Powder treating agent, two-component heat-conducting gel and preparation method and application of two-component heat-conducting gel

By using a new powder treatment agent prepared from D4H cyclotetrasiloxane, vinyl silane, olefin, and phenyl vinyl silicone oil, the problem of rising hardness and thermal resistance of two-component thermal gel at high temperatures is solved, and the problem of increasing hardness and thermal resistance of two-component thermal gel is achieved. The thermal stability and extrusion of thermal conductivity of thermal gels extend the service life of electronic components.

CN119463186AActive Publication Date: 2025-02-18GUANGZHOU BAIYUN CHEM IND +1

Patent Information

Application Number
CN202411646375.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-18
Publication Date
2025-02-18
Estimated Expiration
2044-11-18

AI Technical Summary

Technical Problem

In high-temperature use environments, the hardness and thermal resistance of existing two-component thermal gels are prone to increase, affecting the service life of electronic components.

Method used

A new powder treatment agent prepared by hydrogen silicone reaction of D4H cyclotetrasiloxane, vinyl silane, olefin, and phenyl vinyl silicone oil was prepared by hydrogen silicone addition. The powder treatment agent introduces polysiloxane and phenyl groups into the molecular chain structure to improve their temperature resistance and wettability.

Benefits of technology

In a long-term high-temperature environment, the hardness and thermal resistance of the thermal gel remain stable, which significantly improves the thermal stability of the thermal gel, thereby extending the service life of electronic components and improving its extrusion.

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Abstract

The invention discloses a powder treating agent, two-component heat-conducting gel as well as a preparation method and application of the two-component heat-conducting gel. The powder treating agent is prepared by sequentially carrying out hydrosilylation reaction on D4H cyclotetrasiloxane, vinyl silane, olefin and phenyl vinyl silicone oil. Wherein the structural formula of the vinyl silane is Vi-Si-(OR1) 3, and OR1 is a methoxy group, an ethyoxyl group, a formyloxy group or an acetoxyl group; the structural formula of the olefin is # imgabs0 # 20 > = q > = 8; and Vi is vinyl. According to the powder treating agent disclosed by the invention, a polysiloxane polymer and a phenyl group are introduced, so that the powder treating agent has excellent temperature resistance, is not degraded and volatilized under the condition of long-time high-temperature aging, ensures that hardness and thermal resistance are not obviously increased and has excellent thermal stability, and when the powder treating agent is used in heat-conducting gel, the thermal stability of the heat-conducting gel is effectively improved, and the service life of the heat-conducting gel is prolonged. And the service life and the period of the electronic component are prolonged.
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Description

Technical Field

[0001] The present invention belongs to the technical field of polymer materials, and more specifically, the present invention relates to a powder treatment agent, a two-component thermal conductive gel prepared by using the powder treatment agent, and a preparation method and application thereof. Background Art

[0002] In recent years, the automotive and electronic communications industries have developed rapidly, such as new energy vehicles, 5G communications, smart phones and laptops. The heat dissipation problem has gradually received widespread attention, and silicone thermal conductive gel, thermal conductive gasket and thermal conductive silicone grease have also been widely used. Among them, silicone thermal conductive gel can be divided into single-component and two-component. The single-component is similar to thermal conductive mud and thermal conductive silicone grease, and is an amorphous substance. The two-component thermal conductive gel is a mixture of two components and then cross-linked and cured. After curing, it is similar to a thermal conductive gasket. The construction process of the two-component thermal conductive gel is simple and can meet various complex construction conditions.

[0003] The main function of thermally conductive gel is to dissipate heat. In a long-term high-temperature environment, its thermal resistance and hardness will increase significantly, which will have a great impact on the service life of electronic components. CN 116285366A discloses a two-component thermally conductive gel. The prepared hydrogen-containing organic polysiloxane is matched with a tackifier to improve the interface compatibility between the filler and the silicone, and effectively improve the bonding force between the thermally conductive gel and the interface, but the hardness and thermal resistance of high-temperature aging are not tested. CN 118271851A discloses a two-component high thermal conductivity gel and its preparation method. A high thermal conductivity thermally conductive gel can be obtained by mixing a long-chain silane coupling agent for treatment, and its long-term stability is not studied. CN113248928A discloses a vinyl silicone oil with a long-chain alkyl side chain. The thermally conductive gel prepared by using this silicone oil has a high thermal conductivity and high extrudability. Since the powder treatment agent used is conventional hexadecylmethoxysilane, the thermal resistance stability of the thermally conductive gel at high temperature is not studied.

[0004] The increase in hardness and thermal resistance of two-component thermal conductive gel is mainly related to the powder treatment agent. Ordinary long-chain alkyl treatment agents are easily cracked in a long-term high-temperature use environment, and the hardness and thermal resistance both increase significantly. The increase in thermal resistance will directly affect the service life of electronic components.

[0005] Therefore, it is very meaningful to provide a two-component thermally conductive gel that can maintain long-term stability of hardness and thermal resistance in a high-temperature use environment. Summary of the invention

[0006] Based on this, the purpose of the present invention is to provide a powder treatment agent, a two-component thermal conductive gel, and a preparation method and application thereof. The present invention prepares a new type of powder treatment agent based on the molecular chain structure. In the two-component thermal conductive gel prepared using the powder treatment agent, the hardness and thermal resistance of the two-component thermal conductive gel do not increase significantly during long-term use in a high-temperature environment, effectively improving the thermal stability of the thermal conductive gel.

[0007] The specific technical solutions for achieving the above-mentioned invention objectives include the following.

[0008] In a first aspect of the present invention, a powder treatment agent is provided, which is prepared by sequentially reacting D4H cyclotetrasiloxane with vinyl silane, olefin, and phenyl vinyl silicone oil to undergo a hydrosilylation reaction;

[0009] Wherein, the structural formula of the vinyl silane is Vi-Si-(OR1)3, OR1 is methoxy, ethoxy, formyloxy or acetoxy; the structural formula of the olefin is 20≥q≥8, preferably 20≥q≥12, more preferably 15≥q≥12; Vi is vinyl.

[0010] The second aspect of the present invention provides a powder treatment agent having a structure as shown in formula (I):

[0011]

[0012] Wherein: two of A, B, C, and D are identical substituents having the structure of formula (II), and the other two are substituents having the structures of formula (III) and formula (IV), respectively;

[0013]

[0014] In formula (II), 20≥q≥8; in formula (III), 20≥m≥5, 20≥n≥5, Vi is vinyl; in formula (IV), OR1 is methoxy, ethoxy, formyloxy or acetoxy.

[0015] The third aspect of the present invention provides a method for preparing the above-mentioned powder treating agent, comprising the following steps:

[0016] (1) Add vinyl silane dropwise into a reaction kettle containing D4H and platinum catalyst, and reflux for reaction for 60 min to 100 min after the addition is complete;

[0017] (2) Add olefin dropwise, raise the temperature to 80°C to 100°C and reflux for 60 min to 100 min;

[0018] (3) Then, add phenyl vinyl silicone oil dropwise, and continue to reflux the reaction at 80°C to 100°C for 60min to 100min to remove the platinum catalyst.

[0019] In a fourth aspect of the present invention, there is provided a two-component thermally conductive gel prepared using the above-mentioned powder treatment agent, which is prepared from component A and component B; the component A comprises the following raw materials in parts by weight:

[0020]

[0021] The B component includes the following raw materials in parts by weight:

[0022]

[0023]

[0024] A fifth aspect of the present invention provides a method for preparing the above-mentioned two-component thermally conductive gel, comprising the following steps:

[0025] (1) Add vinyl silicone oil, platinum catalyst and powder treatment agent into a planetary mixer and mix them evenly. Then add thermal conductive powder in batches and stir until the mixture is evenly mixed. Then heat the mixture to 90°C to 110°C and stir for 30 to 60 minutes. Then cool the mixture to obtain component A.

[0026] (2) Add vinyl silicone oil, hydrogenated silicone oil, inhibitor and powder treatment agent into a planetary mixer and stir evenly. Then add thermal conductive powder in batches and stir until the mixture is evenly mixed. Then heat to 90℃~110℃ and stir for 30min~60min. Cool to obtain component B.

[0027] A sixth aspect of the present invention provides the use of the above two-component thermally conductive gel in the preparation of electronic components.

[0028] In the present invention, the inventors prepared a new type of powder treatment agent based on the molecular chain structure. On the one hand, the polymer and phenyl group of polysiloxane were introduced into the molecular chain segment of the powder treatment agent, so that the powder treatment agent has excellent temperature resistance, does not degrade and volatilize under long-term high-temperature aging, ensures that the hardness and thermal resistance do not increase significantly, and has excellent thermal stability. Therefore, when it is used in thermal conductive gel, it effectively improves the thermal stability of the thermal conductive gel and improves the service life and cycle of electronic components; on the other hand, the powder treatment agent introduces two long-chain alkyl groups, which can more effectively infiltrate the thermal conductive powder when preparing the thermal conductive gel, thereby facilitating the extrusion of the thermal conductive gel. Therefore, the use of the powder treatment agent of the present invention to prepare thermal conductive gel can effectively improve the thermal stability and application stability of electronic components. DETAILED DESCRIPTION

[0029] In order to facilitate the understanding of the present invention, the present invention will be described more fully below. The present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive.

[0030] Unless otherwise defined, all technical and scientific terms used in the present invention have the same meaning as those commonly understood by those skilled in the art to which the present invention belongs. The terms used in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used in the present invention includes any and all combinations of one or more of the related listed items.

[0031] Unless otherwise specified, the examples were performed according to conventional experimental conditions or the conditions recommended by the manufacturer's instructions.

[0032] The powder treatment agent of the present invention has four substituent groups on its molecular chain segment and has the following performance advantages: 1. The polymer with polysiloxane introduced into the main chain has better temperature resistance than ordinary long-chain silane such as hexadecyloxysilane, and the introduction of phenyl groups into the molecular chain segment can further improve the temperature resistance of the powder treatment agent, and no degradation and volatilization occur under long-term high-temperature aging conditions, ensuring that the hardness and thermal resistance do not increase, and having excellent stability; 2. Two of the substituents are long-chain alkyl groups, which can more effectively infiltrate the thermal conductive powder and improve the extrusion performance compared with ordinary long-chain alkyl coupling agents; 3. The molecular chain segment contains a monovinyl group, and the group is located at the outermost end of the molecule, which is easy to react, avoiding the problem of hardness increase caused by post-curing due to steric hindrance, and can participate in the cross-linking reaction of the system to enhance the binding force between silicone oil and the powder treatment agent; 4. The triacetoxy group in the molecule has high reactivity and can react with the hydroxyl group on the surface of the thermal conductive powder to form a chemical bond, effectively modifying the thermal conductive powder.

[0033] In some embodiments of the present invention, a powder treatment agent is disclosed, which is prepared by hydrosilylation reaction of D4H cyclotetrasiloxane with vinyl silane, olefin, and phenyl vinyl silicone oil in sequence;

[0034] Wherein, the structural formula of the vinyl silane is Vi-Si-(OR1)3, OR1 is methoxy, ethoxy, formyloxy or acetoxy; the structural formula of the olefin is 20≥q≥8, preferably 20≥q≥12, more preferably 15≥q≥12; Vi is vinyl.

[0035] In some embodiments, the vinyl silane is vinyl triacetoxy silane.

[0036] In some embodiments, the olefin is 1-hexadecene.

[0037] In some embodiments, the structural formula of the phenyl vinyl silicone oil is Its viscosity at 25°C is 100cp~2000cp.

[0038] In some embodiments, the molar ratio of the D4H cyclotetrasiloxane, vinyl silane, olefin and the vinyl group in the phenyl vinyl silicone oil is 1:0.5-1.5:1.5-2.5:0.5-1.5, preferably 1:0.8-1.2:1.8-2.2:0.8-1.2, and more preferably 1:1:2:1.

[0039] In some embodiments, the viscosity of the phenyl vinyl silicone oil is 100 cp to 120 cp.

[0040] In some embodiments, the vinyl content of the phenyl vinyl silicone oil is 0.2 wt % to 8 wt %, preferably 5 wt % to 6 wt %.

[0041] In some embodiments, the phenyl content of the phenyl vinyl silicone oil is 25 wt % to 35 wt %, preferably 29 wt % to 31 wt %.

[0042] In other embodiments of the present invention, a powder treatment agent is disclosed, which has a structure as shown in formula (I):

[0043]

[0044] Wherein: two of A, B, C, and D are identical substituents having the structure of formula (II), and the other two are substituents having the structures of formula (III) and formula (IV), respectively;

[0045]

[0046] In formula (II), 20≥q≥8; in formula (III), 20≥m≥5, 20≥n≥5, Vi is vinyl; in formula (IV), OR1 is methoxy, ethoxy, formyloxy or acetoxy.

[0047] In some embodiments, 20≥q≥12, more preferably 15≥q≥12, and OR1 is formyloxy or acetoxy.

[0048] In other embodiments of the present invention, a method for preparing the above-mentioned powder treatment agent is disclosed, comprising the following steps:

[0049] (1) Add vinyl silane dropwise into a reaction kettle containing D4H and platinum catalyst, and reflux for reaction for 60 min to 100 min after the addition is complete;

[0050] (2) Add olefin dropwise, raise the temperature to 80°C to 100°C and reflux for 60 min to 100 min;

[0051] (3) Then, add phenyl vinyl silicone oil dropwise, and continue to reflux at 80°C to 100°C for 60min to 100min to remove the platinum catalyst.

[0052] In some embodiments, the method for preparing the powder treatment agent comprises the following steps:

[0053] (1) Add vinyl triacetoxysilane dropwise into a reaction kettle containing D4H and platinum catalyst, and reflux for reaction for 60 min to 100 min after the addition is complete;

[0054] (2) then dripping 1-hexadecene, raising the temperature to 80°C to 100°C and reflux reacting for 60min to 100min;

[0055] (3) Then, 100 parts of phenyl vinyl silicone oil with a viscosity of 100 cp and a vinyl content of 5 wt% is added dropwise, and after the addition is completed, the reaction is continued under reflux at 80° C. to 100° C. for 60 min to 100 min to remove the platinum catalyst.

[0056] In other embodiments of the present invention, the use of the above-mentioned powder treatment agent in the preparation of a two-component thermally conductive gel is disclosed.

[0057] In other embodiments of the present invention, a two-component thermally conductive gel is disclosed, which is prepared from component A and component B; the component A comprises the following raw materials in parts by weight:

[0058]

[0059] The B component includes the following raw materials in parts by weight:

[0060]

[0061] In some embodiments, the viscosity of the vinyl-terminated silicone oil is 100cp~1000cp, and the vinyl content is 0.1wt%~1wt%. Preferably, the viscosity of the vinyl-terminated silicone oil is 100cp~500cp, and the vinyl content is 0.1wt%~0.6wt%; and / or, the hydrogen content of the hydrogen-terminated silicone oil is 0.01wt%~0.5wt%, and the viscosity is 50mPa·s~500mPa·s. Preferably, the hydrogen content of the hydrogen-terminated silicone oil is 0.016wt%~0.36wt%, and the viscosity is 50mPa·s~100mPa·s; and / or, the hydrogen content of the side hydrogen-containing silicone oil is 0.05wt%~1.0wt%, and the viscosity is 50mPa·s~500mPa·s. Preferably, the hydrogen-terminated silicone oil is 0.01wt%~0.5wt%, and the viscosity is 50mPa·s~500mPa·s. The hydrogen content of the silicone oil is 0.05wt% to 0.5wt%, and the viscosity is 50mPa·s to 100mPa·s; and / or, the thermal conductive powder is alumina powder, and the average particle size of the alumina powder is 2um to 70um; preferably, the average particle size of the alumina powder is 2um to 50um; and / or, the platinum catalyst is one or more of chloroplatinic acid, chloroplatinic acid-isopropanol complex, and chloroplatinic acid-divinyltetramethyldisiloxane complex; and / or, the inhibitor is one or more of 1-ethynyl-1-cyclohexanol, tetramethyltetravinylcyclotetrasiloxane, 2-methyl-3-butynyl-2-ol, 3-methyl-1-ethynyl-3-ol, 3,5-dimethyl-1-hexynyl-3-ol, and 3-methyl-1-dodecynyl-3-ol.

[0062] In some other embodiments of the present invention, a method for preparing the above-mentioned two-component thermally conductive gel is also disclosed, comprising the following steps:

[0063] (1) Add vinyl silicone oil, platinum catalyst and powder treatment agent into a planetary mixer and mix them evenly. Then add thermal conductive powder in batches and stir until the mixture is evenly mixed. Then heat the mixture to 90°C to 110°C and stir for 30 to 60 minutes. Then cool the mixture to obtain component A.

[0064] (2) Add vinyl silicone oil, hydrogenated silicone oil, inhibitor and powder treatment agent into a planetary mixer and stir evenly. Then add thermal conductive powder in batches and stir until the mixture is evenly mixed. Then heat to 90℃~110℃ and stir for 30min~60min. Cool to obtain component B.

[0065] In other embodiments of the present invention, the application of the above two-component thermally conductive gel in the preparation of electronic components is also disclosed.

[0066] The present invention is described in detail below with reference to specific embodiments.

[0067] Example 1 Preparation of powder treatment agent

[0068] The preparation method of the powder treatment agent of this embodiment comprises the following steps:

[0069] (1) D4H and 5 ppm (based on Pt content) of Custer catalyst were first added to a reaction kettle equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, and stirred evenly;

[0070] (2) Slowly drip vinyl triacetoxysilane into the reactor, and continue to reflux for 60 minutes after dripping; the molar ratio of vinyl triacetoxysilane to D4H is 1:1;

[0071] (3) slowly dripping 1-hexadecene into the above mixed solution, and after dripping, heating to 80° C. and reflux reaction for 60 min; the molar ratio of 1-hexadecene to D4H is 2:1;

[0072] (4) Slowly drip 100 parts of phenyl vinyl silicone oil with a viscosity of 100 cp (at 25° C.), a vinyl content of 5 wt% and a phenyl content of 30 wt% into the reactor, and continue to reflux at 80° C. for 100 min. Remove the platinum catalyst by adsorption on activated carbon to obtain the product; the molar ratio of vinyl to D4H in the phenyl vinyl silicone oil is 1:1.

[0073] The powder treatment agent is obtained by reacting the four silicon-hydrogen groups in D4H with vinyl triacetoxysilane, 1-hexadecene, and the vinyl group in phenyl vinyl silicone oil through silicon-hydrogen addition reaction. The specific product structure is affected by the raw material ratio and the reaction site (in this embodiment, the molar ratio of silicon-hydrogen in D4H to vinyl triacetoxysilane, 1-hexadecene, and the vinyl group in phenyl vinyl silicone oil is 4:1:2:1). The reaction principle is as follows:

[0074]

[0075] Wherein OR1 is acetoxy, Vi is vinyl, and Ph is phenyl.

[0076] Example 2 Two-component thermally conductive gel and preparation method thereof

[0077] This embodiment provides a two-component thermally conductive gel prepared using the powder treatment agent of Example 1, which is prepared from component A and component B;

[0078] The A component includes the following raw materials in parts by weight:

[0079]

[0080] The B component includes the following raw materials in parts by weight:

[0081]

[0082] The preparation method of the two-component thermally conductive gel of this embodiment comprises the following steps:

[0083] (1) Add vinyl silicone oil, platinum catalyst and powder treatment agent into a planetary mixer and stir for 5 minutes to mix them evenly. Then add thermal conductive powder in batches and stir for 30 minutes to mix them evenly. Then heat to about 100°C and stir for 45 minutes. Cool to obtain component A.

[0084] (2) Add vinyl silicone oil, end hydrogen silicone oil, side hydrogen silicone oil, inhibitor and powder treatment agent into a planetary mixer and stir for 5 minutes. Then add thermal conductive powder in batches and stir for 30 minutes until the mixture is evenly mixed. Then heat to about 100°C and stir for 45 minutes. Cool to obtain component B.

[0085] Example 3 Two-component thermally conductive gel and preparation method thereof

[0086] This embodiment provides a two-component thermally conductive gel prepared using the powder treatment agent of Example 1, which is prepared from component A and component B;

[0087] The A component includes the following raw materials in parts by weight:

[0088]

[0089] The B component includes the following raw materials in parts by weight:

[0090]

[0091] The preparation method of the two-component thermally conductive gel of this embodiment is the same as that of Embodiment 2.

[0092] Example 4 Two-component thermally conductive gel and preparation method thereof

[0093] This embodiment provides a two-component thermally conductive gel prepared using the powder treatment agent of Example 1, which is prepared from component A and component B;

[0094] The A component includes the following raw materials in parts by weight:

[0095]

[0096] The B component includes the following raw materials in parts by weight:

[0097]

[0098] The preparation method of the two-component thermally conductive gel of this embodiment is the same as that of Embodiment 2.

[0099] Example 5 Two-component thermally conductive gel and preparation method thereof

[0100] This embodiment provides a two-component thermally conductive gel prepared using the powder treatment agent of Example 1, which is prepared from component A and component B;

[0101] The A component includes the following raw materials in parts by weight:

[0102]

[0103] The B component includes the following raw materials in parts by weight:

[0104]

[0105]

[0106] The preparation method of the two-component thermally conductive gel of this embodiment is the same as that of Embodiment 2.

[0107] Example 6 Two-component thermally conductive gel and preparation method thereof

[0108] This embodiment provides a two-component thermally conductive gel prepared using the powder treatment agent of Example 1, which is prepared from component A and component B;

[0109] The A component includes the following raw materials in parts by weight:

[0110]

[0111] The B component includes the following raw materials in parts by weight:

[0112]

[0113] The preparation method of the two-component thermally conductive gel of this embodiment is the same as that of Embodiment 2.

[0114] Comparative Example 1

[0115] The two-component thermally conductive gel provided in this comparative example is prepared from component A and component B;

[0116] The A component includes the following raw materials in parts by weight:

[0117]

[0118] The B component includes the following raw materials in parts by weight:

[0119]

[0120] The preparation method of the two-component thermally conductive gel in this comparative example is the same as that in Example 2.

[0121] Comparative Example 2

[0122] The two-component thermally conductive gel provided in this comparative example is prepared from component A and component B;

[0123] The A component includes the following raw materials in parts by weight:

[0124]

[0125] The B component includes the following raw materials in parts by weight:

[0126]

[0127]

[0128] The preparation method of the two-component thermally conductive gel in this comparative example is the same as that in Example 2.

[0129] Comparative Example 3

[0130] The two-component thermally conductive gel provided in this comparative example is prepared from component A and component B;

[0131] The A component includes the following raw materials in parts by weight:

[0132]

[0133] The B component includes the following raw materials in parts by weight:

[0134]

[0135] The preparation method of the two-component thermally conductive gel in this comparative example is the same as that in Example 2.

[0136] The thermally conductive gel adhesives of Examples 2 to 6 and Comparative Examples 1 to 3 were baked at 120°C for 60 minutes and then tested respectively:

[0137] 1. Thermal resistance: measured in accordance with "ASTM D 5470-01 Characterization test for testing the thermal conductivity properties of thin thermally conductive solid electrical insulating materials", unit: ℃*in 2 / W.

[0138] 2. Heat aging resistance: The heat aging condition is 150℃ / 1000h, and the hardness before and after aging is measured. The hardness is measured in accordance with ASTM D2240 Standard Test Method for Rubber Property-Durometer Hardness, and a Shore 00 durometer is used for the measurement.

[0139] 3. Extrusion test: A and B were respectively loaded into 400mL 1:1 two-component rubber cartridges. The mixing tube used was a Shenzhen Pusen round-mouth 13-18 stepped mixing tube. The test pressure was 0.6MPa and the test time was 60s.

[0140] The test results are shown in Table 1.

[0141] Table 1

[0142]

[0143] It can be seen from Table 1 that the thermally conductive gel prepared by using the homemade powder treatment agent in Examples 2 to 6, after being baked at 150°C for 500h and 1000h, the hardness rises by no more than 1000, and the thermal resistance rises within 10%. The powder treatment agent used in Comparative Examples 1 to 3 is a conventional long-chain coupling agent hexadecyl trimethoxy, and the hardness of the thermally conductive gel prepared therefrom rises significantly, basically rising by about 35HA at 150°C / 1000h, and the thermal resistance rises by more than 40% at 150°C / 1000h. This is because the homemade powder treatment agent of the present invention is a polymer of main chain polysiloxane, and compared with ordinary long-chain silanes such as hexadecyloxysilane, its temperature resistance is more excellent, and it is not easy to decompose or volatilize at high temperature. In addition, there are phenyl groups in the polymer chain segment, which can further improve the temperature resistance of the powder treatment agent. The hardness and thermal resistance of the thermally conductive gel will not rise significantly during long-term high-temperature aging.

[0144] In terms of extrudability, the extrudability of the thermally conductive gels of Examples 2 to 6 is significantly better than that of the thermally conductive gels of Comparative Examples 1 to 3. This is because the powder treatment agent of the present invention has long-chain alkyl groups introduced, and multiple long-chain alkyl groups can enhance the wettability of the powder surface, and the wettability is better than that of ordinary single long-chain alkyl silanes, thus effectively improving the extrudability. Under the condition of the same amount of thermally conductive powder added, as the amount of powder treatment agent increases, the extrudability will be improved (the extrudability of Example 5 is higher than that of Example 2, and the extrudability of Example 6 is higher than that of Example 3).

[0145] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0146] The above-mentioned embodiments only express several implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A powder treatment agent, characterized in that: It is prepared by the hydrosilylation reaction of D4H cyclotetrasiloxane with vinyl silane, olefin, and phenyl vinyl silicone oil in sequence; Wherein, the structural formula of the vinyl silane is Vi-Si-(OR1)3, OR1 is methoxy, ethoxy, formyloxy or acetoxy; the structural formula of the olefin is Preferably, it is 20≥q≥12, more preferably, it is 15≥q≥12; Vi is a vinyl group.

2. The powder processing agent according to claim 1, characterized in that: The vinyl silane is vinyl triacetoxy silane; and / or, The olefin is 1-hexadecene; and / or, The structural formula of the phenyl vinyl silicone oil is Its viscosity at 25°C is 100cp to 2000cp; and / or, The molar ratio of the D4H cyclotetrasiloxane, vinyl silane, olefin and the vinyl group in the phenyl vinyl silicone oil is 1:0.5-1.5:1.5-2.5:0.5-1.5, preferably 1:0.8-1.2:1.8-2.2:0.8-1.2, and more preferably 1:1:2:

1.

3. The powder processing agent according to claim 2, characterized in that: The viscosity of the phenyl vinyl silicone oil is 100cp~120cp; And / or, the vinyl content of the phenyl vinyl silicone oil is 0.2wt% to 8wt%, preferably 5wt% to 6wt%; And / or, the phenyl content of the phenyl vinyl silicone oil is 25wt% to 35wt%, preferably 29wt% to 31wt%.

4. A powder treatment agent, characterized in that: It has a structure as shown in formula (I): Wherein: two of A, B, C, and D are identical substituents having the structure of formula (II), and the other two are substituents having the structures of formula (III) and formula (IV), respectively; In formula (II), 20≥q≥8; in formula (III), 20≥m≥5, 20≥n≥5, Vi is vinyl; in formula (IV), OR1 is methoxy, ethoxy, formyloxy or acetoxy.

5. The powder processing agent according to claim 4, characterized in that: 20≥q≥12, more preferably 15≥q≥12, OR1 is formyloxy or acetoxy.

6. The method for preparing a powder treatment agent according to any one of claims 1 to 5, characterized in that: The following steps are involved: (1) Add vinyl silane dropwise into a reaction kettle containing D4H and platinum catalyst, and reflux for 60 to 100 minutes; (2) Add olefin dropwise, raise the temperature to 80°C to 100°C and reflux for 60min to 100min; (3) Then, add phenyl vinyl silicone oil dropwise, reflux at 80°C to 100°C for 60min to 100min, and remove the platinum catalyst to obtain the product.

7. A two-component thermally conductive gel, characterized in that: Prepared from component A and component B; component A includes the following raw materials in parts by weight: The B component includes the following raw materials in parts by weight:

8. The two-component thermally conductive gel according to claim 7, characterized in that: The viscosity of the vinyl-terminated silicone oil is 100 cp to 1000 cp, and the vinyl content is 0.1 wt% to 1 wt%. Preferably, the viscosity of the vinyl-terminated silicone oil is 100 cp to 500 cp, and the vinyl content is 0.1 wt% to 0.6 wt%; and / or, The hydrogen content of the terminal hydrogen-containing silicone oil is 0.01wt% to 0.5wt%, and the viscosity is 50mPa·s to 500mPa·s. Preferably, the hydrogen content of the terminal hydrogen-containing silicone oil is 0.016wt% to 0.36wt%, and the viscosity is 50mPa·s to 100mPa·s; and / or, The side hydrogen-containing silicone oil has a hydrogen content of 0.05wt% to 1.0wt% and a viscosity of 50mPa·s to 500mPa·s. Preferably, the end hydrogen-containing silicone oil has a hydrogen content of 0.05wt% to 0.5wt% and a viscosity of 50mPa·s to 100mPa·s; and / or, The thermally conductive powder is alumina powder, and the average particle size of the alumina powder is 2um to 70um; preferably, the average particle size of the alumina powder is 2um to 50um; and / or, The platinum catalyst is one or more of chloroplatinic acid, chloroplatinic acid-isopropanol complex, and chloroplatinic acid-divinyltetramethyldisiloxane complex; and / or, The inhibitor is one or more of 1-ethynyl-1-cyclohexanol, tetramethyltetravinylcyclotetrasiloxane, 2-methyl-3-butynyl-2-ol, 3-methyl-1-ethynyl-3-ol, 3,5-dimethyl-1-hexynyl-3-ol, and 3-methyl-1-dodecynyl-3-ol.

9. The method for preparing the two-component thermally conductive gel according to claim 7 or 8, characterized in that: The following steps are involved: (1) Add vinyl silicone oil, platinum catalyst and powder treatment agent into a planetary mixer and mix them evenly. Then add thermal conductive powder in batches and stir until the mixture is evenly mixed. Then heat the mixture to 90°C to 110°C and stir for 30 to 60 minutes. Then cool the mixture to obtain component A. (2) Add vinyl silicone oil, hydrogenated silicone oil, inhibitor and powder treatment agent into a planetary mixer and stir evenly. Then add thermal conductive powder in batches and stir until the mixture is evenly mixed. Then heat to 90℃~110℃ and stir for 30min~60min. Cool to obtain component B.

10. Use of the two-component thermally conductive gel according to claim 7 or 8 in the preparation of electronic components.

Citation Information

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