Heat-conducting flexible glue for laser and preparation method of heat-conducting flexible glue

Abstract

The present invention discloses a laser heat conduction flexible glue, which comprises a component A and a component B. The component A comprises first silicone oil, first alumina, a first coupling agent and a catalyst, the component B comprises second silicone oil, second alumina, an inhibitor and a second coupling agent, the first alumina and the second alumina both comprise spherical alumina, and the second alumina comprises spherical alumina. The particle size of the spherical aluminum oxide is 1-40 [mu] m. The fillers with different particle sizes are used at the same time, so that a more compact heat-conducting network can be formed, gaps among the fillers are reduced, and the heat-conducting efficiency is improved; the combination of multi-particle-size fillers avoids the problem of high viscosity caused by single-particle-size fillers, and gives consideration to both high thermal conductivity and fluidity. A stable network structure is formed through specific filler ratio and silicone oil selection, the influence of an external cross-linking agent is resisted, and the problem of soft rubber hardening caused by sealant covering in a traditional scheme is solved.

Description

Technical Field

[0001] This invention relates to the field of polymer compound compositions, and more specifically to a thermally conductive soft adhesive for lasers and its preparation method. Background Technology

[0002] In laser devices, the contact area between the optical fiber and the laser source typically requires encapsulation with a layer of flexible adhesive to protect the fiber and provide thermal conductivity. However, when a sealant is applied to the surface of the adhesive, it hardens significantly due to secondary cross-linking, affecting the quality of optical signal transmission. Furthermore, traditional thermally conductive adhesives struggle to balance thermal conductivity and flowability; high thermal conductivity often comes with high viscosity, which is detrimental to application and filling. Therefore, developing a thermally conductive adhesive for lasers that maintains high thermal conductivity, long-term flexibility, and good application performance is crucial.

[0003] Chinese invention patent application CN117551350A discloses a thermally conductive silicone composition, its preparation method, and its application. Through a refined coating and shaping process, excessively small particles are coated onto the surface of larger particles simultaneously with the coating agent during the coating and shaping process, thereby achieving a narrowing of the particle size distribution range. This allows for high thermal conductivity from high filler content while simultaneously possessing low density and high reliability. However, it tends to harden after being covered with sealant, affecting the transmission of optical signals. Chinese invention patent CN112980189B discloses a thermally conductive silicone pad with low oil seepage rate and good heat resistance, and its preparation method. The thermally conductive silicone pad is composed of a heat-resistant foamed silicone matrix composite with high thermal conductivity fillers and liquid metal. The foamed silicone matrix has high compressibility and resilience, but it cannot simultaneously achieve high thermal conductivity and long-term softness. Summary of the Invention

[0004] In order to develop a laser thermally conductive soft adhesive that can maintain high thermal conductivity, long-term flexibility, and good construction performance, the first aspect of the present invention provides a laser thermally conductive soft adhesive comprising a component A and a component B. The component A comprises a first silicone oil, a first alumina, a first coupling agent, and a catalyst. The component B comprises a second silicone oil, a second alumina, an inhibitor, and a second coupling agent. Both the first alumina and the second alumina comprise spherical alumina with a particle size of 1-40 μm.

[0005] In one embodiment, the first alumina and the second alumina further include angular alumina.

[0006] In one embodiment, the particle size of the angular alumina is 1μm or 3μm, and the particle size of the spherical alumina is 5μm, 20μm or 40μm. The weight ratio of the alumina with particle sizes of 1μm, 3μm, 5μm, 20μm or 40μm in the first alumina and the second alumina is (200-250):(200-300):(150-180):(200-250):(150-250).

[0007] In one embodiment, component A, by weight, comprises 140-150 parts of first silicone oil, 1000-1100 parts of first alumina, 1-3 parts of first coupling agent, and 1-2 parts of catalyst; and component B, by weight, comprises 145-155 parts of second silicone oil, 1000-1100 parts of second alumina, 0.03-0.08 parts of inhibitor, and 1-3 parts of second coupling agent.

[0008] In one embodiment, the first alumina and the second alumina further include quasi-spherical alumina, wherein the particle size of the quasi-spherical alumina is 0.1-1 μm.

[0009] In one embodiment, the first alumina and the second alumina further include quasi-spherical alumina, wherein the particle size of the quasi-spherical alumina is 0.5 μm.

[0010] In one embodiment, both the first silicone oil and the second silicone oil include at least one of methyl silicone oil, hydrogen-containing silicone oil, and vinyl silicone oil.

[0011] As one embodiment, the viscosity of the methyl silicone oil at 25°C is 50-100 cps.

[0012] In one embodiment, the hydrogen-containing silicone oil includes at least one of terminal hydrogen-containing silicone oil and multi-hydrogen-containing silicone oil; the vinyl silicone oil includes at least one of terminal vinyl silicone oil and multi-vinyl silicone oil.

[0013] In one embodiment, the hydrogen-containing silicone oil has a silane content of 0.3-0.8 mmol / g and a viscosity of 50-200 cps at 25°C, while the multi-hydrogen-containing silicone oil has a silane content of 0.5-1.5 mmol / g and a viscosity of 30-200 cps at 25°C.

[0014] In one embodiment, the vinyl content of the terminal vinyl silicone oil is 0.3-1.0 mmol / g, and the viscosity at 25°C is 50-25000 cps; the vinyl content of the polyvinyl silicone oil is 1.5-2.1 mmol / g, and the viscosity at 25°C is 5000-10000 cps.

[0015] In one embodiment, both the first coupling agent and the second coupling agent comprise silane coupling agent and silicate ester coupling agent, wherein the weight ratio of the silane coupling agent to the silicate ester coupling agent is 1:(1-3).

[0016] In one embodiment, the silane coupling agent includes at least one of octyltriethoxysilane coupling agent, isobutyltriethoxysilane, and methyltrimethoxysilane.

[0017] In one embodiment, the silane coupling agent includes an octyltriethoxysilane coupling agent.

[0018] In one embodiment, the silicate coupling agent includes at least one of tetraethyl orthosilicate coupling agent and methyl orthosilicate coupling agent.

[0019] In one embodiment, the silicate coupling agent includes tetraethyl orthosilicate coupling agent.

[0020] In one embodiment, the catalyst is a platinum catalyst, and the content of the platinum catalyst in the thermally conductive soft adhesive for lasers is 4000-6000 ppm.

[0021] In one embodiment, the inhibitor comprises at least one of tetramethyltetravinylcyclotetrasiloxane or ethynylcyclohexanol.

[0022] In one embodiment, the inhibitor is tetramethyltetravinylcyclotetrasiloxane.

[0023] A second aspect of the present invention provides a method for preparing a thermally conductive soft adhesive for lasers, comprising the following steps: The first silicone oil, the first alumina, and the first coupling agent are mixed and stirred, heated to 110-130℃, mixed under vacuum, and cooled to obtain the A component masterbatch. The second silicone oil, the second alumina, and the second coupling agent are mixed and stirred, heated to 110-130℃, mixed under vacuum, and cooled to obtain the B component masterbatch. A catalyst was added to the masterbatch of component A at room temperature, and the mixture was vacuum-mixed to obtain component A. Inhibitors were added to the masterbatch of component B at room temperature and mixed under vacuum to obtain component B; Mix components A and B evenly according to the weight ratio, remove air bubbles, and cure to obtain thermally conductive soft adhesive for lasers.

[0024] As one implementation method, the curing is performed at room temperature for 20-26 hours or at 60-80°C for 50-70 minutes.

[0025] As one implementation method, the curing is performed by curing at room temperature for 24 hours or at 70°C for 60 minutes.

[0026] In one embodiment, the weight ratio of component A to component B is 1:(0.5-2).

[0027] In one embodiment, the weight ratio of component A to component B is 1:1.

[0028] Compared with the prior art, the present invention has the following beneficial effects: (1) The laser thermal conductive soft adhesive of the present invention uses 1μm and 3μm angular alumina and 5μm, 20μm and 40μm spherical alumina. The fillers with different particle sizes and shapes can fill each other to form a denser thermal conductive network, reduce the gaps between fillers and improve thermal conductivity. The combination of multi-particle-size fillers avoids the high viscosity problem caused by single-particle-size fillers and takes into account both high thermal conductivity and flowability.

[0029] (2) The thermally conductive soft adhesive for lasers described in this invention optimizes the crosslinking density by using a combination of methyl silicone oil, hydrogen-containing silicone oil and vinyl silicone oil, so that the soft adhesive can maintain a low crosslinking density after being covered with sealant, thus avoiding the increase in hardness caused by excessive crosslinking.

[0030] (3) The thermally conductive soft adhesive for lasers described in this invention uses silicone oil with specific viscosity, vinyl content and silane content, controls the amount and ratio, avoids excessive cross-linking, and ensures long-term stability; reduces the frictional resistance between fillers, lowers the overall viscosity, and makes the material easier to apply.

[0031] (4) The thermally conductive soft adhesive for lasers described in this invention adopts a two-component soft adhesive structure design, which reduces the secondary cross-linking effect of active ingredients on the soft adhesive after covering with sealant; the specific filler ratio and silicone oil selection form a stable network structure, resisting the influence of external cross-linking agents, and avoiding the problem of soft adhesive hardening caused by covering with sealant in traditional solutions.

[0032] (5) The thermally conductive soft adhesive for lasers described in this invention uses both octyltriethoxysilane coupling agent and tetraethyl orthosilicate coupling agent, which can improve the compatibility between inorganic fillers and organosilicon matrix, further enhance interfacial bonding, and improve the continuity and stability of the thermally conductive network; at the same time, it reduces filler agglomeration, improves dispersibility, further reduces viscosity, and enhances the overall performance of the material. Detailed Implementation

[0033] Example 1 A thermally conductive soft adhesive for lasers includes component A and component B. Component A comprises 150 parts by weight of first silicone oil, 1080 parts by weight of first alumina, 2 parts by weight of first coupling agent and 1 part by weight of catalyst. Component B comprises 152.5 parts by weight of second silicone oil, 1080 parts by weight of second alumina, 0.05 parts by weight of inhibitor and 2 parts by weight of second coupling agent.

[0034] The first silicone oil comprises vinyl-terminated silicone oil and methyl silicone oil in a weight ratio of 100:40; the vinyl-terminated silicone oil has a vinyl content of 0.4 mmol / g and a viscosity of 100-150 cps at 25°C, and is purchased from Ambia Specialty Silicones (Nantong) Co., Ltd., model VS100 silicone oil; the methyl silicone oil has a viscosity of 50 cps at 25°C, and is purchased from Dow Silicones Co., Ltd., model PMX-200 silicone oil.

[0035] The second silicone oil comprises vinyl-terminated silicone oil, hydrogen-terminated silicone oil, multi-hydrogen-containing silicone oil, and methyl silicone oil in a weight ratio of 44:94:4.5:10. The vinyl-terminated silicone oil has a vinyl content of 0.4 mmol / g and a viscosity of 100-150 cps at 25°C; it was purchased from Ambia Specialty Silicones (Nantong) Co., Ltd., and is designated as VS100 silicone oil. The hydrogen-terminated silicone oil has a silane content of 0.5 mmol / g and a viscosity of 50-100 cps at 25°C; it was purchased from Keqi Polymer Materials, and is designated as D-50. The multi-hydrogen-containing silicone oil has a silane content of 0.7 mmol / g and a viscosity of 30-50 cps at 25°C; it was purchased from Shanghai Jingri New Materials Technology Co., Ltd., and is designated as DH007. The methyl silicone oil has a viscosity of 50 cps at 25°C and was purchased from Dow Silicones Co., Ltd., and is designated as PMX-200 silicone oil.

[0036] The particle sizes of the first alumina and the second alumina are 1μm, 3μm, 5μm, 20μm, and 40μm; the weight ratio of angular alumina with particle sizes of 1μm and 3μm to spherical alumina with particle sizes of 5μm, 20μm, and 40μm is 200:300:150:250:180.

[0037] 1μm angular alumina, purchased from Zhengzhou Yufa High-Tech Materials Co., Ltd., model RA1G; 3μm angular alumina, purchased from Zhengzhou Yufa High-Tech Materials Co., Ltd., model FA3; 5μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE05; 20μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE20; 40μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE40.

[0038] The first coupling agent and the second coupling agent are both combinations of octyltriethoxysilane coupling agent and tetraethyl orthosilicate coupling agent, with a weight ratio of 1:1.

[0039] The catalyst is a platinum catalyst; the inhibitor is tetramethyltetravinylcyclotetrasiloxane.

[0040] A method for preparing a thermally conductive soft adhesive for laser applications includes the following steps: The first silicone oil, the first alumina, and the first coupling agent were mixed and stirred for 1 hour, heated to 120°C, and mixed under vacuum for 4 hours. After cooling, component A masterbatch was obtained. The second silicone oil, the second alumina, and the second coupling agent were mixed and stirred for 1 hour, heated to 120°C, and mixed under vacuum for 4 hours. After cooling, the B component masterbatch was obtained. A catalyst was added to the masterbatch of component A at room temperature, and the mixture was vacuum-mixed to obtain component A. Inhibitors were added to the masterbatch of component B at room temperature and mixed under vacuum to obtain component B; Mix components A and B evenly according to the weight ratio, remove air bubbles, and cure at 70℃ for 60 minutes to obtain thermally conductive soft adhesive for laser use.

[0041] The weight ratio of component A to component B is 1:1.

[0042] Example 2 A thermally conductive soft adhesive for lasers includes component A and component B. Component A comprises, by weight, 150 parts of first silicone oil, 1080 parts of first alumina, 2 parts of first coupling agent and 1 part of catalyst. Component B comprises, by weight, 150 parts of second silicone oil, 1080 parts of second alumina, 0.05 parts of inhibitor and 2 parts of second coupling agent.

[0043] The first silicone oil is a vinyl-terminated silicone oil; the vinyl content of the vinyl-terminated silicone oil is 0.8 mmol / g, the viscosity at 25°C is 50-100 cps, and it is purchased from Ambia Specialty Silicones (Nantong) Co., Ltd., model VS50 silicone oil; the second silicone oil includes vinyl-terminated silicone oil, hydrogen-terminated silicone oil, and multi-hydrogen-containing silicone oil, with a weight ratio of 25:120:5. The vinyl-terminated silicone oil has a vinyl content of 0.8 mmol / g and a viscosity of 50-100 cps at 25°C. It was purchased from Ambia Specialty Silicones (Nantong) Co., Ltd., and its model is VS50 silicone oil. The hydrogen-terminated silicone oil has a silicon-hydrogen content of 0.5 mmol / g and a viscosity of 50-100 cps at 25°C. It was purchased from Keqi Polymer Materials, and its model is D-50. The multi-hydrogen-containing silicone oil has a silicon-hydrogen content of 0.7 mmol / g and a viscosity of 30-50 cps at 25°C. It was purchased from Shanghai Jingri New Materials Technology Co., Ltd., and its model is DH007. The particle sizes of the first alumina and the second alumina are 0.5 μm, 1 μm, 3 μm, 5 μm, 20 μm, and 40 μm. The weight ratio of spherical alumina with a particle size of 0.5 μm to angular alumina with a particle size of 1 μm and 3 μm, and spherical alumina with a particle size of 5 μm, 20 μm, and 40 μm is 100:250:200:180:200:150.

[0044] 0.5μm spherical alumina, purchased from Besto, model NSM-1S; 1μm angular alumina, purchased from Zhengzhou Yufa High-Tech Materials Co., Ltd., model RA1G; 3μm angular alumina, purchased from Zhengzhou Yufa High-Tech Materials Co., Ltd., model FA3; 5μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE05; 20μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE20; 40μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE40.

[0045] The first coupling agent and the second coupling agent are both combinations of octyltriethoxysilane coupling agent and tetraethyl orthosilicate coupling agent, with a weight ratio of 1:1.

[0046] The catalyst is a platinum catalyst; the inhibitor is tetramethyltetravinylcyclotetrasiloxane.

[0047] A method for preparing a thermally conductive soft adhesive for laser applications includes the following steps: The first silicone oil, the first alumina, and the first coupling agent were mixed and stirred for 1 hour, heated to 120°C, and mixed under vacuum for 4 hours. After cooling, component A masterbatch was obtained. The second silicone oil, the second alumina, and the second coupling agent were mixed and stirred for 1 hour, heated to 120°C, and mixed under vacuum for 4 hours. After cooling, the B component masterbatch was obtained. A catalyst was added to the masterbatch of component A at room temperature, and the mixture was vacuum-mixed to obtain component A. Inhibitors were added to the masterbatch of component B at room temperature and mixed under vacuum to obtain component B; Mix components A and B evenly according to the weight ratio, remove air bubbles, and cure at room temperature for 24 hours to obtain thermally conductive soft adhesive for lasers.

[0048] The weight ratio of component A to component B is 1:1.

[0049] Example 3 A thermally conductive soft adhesive for lasers includes component A and component B. Component A comprises, by weight, 150 parts of first silicone oil, 1080 parts of first alumina, 2 parts of first coupling agent and 1 part of catalyst. Component B comprises, by weight, 150 parts of second silicone oil, 1080 parts of second alumina, 0.05 parts of inhibitor and 2 parts of second coupling agent.

[0050] The first silicone oil is a vinyl-terminated silicone oil and a polyvinyl silicone oil in a weight ratio of 140:10. The vinyl-terminated silicone oil has a vinyl content of 0.8 mmol / g and a viscosity of 50-100 cps at 25°C. It was purchased from Ambia Specialty Silicones (Nantong) Co., Ltd., and its model is VS50 silicone oil. The polyvinyl silicone oil has a vinyl content of 2.1 mmol / g and a viscosity of 5000-10000 cps at 25°C. It was purchased from Zhejiang Wink New Materials Co., Ltd., and its model is 210.

[0051] The second silicone oil comprises vinyl-terminated silicone oil, hydrogen-terminated silicone oil, and multi-hydrogen-terminated silicone oil in a weight ratio of 20:120:10. The vinyl-terminated silicone oil has a vinyl content of 0.8 mmol / g and a viscosity of 50-100 cps at 25°C; it was purchased from Anbia Specialty Silicones (Nantong) Co., Ltd., and is designated as VS50 silicone oil. The hydrogen-terminated silicone oil has a silane content of 0.5 mmol / g and a viscosity of 50-100 cps at 25°C; it was purchased from Keqi Polymer Materials, and is designated as D-50. The multi-hydrogen-terminated silicone oil has a silane content of 1.2 mmol / g and a viscosity of 50-100 cps at 25°C; it was purchased from Runhe Silicones, and is designated as RH-H512.

[0052] The particle sizes of the first alumina and the second alumina are 0.5 μm, 1 μm, 3 μm, 5 μm, 20 μm, and 40 μm. The weight ratio of spherical alumina with a particle size of 0.5 μm to angular alumina with a particle size of 1 μm and 3 μm, and spherical alumina with a particle size of 5 μm, 20 μm, and 40 μm is 50:200:200:180:200:250.

[0053] 0.5μm spherical alumina, purchased from Besto, model NSM-1S; 1μm angular alumina, purchased from Zhengzhou Yufa High-Tech Materials Co., Ltd., model RA1G; 3μm angular alumina, purchased from Zhengzhou Yufa High-Tech Materials Co., Ltd., model FA3; 5μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE05; 20μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE20; 40μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE40.

[0054] The first coupling agent and the second coupling agent are both combinations of octyltriethoxysilane coupling agent and tetraethyl orthosilicate coupling agent, with a weight ratio of 1:1.

[0055] The catalyst is a platinum catalyst; the inhibitor is tetramethyltetravinylcyclotetrasiloxane.

[0056] A method for preparing a thermally conductive soft adhesive for laser applications includes the following steps: The first silicone oil, the first alumina, and the first coupling agent were mixed and stirred for 1 hour, heated to 120°C, and mixed under vacuum for 4 hours. After cooling, component A masterbatch was obtained. The second silicone oil, the second alumina, and the second coupling agent were mixed and stirred for 1 hour, heated to 120°C, and mixed under vacuum for 4 hours. After cooling, the B component masterbatch was obtained. A catalyst was added to the masterbatch of component A, and the mixture was vacuum-mixed to obtain component A. Inhibitors were added to the masterbatch of component B, and the mixture was vacuum-mixed to obtain component B. Mix components A and B evenly according to the weight ratio, remove air bubbles, and cure at 70℃ for 60 minutes to obtain thermally conductive soft adhesive for laser use.

[0057] The weight ratio of component A to component B is 1:1.

[0058] Comparative Example 1 A thermally conductive soft adhesive for lasers includes component A and component B. Component A comprises, by weight, 140 parts of first silicone oil, 1030 parts of first alumina, 2 parts of first coupling agent and 1 part of catalyst. Component B comprises, by weight, 150 parts of second silicone oil, 1030 parts of second alumina, 0.05 parts of inhibitor and 2 parts of second coupling agent.

[0059] The first silicone oil comprises vinyl-terminated silicone oil and methyl silicone oil in a weight ratio of 90:50; the vinyl-terminated silicone oil has a vinyl content of 0.15 mmol / g and a viscosity of 500-1000 cps at 25°C, and is purchased from Anbia Specialty Silicones, model VS500; the methyl silicone oil has a viscosity of 50 cps at 25°C and is purchased from Dow Silicones Co., Ltd., model PMX-200 silicone oil.

[0060] The second silicone oil comprises vinyl-terminated silicone oil, hydrogen-terminated silicone oil, and multi-hydrogen-containing silicone oil in a weight ratio of 60:70:20. The vinyl-terminated silicone oil has a vinyl content of 0.15 mmol / g and a viscosity of 500-1000 cps at 25°C; it was purchased from Anbia Specialty Silicones, model VS500. The hydrogen-terminated silicone oil has a silane content of 0.5 mmol / g and a viscosity of 50-100 cps at 25°C; it was purchased from Keqi Polymer Materials, model D-50. The multi-hydrogen-containing silicone oil has a silane content of 1.2 mmol / g and a viscosity of 50-100 cps at 25°C; it was purchased from Runhe Silicones, model RH-H512.

[0061] The particle sizes of the first alumina and the second alumina are 1μm, 3μm, 5μm, 20μm, and 40μm, and the weight ratio of angular alumina with particle sizes of 1μm and 3μm to spherical alumina with particle sizes of 5μm, 20μm, and 40μm is 100:100:180:200:450.

[0062] 1μm angular alumina, purchased from Zhengzhou Yufa High-Tech Materials Co., Ltd., model RA1G; 3μm angular alumina, purchased from Zhengzhou Yufa High-Tech Materials Co., Ltd., model FA3; 5μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE05; 20μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE20; 40μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE40.

[0063] The first coupling agent and the second coupling agent are both combinations of octyltriethoxysilane coupling agent and tetraethyl orthosilicate coupling agent, with a weight ratio of 1:1.

[0064] The catalyst is a platinum catalyst; the inhibitor is tetramethyltetravinylcyclotetrasiloxane.

[0065] A method for preparing a thermally conductive soft adhesive for laser applications includes the following steps: The first silicone oil, the first alumina, and the first coupling agent were mixed and stirred for 1 hour, heated to 120°C, and mixed under vacuum for 4 hours. After cooling, component A masterbatch was obtained. The second silicone oil, the second alumina, and the second coupling agent were mixed and stirred for 1 hour, heated to 120°C, and mixed under vacuum for 4 hours. After cooling, the B component masterbatch was obtained. A catalyst was added to the masterbatch of component A at room temperature, and the mixture was vacuum-mixed to obtain component A. Inhibitors were added to the masterbatch of component B at room temperature and mixed under vacuum to obtain component B; Mix components A and B evenly according to the weight ratio, remove air bubbles, and cure at 70℃ for 60 minutes to obtain thermally conductive soft adhesive for laser use.

[0066] The weight ratio of component A to component B is 1:1.

[0067] Comparative Example 2 A thermally conductive soft adhesive for lasers includes component A and component B. Component A comprises, by weight, 150 parts of first silicone oil, 1030 parts of first alumina, 2 parts of first coupling agent and 1 part of catalyst. Component B comprises, by weight, 150 parts of second silicone oil, 1000 parts of second alumina, 0.05 parts of inhibitor and 2 parts of second coupling agent.

[0068] The first silicone oil comprises vinyl-terminated silicone oil and methyl silicone oil in a weight ratio of 60:90; the vinyl-terminated silicone oil has a vinyl content of 0.06 mmol / g and a viscosity of 4000-5000 cps at 25°C, and is purchased from Anbia Specialty Silicones, model VS5000; the methyl silicone oil has a viscosity of 50 cps at 25°C and is purchased from Dow Silicones Co., Ltd., model PMX-200 silicone oil.

[0069] The second silicone oil comprises vinyl-terminated silicone oil, methyl silicone oil, hydrogen-terminated silicone oil, and multi-hydrogen-terminated silicone oil in a weight ratio of 60:40:45:5. The vinyl-terminated silicone oil has a vinyl content of 0.06 mmol / g and a viscosity of 4000-5000 cps at 25°C; it was purchased from Anbia Specialty Silicones, model VS5000. The hydrogen-terminated silicone oil has a silane content of 0.5 mmol / g and a viscosity of 50-100 cps at 25°C; it was purchased from Keqi Polymer Materials, model D-50. The multi-hydrogen-terminated silicone oil has a silane content of 0.7 mmol / g and a viscosity of 30-50 cps at 25°C; it was purchased from Shanghai Jingri New Materials Technology Co., Ltd., model DH007. The methyl silicone oil has a viscosity of 50 cps at 25°C; it was purchased from Dow Silicones Co., Ltd., model PMX-200 silicone oil.

[0070] The particle sizes of the first alumina and the second alumina are 1μm, 3μm, 5μm, 20μm, and 40μm, and the weight ratio of angular alumina with particle sizes of 1μm and 3μm to spherical alumina with particle sizes of 5μm, 20μm, and 40μm is 300:100:180:200:250.

[0071] 1μm angular alumina, purchased from Zhengzhou Yufa High-Tech Materials Co., Ltd., model RA1G; 3μm angular alumina, purchased from Zhengzhou Yufa High-Tech Materials Co., Ltd., model FA3; 5μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE05; 20μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE20; 40μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE40.

[0072] The first coupling agent and the second coupling agent are both combinations of octyltriethoxysilane coupling agent and tetraethyl orthosilicate coupling agent, with a weight ratio of 1:1.

[0073] The catalyst is a platinum catalyst; the inhibitor is tetramethyltetravinylcyclotetrasiloxane.

[0074] A method for preparing a thermally conductive soft adhesive for laser applications includes the following steps: The first silicone oil, the first alumina, and the first coupling agent were mixed and stirred for 1 hour, heated to 120°C, and mixed under vacuum for 4 hours. After cooling, component A masterbatch was obtained. The second silicone oil, the second alumina, and the second coupling agent were mixed and stirred for 1 hour, heated to 120°C, and mixed under vacuum for 4 hours. After cooling, the B component masterbatch was obtained. A catalyst was added to the masterbatch of component A, and the mixture was vacuum-mixed to obtain component A. Inhibitors were added to the masterbatch of component B, and the mixture was vacuum-mixed to obtain component B. Mix components A and B evenly according to the weight ratio, remove air bubbles, and cure at 70℃ for 60 minutes to obtain thermally conductive soft adhesive for laser use.

[0075] The weight ratio of component A to component B is 1:1.

[0076] Comparative Example 3 A thermally conductive soft adhesive for lasers includes component A and component B. Component A comprises 150 parts by weight of first silicone oil, 1030 parts by weight of first alumina, 2 parts by weight of first coupling agent and 1 part by weight of catalyst. Component B comprises 152.5 parts by weight of second silicone oil, 1030 parts by weight of second alumina, 0.05 parts by weight of inhibitor and 2 parts by weight of second coupling agent.

[0077] The first silicone oil comprises vinyl-terminated silicone oil 1, vinyl-terminated silicone oil 2, and methyl silicone oil in a weight ratio of 50:50:50. Vinyl-terminated silicone oil 1 has a vinyl content of 0.04 mmol / g and a viscosity of 15,000-25,000 cps at 25°C. It was purchased from Anbia Specialty Silicones, model VS20000. Vinyl-terminated silicone oil 2 has a vinyl content of 0.15 mmol / g and a viscosity of 500-1000 cps at 25°C. It was purchased from Anbia Specialty Silicones, model VS500. The methyl silicone oil has a viscosity of 50 cps at 25°C and was purchased from Dow Silicones Co., Ltd., model PMX-200 silicone oil.

[0078] The second silicone oil comprises vinyl-terminated silicone oil 1, vinyl-terminated silicone oil 2, methyl silicone oil, hydrogen-terminated silicone oil, and multi-hydrogen-terminated silicone oil in a weight ratio of 30:30:20:60:10. The vinyl-terminated silicone oil 1 has a vinyl content of 0.04 mmol / g and a viscosity of 15,000-25,000 cps at 25°C; it was purchased from Anbia Specialty Silicones, model VS20000. The vinyl-terminated silicone oil 2 has a vinyl content of 0.15 mmol / g and a viscosity of 500-1000 cps at 25°C; it was purchased from Anbia Specialty Silicones, model VS500. The methyl silicone oil has a viscosity of 50 cps at 25°C and was purchased from Dow Silicones Co., Ltd., model PMX-200 silicone oil. The hydrogen-containing silicone oil has a silicon-hydrogen content of 0.5 mmol / g and a viscosity of 50-100 cps at 25°C. It was purchased from Keqi Polymer Materials, model D-50. The multi-hydrogen-containing silicone oil has a silicon-hydrogen content of 0.7 mmol / g and a viscosity of 30-50 cps at 25°C. It was purchased from Shanghai Jingri New Materials Technology Co., Ltd., model DH007. The particle sizes of the first alumina and the second alumina are 1μm, 3μm, 5μm, 20μm, and 40μm, and the weight ratio of angular alumina with particle sizes of 1μm and 3μm to spherical alumina with particle sizes of 5μm, 20μm, and 40μm is 250:100:180:200:300.

[0079] 1μm angular alumina, purchased from Zhengzhou Yufa High-Tech Materials Co., Ltd., model RA1G; 3μm angular alumina, purchased from Zhengzhou Yufa High-Tech Materials Co., Ltd., model FA3; 5μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE05; 20μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE20; 40μm spherical alumina, purchased from Bengbu Zhongheng New Material Technology Co., Ltd., model CTE40.

[0080] The first coupling agent and the second coupling agent are both combinations of octyltriethoxysilane coupling agent and tetraethyl orthosilicate coupling agent, with a weight ratio of 1:1.

[0081] The catalyst is a platinum catalyst; the inhibitor is tetramethyltetravinylcyclotetrasiloxane.

[0082] A method for preparing a thermally conductive soft adhesive for laser applications includes the following steps: The first silicone oil, the first alumina, and the first coupling agent were mixed and stirred for 1 hour, heated to 120°C, and mixed under vacuum for 4 hours. After cooling, component A masterbatch was obtained. The second silicone oil, the second alumina, and the second coupling agent were mixed and stirred for 1 hour, heated to 120°C, and mixed under vacuum for 4 hours. After cooling, the B component masterbatch was obtained. A catalyst was added to the masterbatch of component A at room temperature, and the mixture was vacuum-mixed to obtain component A. Inhibitors were added to the masterbatch of component B at room temperature and mixed under vacuum to obtain component B; Mix components A and B evenly according to the weight ratio, remove air bubbles, and cure at 70℃ for 60 minutes to obtain thermally conductive soft adhesive for laser use.

[0083] The weight ratio of component A to component B is 1:1.

[0084] Performance testing 1. Shore 00 hardness: Refer to the GB / T531.1-2008 standard to test the initial hardness of the test examples and comparative examples, and then cover the thermally conductive soft rubber with a 3mm thick sealant and leave it for 7 days before testing the hardness of the thermally conductive soft rubber.

[0085] The sealant formulation is as follows: Component A: Vinyl silicone oil 1: 80 parts; Vinyl silicone oil 2: 65 parts; Platinum catalyst: 0.3 parts; Component B: Vinyl silicone oil 3: 15 parts; Vinyl silicone oil 4: 75 parts; Tetramethyltetravinylcyclotetrasiloxane (inhibitor): 0.02 parts; Hydrogen-terminated silicone oil: 50 parts; Multi-hydrogen-containing silicone oil: 4 parts.

[0086] The vinyl silicone oils 1 and 3 have a vinyl content of 0.15 mmol / g and a viscosity of 500-1000 cps at 25°C. They were purchased from Anbia Specialty Silicones, model VS500. The vinyl silicone oils 2 and 4 have a vinyl content of 0.04 mmol / g and a viscosity of 18000-25000 cps at 25°C. They were purchased from Anbia Specialty Silicones, model VS20000. The hydrogen-terminated silicone oil has a silane content of 0.5 mmol / g and a viscosity of 50-100 cps at 25°C. It was purchased from Keqi Polymer Materials, model D-50. The multi-hydrogen-containing silicone oil has a silane content of 0.7 mmol / g and a viscosity of 30-50 cps at 25°C. It was purchased from Shanghai Jingri New Materials Technology Co., Ltd., model DH007.

[0087] The method for preparing the sealant includes the following steps: Vinyl silicone oil 1, vinyl silicone oil 2, and platinum catalyst were mixed and stirred for 1 hour, and then mixed under vacuum for 1 hour to obtain component A. Vinyl silicone oil 3, vinyl silicone oil 4, hydrogen-terminated silicone oil, multi-hydrogen-containing silicone oil and inhibitor were mixed and stirred for 1 hour, and then vacuum mixed for 1 hour to obtain component B. Mix component A and component B in a 1:1 weight ratio and cure at 25°C for 24 hours to obtain the final product.

[0088] 2. Thermal conductivity: Thermal conductivity of the test examples and comparative examples are based on ASTM-5470 standard.

[0089] 3. Viscosity: Refer to the viscosity of the test examples and comparative examples in ASTM D2196-15 standard.

[0090] The performance test results are shown in Table 1.

[0091] Table 1

Claims

1. A heat conductive soft glue for laser, characterized by, The A component comprises a first silicone oil, a first alumina, a first coupling agent and a catalyst, and the B component comprises a second silicone oil, a second alumina, an inhibitor and a second coupling agent, the first alumina and the second alumina each comprise spherical alumina, and the particle size of the spherical alumina is 1-40 μm.

2. The heat conductive soft adhesive for laser according to claim 1, wherein The particle size of the first alumina and the second alumina is 1 μm, 3 μm, 5 μm, 20 μm or 40 μm, and the weight ratio of the spherical alumina with the particle size of 1 μm, 3 μm, 5 μm, 20 μm or 40 μm in the first alumina and the second alumina is (200-250):(200-300):(150-180):(200-250):(150-250).

3. The heat conductive soft glue for laser as claimed in claim 2, wherein The first alumina and the second alumina further comprise spheroidal alumina, and the particle size of the spheroidal alumina is 0.1-1 μm.

4. The heat conductive soft adhesive for laser according to claim 1, wherein The first silicone oil and the second silicone oil each comprise at least one of a methyl silicone oil, a hydrogen-containing silicone oil and a vinyl silicone oil.

5. The heat conductive soft glue for laser as claimed in claim 4, wherein The hydrogen-containing silicone oil comprises at least one of a terminal hydrogen-containing silicone oil and a multi-hydrogen-containing silicone oil, and the vinyl silicone oil comprises at least one of a terminal vinyl silicone oil and a multi-vinyl silicone oil.

6. The heat conductive soft glue for laser as claimed in claim 5, wherein The terminal hydrogen-containing silicone oil has a silicon-hydrogen content of 0.3-0.8 mmol / g and a viscosity of 50-200 cps at 25 ℃, and the multi-hydrogen-containing silicone oil has a silicon-hydrogen content of 0.5-1.5 mmol / g and a viscosity of 30-200 cps at 25 ℃.

7. The heat conductive soft glue for laser as claimed in claim 5, wherein The terminal vinyl silicone oil has a vinyl content of 0.3-1.0 mmol / g and a viscosity of 50-25000 cps at 25 ℃, and the multi-vinyl silicone oil has a vinyl content of 1.5-2.1 mmol / g and a viscosity of 5000-10000 cps at 25 ℃.

8. The heat conductive soft glue for laser according to claim 1, wherein The first coupling agent and the second coupling agent each comprise a silane coupling agent and a silicate coupling agent, and the weight ratio of the silane coupling agent to the silicate coupling agent is 1:(1-3).

9. The heat conductive soft glue for laser according to claim 1, wherein The catalyst is a platinum-gold catalyst, and the content of the platinum-gold catalyst in the heat-conducting soft glue for laser is 4000-6000 ppm.

10. A method of producing the heat conductive soft glue for laser according to any one of claims 1 to 9, characterized by, The method comprises the following steps: The first silicone oil, the first alumina and the first coupling agent are mixed and stirred, heated to 110-130 ℃, vacuumized and mixed, and the A component masterbatch is prepared after cooling; The second silicone oil, the second alumina and the second coupling agent are mixed and stirred, heated to 110-130 ℃, vacuumized and mixed, and the B component masterbatch is prepared after cooling; The catalyst is added to the A component masterbatch at room temperature, vacuumized and mixed to obtain the A component; The inhibitor is added to the B component masterbatch at room temperature, vacuumized and mixed to obtain the B component; The A component and the B component are mixed uniformly according to the weight ratio, degassed, cured and the heat-conducting soft glue for laser is obtained.

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