aluminum oxide, magnesium oxide, and aluminum oxide and magnesium oxide at a mass ratio of 1:1, respectively.
Preferred flame retardants of the present invention were selected for use in examples 14-16.
Examples 17 to 19
Different from the embodiment 14, the heat-conducting silica gel sheet in the embodiments 17 to 19 has the advantages that the silicon dioxide is replaced by the talcum powder, the titanium dioxide and the talcum powder and the titanium dioxide in the mass ratio of 1:1 respectively.
Preferred enhancers of the invention are selected for use in examples 17-19.
Examples 20 to 22
A heat conductive silicone rubber sheet, which is different from example 18 in that in examples 20 to 22, hydrogen-containing silicone oil was replaced with bistetra, and bistetra at a mass ratio of 1:1, respectively.
Preferred cross-linking agents of the present invention are selected for use in examples 20-22.
Examples 23 to 25
A heat conductive silicone sheet, which is different from example 20 in that the thicknesses of the heat conductive silicone sheets in examples 23 to 25 were 0.5mm, 1mm and 2mm, respectively.
The preparation method of the heat-conducting silica gel sheet in each embodiment comprises the following steps: uniformly mixing the raw materials, molding and curing to obtain the heat-conducting silica gel sheet, wherein the curing molding pressure is 250kgfcm, and the curing molding time is 40 seconds; the curing and molding temperature is 220 ℃.
Example 26
A preparation method of a heat-conducting silica gel sheet comprises the following steps: weighing the raw materials according to the formula of the embodiment 25, uniformly mixing the raw materials, molding and curing to obtain the heat-conducting silica gel sheet, wherein the curing molding pressure is 275kgfcm, and the curing molding time is 25 seconds; the curing and molding temperature is 220 ℃.
The curing molding pressure and curing molding time in the present embodiment are within the preferred ranges of the present invention.
Example 27
A method for preparing a heat-conducting silica gel sheet, which is different from the method in example 26 in that the curing and forming temperature is 200 ℃.
The curing molding temperature in this embodiment is within the preferred range of the present invention.
Example 28
A heat conduction heating silica gel sheet comprises a heating component and two heat conduction silica gel sheets respectively arranged on two sides of the heating component, wherein the heating component is a nickel-chromium-aluminum alloy resistance sheet, and the thickness of the heating component is 0.05 mm;
the heat-conducting silica gel sheet is prepared from the following raw materials: 50 parts of silicon rubber, and the mass ratio of the silicon rubber is 5: 1, 1200 parts of aluminum oxide and silicon nitride, 45 parts of aluminum oxide, 4 parts of titanium dioxide and 30 parts of bis-di-tetra-n; the weight average molecular weight of the silicon rubber is 80 ten thousand; the thickness of heat conduction silica gel piece is 0.5 mm.
The preparation method of the heat-conducting heating silica gel sheet comprises the following steps:
(a) uniformly mixing the raw materials of the heat-conducting silica gel sheet, and then performing die pressing at 35 ℃ to obtain an uncured heat-conducting silica gel sheet;
(b) stacking the uncured heat-conducting silica gel sheet, the heating assembly and the uncured heat-conducting silica gel sheet layer by layer, molding and curing to obtain the heat-conducting heating silica gel sheet, wherein the curing molding pressure is 300kgfcm, the curing molding time is 25 seconds, and the curing molding temperature is 180 ℃.
Examples 29 to 30
A heat conductive heating silicone sheet, which is different from embodiment 28 in that the thicknesses of the heat conductive silicone sheets in embodiments 29 to 30 are 1mm and 2mm, respectively.
Comparative example 1
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by mass: 10 parts of silicon rubber, 300 parts of aluminum nitride, 0.5 part of aluminum hydroxide, 0.3 part of silicon dioxide and 3 parts of hydrogen-containing silicone oil; the weight average molecular weight of the silicon rubber is 30 ten thousand; the thickness of heat conduction silica gel piece is 0.3 mm.
Unlike example 1, the weight average molecular weight of the silicone rubber in this comparative example is outside the range provided by the present invention.
Comparative example 2
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by mass: 10 parts of silicon rubber, 300 parts of aluminum nitride, 0.5 part of aluminum hydroxide, 0.3 part of silicon dioxide and 3 parts of hydrogen-containing silicone oil; the weight average molecular weight of the silicon rubber is 100 ten thousand; the thickness of heat conduction silica gel piece is 0.3 mm.
Unlike example 1, the weight average molecular weight of the silicone rubber in this comparative example is outside the range provided by the present invention.
Comparative example 3
The heat-conducting silica gel sheet is prepared from the following raw materials in parts by mass: 5 parts of silicon rubber, 2000 parts of aluminum nitride, 0.1 part of aluminum hydroxide, 10 parts of silicon dioxide and 60 parts of hydrogen-containing silicone oil; the weight average molecular weight of the silicon rubber is 70 ten thousand; the thickness of heat conduction silica gel piece is 0.3 mm.
Unlike example 1, the content of each raw material in this comparative example was out of the range provided by the present invention.
Effect test
The performance of the silica gel sheets in each example and each comparative example was tested, and the test results are shown in table 1.
Wherein: the hardness is measured by a Shore 00 hardness tester, and the detection standard is ASTM D2240; the thermal conductivity adopts a DRL-3 thermal conductivity tester, and the detection standard is ASTM D5470; after the heat-conducting heating silica gel sheet is electrified, the heating power is tested by using a UTP3303/3305 double-channel adjustable direct-current stabilized voltage power supply; the high temperature resistance is tested by a method of placing the high temperature test box at 200 ℃ for 48h to see the appearance change.
TABLE 1
As can be seen from the table 1, the comprehensive performance of each embodiment is superior to that of each comparative example, so that the formula of the heat-conducting silica gel sheet provided by the invention is scientific and reasonable, and the obtained heat-conducting silica gel sheet has excellent heat conductivity coefficient, more reasonable hardness and higher high-temperature resistance.
Further analysis shows that the comprehensive properties of examples 6-8 are better than those of example 5, which indicates that the comprehensive properties of the heat-conducting silica gel sheet can be further improved by optimizing the weight average molecular weight of the silicone rubber; the overall performance of examples 9-13 is better than that of example 7, which demonstrates that the overall performance of the thermally conductive silicone sheet can be further improved by using the preferred thermally conductive agent of the present invention; the comprehensive performance of the examples 10-13 is better than that of the example 9, which shows that the comprehensive performance of the heat-conducting silica gel sheet can be further improved by adopting the heat-conducting agent with the preferred specific proportion of the invention; the overall performance of examples 12-13 is superior to that of examples 10-11, demonstrating that the overall performance of the thermally conductive silicone sheet can be further improved with the further preferred specific proportions of the thermally conductive agent of the present invention.
The overall performance of examples 14-16 is better than that of example 13, which demonstrates that the overall performance of the thermally conductive silicone sheet can be further improved by using the preferred flame retardant of the present invention; the overall performance of examples 17-19 is superior to that of example 14, demonstrating that the use of the preferred reinforcing agents of the present invention can further improve the overall performance of the thermally conductive silicone sheet; the overall performance of examples 20-22 is superior to that of example 18, demonstrating that the use of the preferred cross-linking agent of the present invention can further improve the overall performance of the thermally conductive silicone sheet; the overall performance of examples 23-25 is superior to that of example 20, demonstrating that the overall performance of the thermally conductive silicone sheet can be further improved with the preferred thickness of the present invention; the overall performance of examples 25-27 was sequentially improved, demonstrating that the overall performance of the thermally conductive silicone sheet could be further improved by a step-wise optimization of the preparation process.
The heat-conducting heating silica gel sheet in embodiments 28 to 30 has both heat-conducting and heating functions, and has a wider application range.
In addition, after the high temperature resistance test of each embodiment, the silica gel sheet is unchanged, which shows that the silica gel sheet provided by the invention can resist the high temperature of 200 ℃ and has good high temperature resistance; after the high temperature resistance test of each proportion, the surface of the silica gel sheet has different degrees of heat damage, which indicates that the high temperature resistance is poor.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (21)
1. The heat-conducting silica gel sheet is characterized by being prepared from the following raw materials in parts by mass: 20-80 parts of silicon rubber, 500-1700 parts of heat-conducting agent, 10-80 parts of flame retardant, 1-6 parts of reinforcing agent and 5-45 parts of cross-linking agent; the weight average molecular weight of the silicon rubber is 70-85 ten thousand;
the heat conducting agent consists of aluminum oxide and boron nitride, and the mass ratio of the aluminum oxide to the boron nitride is (10-15): (1-5);
the flame retardant is selected from aluminum oxide and magnesium oxide;
the reinforcing agent is selected from talcum powder and titanium dioxide;
the cross-linking agent is selected from bis-tetra and bis-penta;
the thickness of heat conduction silica gel piece is 0.5 mm.
2. The heat-conducting silica gel sheet according to claim 1, wherein the heat-conducting silica gel sheet is prepared from the following raw materials in parts by mass: 35-70 parts of silicon rubber, 800-1500 parts of heat-conducting agent, 30-70 parts of flame retardant, 2-5 parts of reinforcing agent and 10-40 parts of cross-linking agent.
3. A thermally conductive silica gel sheet according to claim 1, wherein the mass ratio of aluminum oxide to boron nitride is 12: (1-2).
4. The preparation method of the heat-conducting silica gel sheet according to any one of claims 1 to 3, characterized by comprising the following steps: and uniformly mixing the raw materials, and curing and forming to obtain the heat-conducting silica gel sheet.
5. The method for preparing the heat-conducting silicone sheet according to claim 4, wherein the curing molding includes pressure curing molding.
6. The method for preparing the heat-conducting silica gel sheet according to claim 4, wherein the curing molding pressure is greater than 250kgfcm, and the curing molding time is 20 to 30 seconds.
7. The method for preparing the heat-conducting silica gel sheet as claimed in claim 4, wherein the curing and molding temperature is 150-200 ℃.
8. The utility model provides a heat conduction heating silica gel piece which characterized in that includes: a heat-generating component, and the heat-conducting silicone sheet according to any one of claims 1 to 3, wherein the heat-conducting silicone sheet is disposed on at least one side of the heat-generating component.
9. The heat-conducting heating silica gel sheet according to claim 8, wherein the heat-conducting silica gel sheet is respectively arranged on two sides of the heating component.
10. The thermally conductive heating silicone sheet according to claim 8, wherein the heat generating component comprises a metal material and/or a carbon material.
11. The thermally conductive heating silicone sheet according to claim 10, wherein the metal material comprises a pure metal or an alloy.
12. The thermally conductive heating silicone sheet according to claim 11, wherein the pure metal comprises one of copper, aluminum, manganese, or silver.
13. The thermally conductive heating silicone sheet of claim 11, wherein the alloy comprises at least one of nichrome, nichrome alloy, stainless steel, constantan resistance alloy, neoconstantan resistance alloy, or copper manganese alloy.
14. The thermally conductive heated silicone sheet according to claim 10, wherein the carbon material comprises carbon paste and/or carbon fibers.
15. The heat-conducting heating silica gel sheet according to claim 8, wherein the thickness of the heating component is 0.03-0.5 mm.
16. The preparation method of the heat-conducting heating silica gel sheet according to any one of claims 8 to 15, comprising the following steps:
(a) uniformly mixing the raw materials of the heat-conducting silica gel sheet, and performing to obtain an uncured heat-conducting silica gel sheet;
(b) and arranging the uncured heat-conducting silica gel sheet on at least one side of the heating assembly, and curing and molding to obtain the heat-conducting heating silica gel sheet.
17. The method for preparing the heat-conducting heating silica gel sheet according to claim 16, wherein the curing molding comprises pressure curing molding.
18. The method for preparing the heat-conducting heating silica gel sheet according to claim 16, wherein the curing molding pressure is greater than 250kgfcm, and the curing molding time is 20-30 seconds.
19. The method for preparing the heat-conducting and heating silica gel sheet as claimed in claim 16, wherein the curing and molding temperature is 150-200 ℃.
20. The use of the thermally conductive silicone sheet according to any one of claims 1 to 3 or the thermally conductive heating silicone sheet according to any one of claims 8 to 15 in an electronic product.
21. A security video monitoring product, a semiconductor device, a relay, a circuit board or a battery pack is characterized by comprising the heat-conducting silica gel sheet in any one of claims 1 to 3 or the heat-conducting heating silica gel sheet in any one of claims 8 to 15.
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| CN111518367A (en) * | 2020-04-29 | 2020-08-11 | 昆山兆科电子材料有限公司 | High-efficient heat conduction film |
| CN111690333B (en) * | 2020-06-11 | 2022-03-25 | 东莞市兆科电子材料科技有限公司 | Heat-conducting gasket and preparation method and application thereof |
| CN113015413B (en) * | 2021-03-02 | 2023-12-15 | 合肥布诺太阳能科技有限公司 | Heat-conducting silica gel sheet for solar inverter and preparation method thereof |
| CN113512293A (en) * | 2021-07-26 | 2021-10-19 | 深圳市富发世纪科技有限公司 | Silica gel sealing element 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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