A pluggable, low-thermal-resistance phase-change heat-conducting film material and a preparation method thereof

Abstract

The application discloses a kind of phase change heat-conducting film material of resistance to plug, low thermal resistance and preparation method thereof, including the protective film of sequentially adhering, phase change material and metal foil, the phase change material includes by mass fraction: 2~3 portions premix glue, 55~75 portions aluminum powder, 20~30 portions zinc oxide, 0.5~1.5 portions phase change wax, 0.05~1.15 portions antioxidant, 0.3~0.6 portions coupling agent, 1.2~2.5 portions paraffin oil, 0~0.4 portions first antioxidant;The premix glue includes by mass fraction: 15~20 portions styrene-butadiene block copolymer, 10~15 portions polyisobutylene, 5~8 portions plasticizer, 20~30 portions tackifying resin, 45~50 portions paraffin oil, 0.5~1 portions second antioxidant.The scheme of metal foil+phase change material has higher puncture resistance and tear resistance, better heat gain is obtained, service life is improved, and the heat dissipation demand of optical module is met.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of heat-conducting materials, and particularly relates to a pluggable and low-thermal-resistance phase-change heat-conducting film material and a preparation method thereof. BACKGROUND

[0002] With the development of 5G technology, the demand for application scenarios in the field of data communication is also rapidly iterating, and the daily maintenance and expansion of modules have put forward higher requirements for the installation and removal (insertion force and pull-out force) of the port optical module of electronic products and the heat dissipation performance. At the same time, with the development of large-scale application requirements of devices, the increase of power consumption will inevitably lead to an increase in the overall heat generation of the module, so how to solve the heat dissipation demand of the module and meet the pluggable performance has become an important problem.

[0003] The existing common scheme adopts a phase-change material + PI (polyimide) film for heat dissipation, however, the phase-change heat-conducting material attached to the optical film block will contact the metal socket and produce scratches during installation and removal, and the phase-change material + PI film has poor puncture and tear resistance and low heat yield, which leads to the inability to simultaneously meet the multiple disassembly and heat dissipation requirements.

[0004] Therefore, the prior art still needs to be improved and developed. SUMMARY

[0005] In view of the above problems of the prior art, the present application aims to provide a pluggable and low-thermal-resistance phase-change heat-conducting film material and a preparation method thereof, and aims to solve the problem that the existing phase-change material + PI film cannot simultaneously meet the multiple disassembly and heat dissipation requirements.

[0006] The technical scheme adopted by the present application to solve the above technical problems is as follows:

[0007] A pluggable and low-thermal-resistance phase-change heat-conducting film material, comprising, in sequence, a protective film, a phase-change material and a metal foil, wherein the phase-change material comprises, in terms of mass fraction, 2-3 parts of a premixed glue, 55-75 parts of aluminum powder, 20-30 parts of zinc oxide, 0.5-1.5 parts of a phase-change wax, 0.05-1.15 parts of an antioxidant, 0.3-0.6 parts of a coupling agent, 1.2-2.5 parts of paraffin oil and 0-0.4 parts of a first antioxidant.

[0008] The premixed glue comprises, in terms of mass fraction, 15-20 parts of a styrene-butadiene block copolymer, 10-15 parts of polyisobutylene, 5-8 parts of a plasticizer, 20-30 parts of an adhesion resin, 45-50 parts of paraffin oil and 0.5-1 part of a second antioxidant.

[0009] The plug-resistant, low-thermal-resistance phase change heat-conducting film material, wherein the aluminum powder comprises 40-50 parts of aluminum powder of a first particle size and 5-25 parts of aluminum powder of a second particle size, the first particle size is 7.5-10 μm, and the second particle size is 1-5 μm.

[0010] The plug-resistant, low-thermal-resistance phase change heat-conducting film material, wherein the phase change wax is 54° full refined paraffin wax; the antioxidant is antioxidant RD or antioxidant RD and antioxidant 6PPD; and the coupling agent is siloxane coupling agent.

[0011] The plug-resistant, low-thermal-resistance phase change heat-conducting film material, wherein the antioxidant comprises one or both of antioxidant 1076 and antioxidant 168; and the second antioxidant is antioxidant 264.

[0012] The plug-resistant, low-thermal-resistance phase change heat-conducting film material, wherein the plasticizer is selected from one or more of ortho-dimethylate, diisodecyl phthalate, straight-chain alcohol ester, fatty acid ester, epoxy ester, trimellitate ester, and phosphate ester.

[0013] The plug-resistant, low-thermal-resistance phase change heat-conducting film material, wherein the tackifying resin is selected from one or more of C5 petroleum resin, C9 petroleum resin, DCPD resin, alkyl phenol-formaldehyde resin, and xylene resin.

[0014] The plug-resistant, low-thermal-resistance phase change heat-conducting film material, wherein the metal foil is selected from one or more of copper foil, aluminum foil, stainless steel foil, PI-coated copper foil, PI-coated aluminum foil, and PI-coated stainless steel foil; and the protective film is selected from one of PET release film, PE film, and release paper.

[0015] The preparation method of the plug-resistant, low-thermal-resistance phase change heat-conducting film material, comprising the steps of:

[0016] The styrene-butadiene block copolymer, polyisobutylene, plasticizer, tackifying resin, and paraffin oil and second antioxidant are mixed and subjected to first stirring treatment at a first predetermined temperature to obtain a premixing glue;

[0017] The premixing glue is mixed with aluminum powder, zinc oxide, phase change wax, antioxidant, coupling agent, paraffin oil, and first antioxidant and subjected to second stirring treatment at a second predetermined temperature to obtain the phase change material;

[0018] The phase change material is subjected to calendering treatment and die cutting treatment, and a protective film is attached to the phase change material to obtain a semi-finished product with back glue;

[0019] The semi-finished product with back glue is attached to a metal foil to obtain the plug-resistant, low-thermal-resistance phase change heat-conducting film material.

[0020] The method, wherein the first predetermined temperature is 120-140 DEG C; the first stirring treatment is specifically: stirring at 20-30 r / min for 20 min, stirring at 40-50 r / min for 30 min, stirring at 100-110 r / min for 180 min, cooling to 100 DEG C and stirring at 40-50 r / min for 110 min.

[0021] The method, wherein the second predetermined temperature is 120-140 DEG C; the second stirring treatment is specifically: stirring at 8-15 r / min for 60-70 min, stirring at 25-30 r / min for 10-15 min, and dispersing at 2500-3000 r / min for 120-140 min.

[0022] Beneficial effects: the application discloses a phase-change heat-conducting film material with plugging resistance and low thermal resistance and a preparation method thereof, the scheme of metal foil+phase-change material has high puncture resistance and tear resistance, can meet the needs of multiple installation and dismounting of the optical module without damage, and can phase change during work after the phase-change material is combined with the metal foil, fill space gaps, minimize thermal resistance, continuously transfer heat, improve heat dissipation effect, thereby achieving good heat benefits, maintaining the working temperature of the whole optical module at a proper level, improving the service life of the optical module, and meeting the heat dissipation needs of the optical module; further, the molecular chains of paraffin oil, styrene-butadiene block copolymer, polyisobutylene and tackifying resin in the phase-change material are intertwined with each other to form a network structure, aluminum powder and zinc oxide powder are dispersed in the network structure, and are closely connected and inlaid in the skeleton of the network structure, so that the components play a synergistic effect in the heat conduction performance, the hardness of the finished product and the viscosity after phase change can be controlled by adjusting the proportion of paraffin oil, styrene-butadiene block copolymer, polyisobutylene and tackifying resin; the phase-change heat-conducting film material is a good conductor of heat, the flame retardant level can reach V0, the insulation is excellent, and efficient heat management of the optical module and other components in the switch can be realized. BRIEF DESCRIPTION OF DRAWINGS

[0023] Figure 1 It is a structure schematic diagram of the phase-change heat-conducting film material with plugging resistance and low thermal resistance.

[0024] Figure 2 It is a flow chart of the preparation method of the phase-change heat-conducting film material with plugging resistance and low thermal resistance.

[0025] Figure 3 It is a use schematic diagram of the phase-change heat-conducting film material with plugging resistance and low thermal resistance. DETAILED DESCRIPTION

[0026] The present application provides a pluggable, low thermal resistance phase change heat conducting film material and a preparation method thereof. To make the purpose, technical solutions and effects of the present application clearer and more explicit, the present application is further described in detail below with reference to the drawings and examples. It should be understood that the specific examples described herein are only used to explain the present application and do not limit the present application.

[0027] Those skilled in the art can understand that the singular forms "a", "an" and "the" used herein include plural forms unless specifically stated otherwise. It should be further understood that the use of the term "including" in the specification of the present application means that the described features, integers, steps, operations, elements, and / or components exist, but do not exclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups thereof. Those skilled in the art can understand that unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as that generally understood by those skilled in the art to which the present application belongs. It should also be understood that terms such as those defined in general dictionaries should be understood to have meanings consistent with those in the context of the prior art, and unless specifically defined as such, should not be interpreted in an idealized or overly formal sense.

[0028] With the development of 5G technology, the demand for application scenarios in the field of data communication is also rapidly iterating, and the daily maintenance and expansion of modules put forward higher requirements for the installation and removal (insertion force and pull-out force) and heat dissipation performance of the port optical module of electronic products. The existing common solution uses phase change material + PI (polyimide) film for heat dissipation. However, the phase change heat conducting material attached to the optical film block will contact the metal socket and produce scratches during installation and removal, and the phase change material + PI film has poor puncture and tear resistance, and low heat gain, which makes it unable to meet the requirements of multiple disassembly and heat dissipation at the same time.

[0029] Based on this, the present application provides a pluggable, low thermal resistance phase change heat conducting film material 10, see Figure 1 which comprises a protective film 11, a phase change material 12 and a metal foil 13 attached in sequence, the phase change material comprises, by mass fraction: 2-3 parts of premixed glue, 55-75 parts of aluminum powder, 20-30 parts of zinc oxide, 0.5-1.5 parts of phase change wax, 0.05-1.15 parts of antioxidant, 0.3-0.6 parts of coupling agent, 1.2-2.5 parts of paraffin oil, and 0-0.4 parts of first antioxidant.

[0030] The premixed glue comprises, in terms of mass fraction, 15-20 parts of styrene-butadiene block copolymer, 10-15 parts of polyisobutylene, 5-8 parts of plasticizer, 20-30 parts of tackifying resin, 45-50 parts of paraffin oil, and 0.5-1 part of second antioxidant.

[0031] Specifically, the present application has higher puncture resistance and tear resistance by adopting the scheme of metal foil + phase change material, can meet the needs of multiple installation and disassembly of optical modules without damage, and the phase change material can phase change during work after being compounded with the metal foil, fill the space gap, minimize the thermal resistance, continuously transfer heat, improve the heat dissipation effect, thereby achieving good heat benefits, maintaining the working temperature of the entire optical module at a suitable level, improving the service life of the optical module, and meeting the heat dissipation needs of the optical module; further, the molecular chains of the paraffin oil, styrene-butadiene block copolymer, polyisobutylene, and tackifying resin in the phase change material in the present application are intertwined with each other to form a network structure, the aluminum powder and zinc oxide powder are dispersed therein, and are closely connected and inlaid in the skeleton of the space network structure, so that the components play a synergistic effect in the thermal conductivity; the proportion of the paraffin oil, styrene-butadiene block copolymer, polyisobutylene, and tackifying resin can be adjusted to control the hardness of the finished product and the viscosity after phase change; the phase change thermal conductive film material of the present application is a good thermal conductor, the flame retardant level can reach V0, and the insulation is excellent, so that efficient thermal management of optical modules and other components in the switch can be realized.

[0032] With the increase of temperature, when the designed temperature (40-50℃) of the phase change material is reached, the crosslinked and intertwined polymer softens, the flowability is enhanced, the phase change material changes from solid to viscous, the flowability of the phase change material is improved, the gap between the components can be filled, the phase change material and the components are fully attached, the dispersed thermal conductive powder in the phase change material has a certain flowability, can better contact the components, and the heat conduction efficiency at the gap is improved; the attachment is sufficient, the contact resistance is reduced, and the heat conduction efficiency is greatly improved. Even in the case of becoming viscous, the crosslinked and intertwined polymer is not easy to overflow, and the safety and insulation between the components can be ensured. The heat generated by the components is transmitted to the heat dissipation device, the temperature of the components tends to be stable, and the working stability of the components is ensured. Even in a low temperature environment, the conduction efficiency of the low thermal resistance phase change thermal conductive material is high, and the reliability and stability of the components can be improved.

[0033] In some embodiments, the aluminum powder is used as a high-thermal-conductivity filler, and includes 40-50 parts by mass of aluminum powder of a first particle size and 5-25 parts by mass of aluminum powder of a second particle size, wherein the first particle size is 7.5-10 μm and the second particle size is 1-5 μm; preferably, the aluminum powder of the first particle size is M-AG-7.5 (aluminum powder of 7.5 μm) and the aluminum powder of the second particle size is M-AG-1 (aluminum powder of 1 μm); the use of two particle sizes of aluminum powder can better fill the gaps of large particle sizes and improve the thermal conductivity of the aluminum powder compared to the use of a single particle size of aluminum powder.

[0034] In some embodiments, the phase-change wax is 54° fully refined paraffin wax (54# phase-change wax) that melts at 54°C and is used to adjust the phase-change temperature of the phase-change material; the antioxidant is antioxidant RD (2,2,4-trimethyl-1,2-dihydroquinoline polymer) or antioxidant RD and antioxidant 6PPD (N-(1,3-dimethylbutyl)-N'-phenyl-p-phenylenediamine); and the coupling agent is a siloxane coupling agent.

[0035] In some embodiments, the antioxidant includes one or both of antioxidant 1076 (β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid n-octadecyl ester, molecular formula C 35 H 62 O3) and antioxidant 168 (a phosphite antioxidant with excellent performance, molecular formula C 42 H 63 O3P); antioxidant 1076 and antioxidant 168 have a good synergistic effect and can effectively prevent thermal degradation of the polymer and provide long-term protection for the polymer; and the second antioxidant is antioxidant 264 (2,6-di-tert-butyl-p-cresol) that can inhibit oxidative degradation of the film material and thus prolong the service life of the film material.

[0036] In some embodiments, the plasticizer is selected from one or more of ortho-dicarboxylic acid esters, diisodecyl phthalate, straight-chain alcohol esters, fatty acid esters, epoxy esters, trimellitate esters, and phosphate esters.

[0037] In some embodiments, the tackifying resin is selected from one or more of C5 petroleum resin, C9 petroleum resin, DCPD (dicyclopentadiene) resin, alkyl phenol-formaldehyde resin, and xylene resin.

[0038] In some embodiments, the metal foil is selected from one or more of copper foil, aluminum foil, stainless steel foil, PI-coated copper foil, PI-coated aluminum foil, and PI-coated stainless steel foil; and the protective film is selected from one of PET (polyethylene terephthalate) release film, PE (polyethylene) film, and release paper.

[0039] The application further provides a preparation method of the plug-resistant and low-thermal-resistance phase change heat-conducting film material. Figure 2 which comprises the following steps:

[0040] S10, mixing styrene-diene block copolymer, polyisobutylene, plasticizer, tackifying resin and paraffin oil, and second antioxidant, and then performing first stirring treatment at a first predetermined temperature to obtain premix glue;

[0041] S20, performing second stirring treatment on the premix glue and aluminum powder, zinc oxide, phase change wax, antioxidant, coupling agent, paraffin oil and first antioxidant at a second predetermined temperature to obtain the phase change material;

[0042] S30, performing calendering treatment and die cutting treatment on the phase change material to attach a protective film to the phase change material to obtain a semi-finished product with back glue;

[0043] S40, attaching the semi-finished product with back glue to a metal foil to obtain the plug-resistant and low-thermal-resistance phase change heat-conducting film material.

[0044] In some embodiments, the first predetermined temperature is 120-140℃; and the first stirring treatment specifically comprises: stirring at a speed of 20-30r / min for 20min, stirring at a speed of 40-50r / min for 30min, and stirring at a speed of 100-110r / min for 180min, and then cooling to 100℃ and stirring at a speed of 40-50r / min for 110min.

[0045] Specifically, the step S10 specifically comprises: preheating a planetary stirrer to a first predetermined temperature, and then sequentially adding styrene-diene block copolymer, polyisobutylene, plasticizer, tackifying resin, paraffin oil and second antioxidant into the planetary stirrer for mixing, and then sequentially stirring at a speed of 20-30r / min for 20min, stirring at a speed of 40-50r / min for 30min, and stirring at a speed of 100-110r / min for 60min, stopping, scraping (dispersing disc), continuing to stir at a speed of 100-110r / min for 60min, stopping, scraping (dispersing disc and cylinder bottom), and then continuing to stir at a speed of 100r / min for 60min; reducing the stirring speed to 40r / min and the temperature to 100℃, and then stirring for 110min, and at the same time, opening a vacuum pump to achieve a vacuum degree of 0.095Mpa or above, and keeping the vacuum degree unchanged to obtain premix glue.

[0046] In some embodiments, the second predetermined temperature is 120-140℃; and the second stirring treatment is specifically: stirring at a speed of 8-15r / min for 60-70min, stirring at a speed of 25-30r / min for 10-15min, and dispersing at a speed of 2500-3000r / min for 120-140min.

[0047] Specifically, the step S20 is specifically: adding the premixed glue, aluminum powder, zinc oxide, phase change wax, antioxidant, coupling agent, paraffin oil and first antioxidant into a preheated planetary mixer for stirring, at a speed of 8-15r / min, for 60-70min; after the end, increasing the speed to 25-30r / min, stirring for 10-15min, stopping and scraping; after scraping is completed, adjusting the stirring speed to 80-110r / min, dispersing at a speed of 2500-3000r / min, stirring and dispersing for 1h, stopping and scraping; starting vacuumizing and continuing stirring and dispersing for 60-80min, with stopping and scraping once at 35min and 70min, to obtain the phase change material.

[0048] In some embodiments, the step S30 is specifically: performing calendering treatment on the phase change material by using a precision calendering machine, cutting into a predetermined size by using a small-hole die cutting machine, and attaching a protective film with adhesive, to obtain a semi-finished product with adhesive; wherein the parameters of the calendering treatment are: the roller temperature is 100℃, the roller linear speed is 1m / min, the pressure is 10Mpa, and the upper and lower deviation pressure is 0.2Mpa.

[0049] In some embodiments, the step S40 is specifically: manually assembling and attaching the semi-finished product with adhesive with a metal foil, to obtain the plug-resistant and low-thermal-resistance phase change heat-conducting film material.

[0050] Figure 3 A schematic diagram for use of the plug-resistant and low-thermal-resistance phase change heat-conducting film material is shown in the figure, which is arranged between an optical module 20 and a switch heat sink 30; in use, the protective film 11 with adhesive is torn off, and the plug-resistant and low-thermal-resistance phase change heat-conducting film material is attached on the optical module, and the metal foil 13 is in contact with the switch heat sink 30 for heat conduction.

[0051] The technical solutions in the embodiments of the present application will be clearly and completely described in combination with the accompanying drawings of the embodiments of the present application. Obviously, the described embodiments are only some of the embodiments of the present application, rather than all the embodiments, and are only used to illustrate the present application, but not to limit the present application. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0052] Unless otherwise specified, all of the reagents and raw materials used in the present application are commercially available or can be prepared by known methods.

[0053] Example 1

[0054] The planetary mixer was preheated to 130°C, and after the temperature was stabilized, 16 parts of styrene-diene block copolymer, 9 parts of polyisobutylene, 5 parts of plasticizer, 26 parts of tackifying resin, 45 parts of paraffin oil, 1 part of antioxidant 264 were weighed in sequence and added to the planetary mixer, and the stirring speed was 20 r / min, and stirring was performed for 20 min; the stirring speed was adjusted to 40 r / min, and stirring was performed for 30 min; the stirring speed was adjusted to 100 r / min, and stirring was performed for 60 min, and the machine was stopped and the material was scraped (dispersion disc); the stirring was continued at 100 r / min for 60 min, the machine was stopped, and the material was scraped (dispersion disc and cylinder bottom); the stirring was continued at 100 r / min for 60 min; the stirring speed was reduced to 40 r / min, and the temperature was reduced to 100°C, and stirring was performed for 110 min, and at the same time, vacuum was applied, and the vacuum degree was above 0.095 MPa, and the vacuum degree was kept constant, and the premixed glue was obtained for standby use.

[0055] The premixed glue 2.5 parts; M-AG-7.5, 47 parts; M-AG-1, 20 parts; ZnO-0.6, 26 parts; 54# phase change wax, 1 part; antioxidant RD, 0.1 part; siloxane coupling agent, 0.5 parts; paraffin oil 2 parts were added to the preheated planetary mixer and stirred at a speed of 15 r / min for 70 min; after the end, the stirring speed was increased to 30 r / min, and stirring was performed for 15 min, the machine was stopped, and the material was scraped; after the scraping was completed, the stirring speed was adjusted to 110 r / min, the dispersion speed was 3000 r / min, and stirring and dispersion were performed for 1 h, the machine was stopped, and the material was scraped; vacuum was applied, and stirring and dispersion were continued for 80 min, and during this period, the machine was stopped and the material was scraped at 35 min and 70 min, respectively; finally, after the mixture was observed to be fully mixed and uniform, the material was discharged for standby use.

[0056] Example 2

[0057] The planetary mixer is preheated to 130°C, after the temperature is stabilized, the following ingredients are weighed in order: styrene-butadiene block copolymer 16 parts, polyisobutylene 9 parts, plasticizer 5 parts, tackifying resin 26 parts, paraffin oil 45 parts, antioxidant 264 1 part, and then added into the planetary mixer, stirring speed 20 r / min, stirring for 20 min; the stirring speed is adjusted to 40 r / min, stirring for 30 min; the stirring speed is adjusted to 100 r / min, stirring for 60 min, stop, scraping (dispersion disc); continue stirring at 100 r / min for 60 min, stop, scraping (dispersion disc and cylinder bottom); continue stirring at 100 r / min for 60 min; the stirring speed is reduced to 40 r / min, the temperature is reduced to 100°C, stirring for 110 min, while stirring, vacuum is started, the vacuum degree is above 0.095 MPa, the vacuum degree is kept unchanged, and the premixed glue is obtained for standby use.

[0058] The following ingredients are added into the preheated planetary mixer: premixed glue 2.5 parts; M-AG-7.5, 47 parts; M-AG-1, 20 parts; ZnO-0.6, 26 parts; 54# phase change wax, 1 part; antioxidant RD, 0.1 part; siloxane coupling agent, 0.5 part; paraffin oil 2 parts; antioxidant 1076, 0.15 part; antioxidant 168, 0.05 part, stirring speed 8-15 r / min, stirring time 60-70 min; after the stirring is finished, the stirring speed is increased to 30 r / min, stirring for 15 min, stop, scraping; after the scraping is finished, the stirring speed is adjusted to 110 r / min, dispersion speed 3000 r / min, stirring and dispersion for 1 h, stop, scraping; vacuum is started, continue stirring and dispersion for 80 min, during which the stirring is stopped and scraped once at 35 min and 70 min, finally the mixture is observed to be fully mixed and uniform, and then discharged for standby use.

[0059] Example 3

[0060] The planetary mixer is preheated to 130°C, after the temperature is stabilized, the following ingredients are weighed in order: styrene-butadiene block copolymer 16 parts, polyisobutylene 9 parts, plasticizer 5 parts, tackifying resin 26 parts, paraffin oil 45 parts, antioxidant 264 1 part, and then added into the planetary mixer, stirring speed 20 r / min, stirring for 20 min; the stirring speed is adjusted to 40 r / min, stirring for 30 min; the stirring speed is adjusted to 100 r / min, stirring for 60 min, stop, scraping (dispersion disc); continue stirring at 100 r / min for 60 min, stop, scraping (dispersion disc and cylinder bottom); continue stirring at 100 r / min for 60 min; the stirring speed is reduced to 40 r / min, the temperature is reduced to 100°C, stirring for 110 min, while stirring, vacuum is started, the vacuum degree is above 0.095 MPa, the vacuum degree is kept unchanged, and the premixed glue is obtained for standby use.

[0061] The premix 2.5 parts; M-AG-7.5, 50 parts; M-AG-1, 17 parts; ZnO-0.6, 26 parts; 54# phase change wax, 1 part; antioxidant RD, 0.1 part; siloxane coupling agent, 0.5 parts; paraffin oil 2 parts; antioxidant 1076, 0.15 parts, antioxidant 168, 0.05 parts are added to the preheated planetary mixer and stirred at a speed of 15 r / min for 70 min; after the end, the speed is increased to 30 r / min, and stirring is carried out for 10-15 min, the machine is stopped and the material is scraped; after scraping, the stirring speed is adjusted to 110 r / min, the dispersion speed is 3000 r / min, and stirring and dispersion are carried out for 1 h, the machine is stopped, and the material is scraped; vacuum is opened and stirring and dispersion are continued for 80 min, and the machine is stopped and scraped at 35 min and 70 min respectively; finally, after the mixture is observed to be fully mixed and uniform, the material is discharged for standby.

[0062] Example 4

[0063] The planetary mixer is preheated to 130°C, and after the temperature is stabilized, styrene-butadiene block copolymer 16 parts, polyisobutylene 9 parts, plasticizer 5 parts, tackifying resin 26 parts, paraffin oil 45 parts, antioxidant 264, 1 part are weighed and added to the planetary mixer, and stirring is carried out at a speed of 20 r / min for 20 min; the speed is adjusted to 40 r / min, and stirring is carried out for 30 min; the speed is adjusted to 100 r / min, and stirring is carried out for 60 min, the machine is stopped, and the material is scraped (dispersion disc); continue stirring at 100 r / min for 60 min, stop the machine, and scrape (dispersion disc and cylinder bottom); continue stirring at 100 r / min for 60 min; reduce the speed to 40 r / min, and reduce the temperature to 100°C, and stir for 110 min; at the same time, vacuum is opened, the vacuum degree is above 0.095 Mpa, the vacuum degree is kept unchanged, and the premix is obtained for standby.

[0064] The premix 2.5 parts; M-AG-7.5, 47 parts; M-AG-1, 20 parts; ZnO-0.6, 26 parts; 54# phase change wax, 1 part; antioxidant RD, 0.1 part; siloxane coupling agent, 0.5 parts; paraffin oil 2 parts are added to the preheated planetary mixer and stirred at a speed of 15 r / min for 70 min; after the end, the speed is increased to 30 r / min, and stirring is carried out for 15 min, the machine is stopped and the material is scraped; after scraping, the stirring speed is adjusted to 110 r / min, the dispersion speed is 3000 r / min, and stirring and dispersion are carried out for 1 h, the machine is stopped, and the material is scraped; vacuum is opened and stirring and dispersion are continued for 80 min, and the machine is stopped and scraped at 35 min and 70 min respectively; finally, after the mixture is observed to be fully mixed and uniform, the material is discharged for standby.

[0065] Example 5

[0066] The planetary mixer is preheated to 130°C, after the temperature is stable, the following ingredients are weighed in order: styrene-butadiene block copolymer 16 parts, polyisobutylene 9 parts, plasticizer 5 parts, tackifying resin 26 parts, paraffin oil 45 parts, antioxidant 264 1 part, and then added into the planetary mixer, stirring speed 20 r / min, stirring for 20 min; the stirring speed is adjusted to 40 r / min, stirring for 30 min; the stirring speed is adjusted to 100 r / min, stirring for 60 min, stop, scraping (dispersion disc); continue stirring at 100 r / min for 60 min, stop, scraping (dispersion disc and cylinder bottom); continue stirring at 100 r / min for 60 min; the stirring speed is reduced to 40 r / min, the temperature is reduced to 100°C, stirring for 110 min, while stirring, vacuum is started, the vacuum degree is above 0.095 MPa, the vacuum degree is kept unchanged, and the premixed glue is obtained for standby use.

[0067] The following ingredients are added into the preheated planetary mixer: premixed glue 2.5 parts; M-AG-7.5, 47 parts; M-AG-1, 20 parts; ZnO-0.6, 26 parts; 54# phase change wax, 1 part; antioxidant RD, 0.1 part; siloxane coupling agent, 0.4 part; paraffin oil 2 parts; antioxidant 1076, 0.1 part; antioxidant 168, 0.1 part, stirring speed 15 r / min, stirring time 70 min; after the stirring is finished, the stirring speed is increased to 30 r / min, stirring for 15 min, stop, scraping; after the scraping is finished, the stirring speed is adjusted to 110 r / min, dispersion speed 3000 r / min, stirring and dispersion for 1 h, stop, scraping; vacuum is started, continue stirring and dispersion for 80 min, during which the stirring is stopped and scraped at 35 min and 70 min respectively, finally the mixture is observed to be fully mixed and uniform, and then discharged for standby use.

[0068] Example 6

[0069] The planetary mixer is preheated to 130°C, after the temperature is stable, the following ingredients are weighed in order: styrene-butadiene block copolymer 16 parts, polyisobutylene 9 parts, plasticizer 5 parts, tackifying resin 26 parts, paraffin oil 45 parts, antioxidant 264 1 part, and then added into the planetary mixer, stirring speed 20 r / min, stirring for 20 min; the stirring speed is adjusted to 40 r / min, stirring for 30 min; the stirring speed is adjusted to 100 r / min, stirring for 60 min, stop, scraping (dispersion disc); continue stirring at 100 r / min for 60 min, stop, scraping (dispersion disc and cylinder bottom); continue stirring at 100 r / min for 60 min; the stirring speed is reduced to 40 r / min, the temperature is reduced to 100°C, stirring for 110 min, while stirring, vacuum is started, the vacuum degree is above 0.095 MPa, the vacuum degree is kept unchanged, and the premixed glue is obtained for standby use.

[0070] The premix glue 2.5 parts; M-AG-7.5, 46 parts; M-AG-1, 20.5 parts; ZnO-0.6, 25.5 parts; 54# phase change wax, 1.2 parts; antioxidant RD, 0.05 parts; siloxane coupling agent, 0.5 parts; paraffin oil 1.9 parts; antioxidant 6PPD, 0.05 parts; are added to the preheated planetary mixer stirring, speed 15r / min, stirring time is 70min; after the end, the speed is increased to 30r / min, stirring 15min, stop, scraping; after scraping is completed, the stirring speed is adjusted to 110r / min, dispersion speed 3000r / min, stirring dispersion 1h, stop, scraping; open vacuum continue to stir dispersion 80min, in 35min and 70min stop scraping each time, finally observed that the mixture has been fully mixed uniform after discharge for standby.

[0071] Example 7

[0072] The planetary stirring is preheated to 130℃, after the temperature is stable, the styrene-butadiene block copolymer 16 parts, polyisobutylene 9 parts, plasticizer 5 parts, tackifying resin 26 parts, paraffin oil 45 parts, antioxidant 264, 1 part are weighed in turn, added to the planetary mixer, stirring speed 20r / min, stirring 20min; the speed is adjusted to 40r / min, stirring 30min; the speed is adjusted to 100r / min, stirring 60min, stop, scraping (dispersion disc); continue 100r / min, stirring 60min, stop, scraping (dispersion disc and cylinder bottom); continue 100r / min, stirring 60min; the speed is reduced to 40r / min, the temperature is reduced to 100℃, stirring 110min, while stirring, open vacuum, vacuum degree is above 0.095Mpa, keep the vacuum degree unchanged, get premix glue standby.

[0073] The premix glue 2.5 parts; M-AG-7.5, 46 parts; M-AG-1, 20.5 parts; ZnO-0.6, 25.5 parts; 54# phase change wax, 1.2 parts; antioxidant RD, 0.05 parts; siloxane coupling agent, 0.4 parts; paraffin oil 1.9 parts; antioxidant 6PPD, 0.05 parts; are added to the preheated planetary mixer stirring, speed 15r / min, stirring time is 70min; after the end, the speed is increased to 30r / min, stirring 15min, stop, scraping; after scraping is completed, the stirring speed is adjusted to 110r / min, dispersion speed 3000r / min, stirring dispersion 1h, stop, scraping; open vacuum continue to stir dispersion 80min, in 35min and 70min stop scraping each time, finally observed that the mixture has been fully mixed uniform after discharge for standby.

[0074] Example 8

[0075] The planetary mixer was preheated to 130°C, and after the temperature was stabilized, 16 parts of styrene-butadiene block copolymer, 9 parts of polyisobutylene, 5 parts of plasticizer, 26 parts of tackifying resin, and 45 parts of paraffin oil were weighed in sequence and added to the planetary mixer, with a stirring speed of 20 r / min, and stirred for 20 min; the stirring speed was adjusted to 40 r / min, and stirred for 30 min; the stirring speed was adjusted to 100 r / min, and stirred for 60 min, and then stopped and scraped (dispersion disc); the stirring was continued at 100 r / min for 60 min, and then stopped and scraped (dispersion disc and cylinder bottom); the stirring was continued at 100 r / min for 60 min; the stirring speed was reduced to 40 r / min, and the temperature was reduced to 100°C, and stirred for 110 min, while vacuum was started, and the vacuum degree was kept above 0.095 MPa, to obtain a premixed glue for standby use.

[0076] The premixed glue 2.5 parts; M-AG-7.5, 50 parts; M-AG-1, 17 parts; ZnO-0.6, 26 parts; 54# phase change wax, 1.2 parts; antioxidant RD, 0.05 parts; siloxane coupling agent, 0.4 parts; paraffin oil 1.9 parts; antioxidant 6PPD, 0.05 parts; were added to the preheated planetary mixer and stirred at a speed of 15 r / min for 70 min; after the stirring was completed, the stirring speed was increased to 30 r / min, and stirred for 15 min, and then stopped and scraped; after the scraping was completed, the stirring speed was adjusted to 110 r / min, and the dispersion speed was 3000 r / min, and stirred and dispersed for 1 h, and then stopped and scraped; vacuum was started and the stirring and dispersion were continued for 80 min, during which the stirring was stopped and scraped at 35 min and 70 min, respectively; finally, after the mixture was observed to be fully mixed and uniform, the mixture was discharged for standby use.

[0077] Example 9

[0078] The planetary mixer was preheated to 130°C, and after the temperature was stabilized, 16 parts of styrene-butadiene block copolymer, 9 parts of polyisobutylene, 5 parts of plasticizer, 26 parts of tackifying resin, and 45 parts of paraffin oil were weighed in sequence and added to the planetary mixer, with a stirring speed of 20 r / min, and stirred for 20 min; the stirring speed was adjusted to 40 r / min, and stirred for 30 min; the stirring speed was adjusted to 100 r / min, and stirred for 60 min, and then stopped and scraped (dispersion disc); the stirring was continued at 100 r / min for 60 min, and then stopped and scraped (dispersion disc and cylinder bottom); the stirring was continued at 100 r / min for 60 min; the stirring speed was reduced to 40 r / min, and the temperature was reduced to 100°C, and stirred for 110 min, while vacuum was started, and the vacuum degree was kept above 0.095 MPa, to obtain a premixed glue for standby use.

[0079] Premix 2.5 parts; M-AG-7.5, 50 parts; M-AG-1, 17 parts; ZnO-0.6, 26 parts; 54# phase change wax, 0.5-1 part; antioxidant RD, 0.05 part; siloxane coupling agent, 0.5 part; paraffin oil 1 part; antioxidant 6PPD, 0.05 part; added to the preheated planetary mixer, stirring speed 15 r / min, stirring time 70 min; after the end, the stirring speed is increased to 30 r / min, stirring 15 min, stop, scraping; after scraping, the stirring speed is adjusted to 110 r / min, dispersion speed 3000 r / min, stirring and dispersion 1 h, stop, scraping; open vacuum and continue stirring and dispersion 80 min, during which stop scraping twice at 35 min and 70 min, finally observe that the mixture is fully mixed and uniform, then discharge for standby.

[0080] Different formulations are tested for thermal resistance value under the same pressure and temperature by ASTM 5470 Reline thermal conductivity tester, and the test results are shown in Table 1 as follows.

[0081] Table 1 Thermal resistance test results of phase change material of examples 1-9

[0082]

[0083]

[0084] As can be seen from Table 1, the phase change material of the present application has smaller thermal resistance, and has excellent heat conduction and heat dissipation performance.

[0085] The mixture described in Example 9 is passed through a precision calender, and the appropriate temperature, pressure and roller linear speed are set, and the film material of appropriate thickness is calendered, and then the semi-finished product with back glue is cut out by a small hole die cutting machine, and finally the metal foil and the phase change heat conducting film with back glue are pasted together to become a plug-resistant heat conducting film material by manual assembly.

[0086] The results of Table 2 can be obtained by comparing the number of times of insertion and extraction of different metal foils or PI films (insertion and extraction force is set according to the use requirements of optical modules) and the heat gain value measured by temperature sensor.

[0087] Table 2 Number of times of insertion and extraction of different metal foils or PI films and heat gain value

[0088]

[0089] From the comparison of the number of times of insertion and extraction of several metal foils and PI films and the measured heat gain, it can be found that the Cu+ phase change material scheme can well meet the requirements of insertion and extraction of optical modules and heat dissipation.

[0090] In summary, the application discloses a kind of phase change heat-conducting film material and preparation method of low thermal resistance of plug resistance, including the protective film of sequentially pasted, phase change material and metal foil, the phase change material includes by mass fraction: 2-3 parts premix glue, 55-75 parts aluminum powder, 20-30 parts zinc oxide, 0.5-1.5 parts phase change wax, 0.05-1.15 parts antioxidant, 0.3-0.6 parts coupling agent, 1.2-2.5 parts paraffin oil, 0-0.4 parts first antioxidant;Wherein, the premix glue includes by mass fraction: 15-20 parts styrene-butadiene block copolymer, 10-15 parts polyisobutylene, 5-8 parts plasticizer, 20-30 parts tackifying resin, 45-50 parts paraffin oil, 0.5-1 parts second antioxidant.The application has higher puncture resistance and tear resistance by using metal foil+phase change material scheme, can meet the needs of multiple installation and disassembly of optical module without damage, and the phase change material can be phase changed after being combined with metal foil during work, fill space gap, can minimize thermal resistance, continuously transfer heat, improve heat dissipation effect, so as to obtain good heat benefit, so that the working temperature of the whole optical module is maintained at a suitable level, improve the service life of optical module, can meet the heat dissipation needs of optical module;Further, the molecular chains of paraffin oil, styrene-butadiene block copolymer, polyisobutylene, tackifying resin in the phase change material in the application are intertwined, form a network structure, disperse aluminum powder, zinc oxide powder and other powders therein, tightly connect and inlay in the skeleton of space network structure, so that the components play a synergistic effect in thermal conductivity, and the hardness of finished product and viscosity after subsequent phase change can be controlled by adjusting the ratio of paraffin oil, styrene-butadiene block copolymer, polyisobutylene and tackifying resin;The phase change heat-conducting film material of the application is a good conductor of heat, and the flame retardant level can reach V0, and the insulation is excellent, so that efficient thermal management of optical module and other components in switch can be realized.

[0091] Finally, it should be pointed out that: the above examples are only used to illustrate the technical solutions of the application, and not to limit them; although the application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that they can modify the technical solutions recorded in the foregoing examples, or make equivalent replacement for part of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the application.

Claims

1. A low thermal resistance, phase change heat conducting film material that is resistant to plug-in, characterized in that, The phase change material comprises, in mass fraction, 2-3 parts of premixed glue, 55-75 parts of aluminum powder, 20-30 parts of zinc oxide, 0.5-1.5 parts of phase change wax, 0.05-1.15 parts of antioxidant, 0.3-0.6 parts of coupling agent, 1.2-2.5 parts of paraffin oil, and 0-0.4 parts of first antioxidant. The premixed glue comprises, in mass fraction, 15-20 parts of styrene-butadiene block copolymer, 10-15 parts of polyisobutylene, 5-8 parts of plasticizer, 20-30 parts of tackifying resin, 45-50 parts of paraffin oil, and 0.5-1 part of second antioxidant. The aluminum powder comprises, in mass fraction, 40-50 parts of aluminum powder of a first particle size and 5-25 parts of aluminum powder of a second particle size, wherein the first particle size is 7.5-10 μm, and the second particle size is 1-5 μm. The first antioxidant comprises one or both of antioxidant 1076 and antioxidant 168; and the second antioxidant is antioxidant 264.

2. The plug-resistant, low thermal resistance, phase change heat conducting thin film material of claim 1, wherein, The phase change wax is 54° full refined paraffin wax; the antioxidant is antioxidant RD, or antioxidant RD and antioxidant 6PPD; and the coupling agent is siloxane coupling agent.

3. The plug-resistant, low thermal resistance, phase change heat conducting thin film material of claim 1, wherein, The plasticizer is selected from one or more of ortho-dimethylate, diisodecyl phthalate, straight-chain alcohol ester, fatty acid ester, epoxy ester, trimellitate, and phosphate ester.

4. The plug-resistant, low thermal resistance, phase change heat conducting thin film material of claim 1, wherein, The tackifying resin is selected from one or more of C5 petroleum resin, C9 petroleum resin, DCPD resin, alkyl phenol formaldehyde resin, and xylene resin.

5. The plug-resistant, low thermal resistance, phase change heat conducting thin film material of claim 1, wherein, The metal foil is selected from one or more of copper foil, aluminum foil, stainless steel foil, PI-coated copper foil, PI-coated aluminum foil, and PI-coated stainless steel foil; and the protective film is selected from one of PET release film, PE film, and release paper.

6. A method for preparing the plug-resistant, low thermal resistance phase change heat conducting film material according to any one of claims 1-5, characterized in that, The method comprises the steps of: mixing styrene-butadiene block copolymer, polyisobutylene, plasticizer, tackifying resin, paraffin oil, and second antioxidant, and then performing first stirring treatment at a first predetermined temperature to obtain premixed glue; mixing the premixed glue with aluminum powder, zinc oxide, phase change wax, antioxidant, coupling agent, paraffin oil, and first antioxidant, and then performing second stirring treatment at a second predetermined temperature to obtain the phase change material; performing calendering treatment and die cutting treatment on the phase change material to adhere the protective film to the phase change material to obtain a semi-finished product with back glue; adhering the semi-finished product with back glue to a metal foil to obtain the phase change heat-conductive film material with resistance to plugging and low thermal resistance.

7. The method of claim 6, wherein, The first predetermined temperature is 120-140℃; and the first stirring treatment specifically comprises the following steps: stirring at a rotation speed of 20-30 r / min for 20 min, stirring at a rotation speed of 40-50 r / min for 30 min, stirring at a rotation speed of 100-110 r / min for 180 min, cooling to 100℃, and then stirring at a rotation speed of 40-50 r / min for 110 min.

8. The method of claim 6, wherein, The second predetermined temperature is 120-140 DEG C; the second stirring treatment is specifically: stirring at 8-15 r / min for 60-70 min, stirring at 25-30 r / min for 10-15 min, and dispersing at 2500-3000 r / min for 120-140 min.

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