CN107141784A - Heat conducting nano composite material based on polyamide and preparation method thereof - Google Patents

Heat conducting nano composite material based on polyamide and preparation method thereof Download PDF

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CN107141784A
CN107141784A CN201610114926.2A CN201610114926A CN107141784A CN 107141784 A CN107141784 A CN 107141784A CN 201610114926 A CN201610114926 A CN 201610114926A CN 107141784 A CN107141784 A CN 107141784A
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galapectite
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crushing
powder
heat conducting
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彭昌兰
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/06Polyamides derived from polyamines and polycarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08Materials not undergoing a change of physical state when used
    • C09K5/14Solid materials, e.g. powdery or granular
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
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  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention relates to heat conducting nano composite material based on polyamide and preparation method thereof, by weight percentage, including following components:Polyamide 66 40-45%;Silicone resin 12-15%;Thermotropic liquid crystal 13-20%;Nanoscale galapectite powder 20%;Ethylene-propylene non-conjugated diene elastomer graft maleic anhydride 10-17%;Nanoscale galapectite powder is prepared via a method which:Contained brown part in natural galapectite is removed, second of crushing after preliminary crushing, heated-air drying is first carried out;Galapectite powder, distilled water and powdery calgon after crushing is taken to be configured to mixed liquor;50~66 hours are stood again after stirring at normal temperatures;The settled solution heated-air drying after stratification is taken to galapectite into bulk;Block galapectite is crushed, and crosses mesh sieve, nano level pure galapectite powder is obtained.

Description

Heat conducting nano composite material based on polyamide and preparation method thereof
Technical field
It is multiple more specifically to a kind of heat conducting nano based on polyamide the present invention relates to technical field of nano material Condensation material and preparation method thereof.
Background technology
The material of excellent thermal conductivity must possess two conditions:The formation of heat conduction network chain and direction of heat flow and heat conduction in matrix The orientation of network chain is consistent.The main method for industrially preparing heat-conducting plastic at present is the filling high heat conduction component into polymeric matrix To prepare polymer-based composite heat conducting material.By the contact and interaction between the filler of high content, formed in system Similar chain and netted distributional pattern --- heat conduction network chain, so as to improve the thermal conductivity of composite.Conventional inorganic filler For graphite, ceramics, carbon fiber, carbon black, Al2O3, MgO, AlN, BN etc..But, in order that polymer composite is in heat conduction Simultaneously there is insulating properties, be often not added with graphite, carbon black, etc. the high filler of electrical conductivity;And AlN, BN respectively due to its cost compared with High, processing characteristics is bad etc., and factor manufactures inexpensive, high performance moulded heat-conductive insulated plastics so as to be not suitable for industrial production;It is more important , the addition of high amount of inorganic filler, how improve heat conductivity while, as far as possible keep matrix resin other Excellent properties turn into the important directions that heat conductive insulating composite is studied.
The content of the invention
The technical problem to be solved in the present invention is that the drawbacks described above for prior art is multiple there is provided a kind of heat conducting nano Condensation material and preparation method thereof.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of heat conducting nano composite material based on polyamide of construction, it is characterised in that by weight percentage, including with Lower component:
Wherein, the nanoscale galapectite powder is prepared via a method which:By contained brown part in natural galapectite Remove, first carry out preliminary crushing, then heated-air drying is crushed for second after 6~9 hours at 80 DEG C~100 DEG C;Take after crushing Galapectite powder, distilled water and powdery calgon mixed liquor is configured to mass ratio 2-5: 7-10: 0.005~0.03; 50~66 hours are stood again after stirring 16~20 hours at normal temperatures;The settled solution after stratification is taken at 80 DEG C~100 DEG C Lower heated-air drying 11~14 hours is to galapectite into bulk;Block galapectite is crushed, and crosses 50~1500 mesh sieves, nanometer is obtained The pure galapectite powder of level.
Heat conducting nano composite material of the present invention, wherein, by weight percentage, including following components:
Heat conducting nano composite material of the present invention, wherein, by weight percentage, including following components:
Heat conducting nano composite material of the present invention, wherein, by weight percentage, including following components:
Present invention also offers a kind of preparation method of the heat conducting nano composite material based on polyamide, wherein, including with Lower step:
Contained brown part in natural galapectite is removed, preliminary crushing is first carried out, then the hot blast at 80 DEG C~100 DEG C Second of crushing after drying 6~9 hours;
Take crush after galapectite powder, distilled water and powdery calgon with mass ratio 2-5: 7-10: 0.005~ 0.03 is configured to mixed liquor;
50~66 hours are stood again after stirring 16~20 hours at normal temperatures;
Take the heated-air drying 11~14 hours at 80 DEG C~100 DEG C of the settled solution after stratification blocking to galapectite Shape;
Block galapectite is crushed, and crosses 50~1500 mesh sieves, nano level pure galapectite powder is obtained;
After the material vacuum of composite is dried, it is well mixed, extrudes, granulates, is molded, heat conducting nano composite wood is made Material.
Preparation method of the present invention, wherein, take galapectite powder, distilled water and the powdery calgon after crushing Mixed liquor is configured to mass ratio 5: 7: 0.005.
Preparation method of the present invention, wherein, take galapectite powder, distilled water and the powdery calgon after crushing Mixed liquor is configured to mass ratio 2: 9: 0.03.
Preparation method of the present invention, wherein, extruder barrel mouthful temperature is 250 DEG C~260 DEG C, transportation section temperature is 260 DEG C~270 DEG C, compression section temperature be 270 DEG C~290 DEG C, metering section temperature be 290 DEG C~280 DEG C;Nozzle temperature is 275 DEG C~280 DEG C;Screw speed is 180~200r/min;Rate of feeding is 15~20r/min.
Preparation method of the present invention, wherein, injection injecting machine material tube used mouthful temperature is 250 DEG C~260 DEG C, defeated To send a section temperature be 260 DEG C~270 DEG C, compression section temperature is 270 DEG C~290 DEG C, metering section temperature is 290 DEG C~295 DEG C;Nozzle Temperature is 295 DEG C~300 DEG C;Mold temperature is 80 DEG C~100 DEG C;Screw speed is 100~120r/min;It is 60 to inject back pressure ~80Mpa.
Preparation method of the present invention, wherein, it will granulate and dry 10 at 100 DEG C~110 DEG C in vacuum drying chamber Room temperature is cooled to after~12h and under sealing condition.
The beneficial effects of the present invention are:Improve and optimize the preparation technology of existing heat conducting nanometer material, by preparing Nano sized inorganic fillers are with thermotropic liquid crystal and in nylon, preparing and having heat conductivility concurrently and excellent mechanical property IN-SITU HYBRID COMPOSITES, not only enrich the modified method of polyamide, and substantially reduce cost, accelerate In-situ reaction The paces of technology commercialization, effectively solve liquid crystal fancy price, and difficulty realizes industrialized problem.
Embodiment
In order that the purpose, technical scheme and advantage of the embodiment of the present invention are clearer, below in conjunction with present invention implementation Technical scheme in example carries out clear, complete description, it is clear that described embodiment is the section Example of the present invention, and It is not all of embodiment.Based on embodiments of the invention, those of ordinary skill in the art are not before creative work is paid The every other embodiment obtained is put, protection scope of the present invention is belonged to.
The heat conducting nano composite material based on polyamide of present pre-ferred embodiments includes following by weight percentage Component:Polyamide 66 40-45%;Silicone resin 12-15%;Thermotropic liquid crystal 13-20%;Nanoscale galapectite powder 20%; Ethylene-propylene non-conjugated diene elastomer graft maleic anhydride 10-17%;Wherein, nanoscale galapectite powder passes through such as lower section It is prepared by method:Contained brown part in natural galapectite is removed, preliminary crushing is first carried out, then the hot blast at 80 DEG C~100 DEG C Second of crushing after drying 6~9 hours;Galapectite powder, distilled water and the powdery calgon after crushing are taken with mass ratio 2-5: 7-10: 0.005~0.03 is configured to mixed liquor;50~66 hours are stood again after stirring 16~20 hours at normal temperatures;Take Settled solution after stratification at 80 DEG C~100 DEG C heated-air drying 11~14 hours to galapectite into bulk;By block angstrom Lip river stone is crushed, and crosses 50~1500 mesh sieves, obtains nano level pure galapectite powder.
Such scheme improves and optimizes the preparation technology of existing heat conducting nanometer material, by preparing nano sized inorganic fillers Heat conductivility is had concurrently with thermotropic liquid crystal and in nylon, preparing and the hybrid in situ of excellent mechanical property is compound Material, not only enriches the modified method of polyamide, and substantially reduces cost, accelerates the industrialized step of in-situ compound technology Cut down, effectively solve liquid crystal fancy price, difficulty realizes industrialized problem.
In above-mentioned heat conducting nano composite material, it is preferable that by weight percentage, including following components:Polyamide 66 45%;Silicone resin 12%;Thermotropic liquid crystal 13%;Nanoscale galapectite powder 20%;Ethylene-propylene non-conjugated diene elasticity Body grafted maleic anhydride 10%.
In above-mentioned heat conducting nano composite material, it is preferable that by weight percentage, including following components:Polyamide 66 40%;Silicone resin 15%;Thermotropic liquid crystal 20%;Nanoscale galapectite powder 15%;Ethylene-propylene non-conjugated diene elasticity Body grafted maleic anhydride 10%.
In above-mentioned heat conducting nano composite material, it is preferable that by weight percentage, including following components:Polyamide 66 42%;Silicone resin 13%;Thermotropic liquid crystal 13%;Nanoscale galapectite powder 15%;Ethylene-propylene non-conjugated diene elasticity Body grafted maleic anhydride 17%.
The preparation method of the above-mentioned heat conducting nano composite material based on polyamide comprises the following steps:
Contained brown part in natural galapectite is removed, preliminary crushing is first carried out, then the hot blast at 80 DEG C~100 DEG C Second of crushing after drying 6~9 hours;
Take crush after galapectite powder, distilled water and powdery calgon with mass ratio 2-5: 7-10: 0.005~ 0.03 is configured to mixed liquor;
50~66 hours are stood again after stirring 16~20 hours at normal temperatures;
Take the heated-air drying 11~14 hours at 80 DEG C~100 DEG C of the settled solution after stratification blocking to galapectite Shape;
Block galapectite is crushed, and crosses 50~1500 mesh sieves, nano level pure galapectite powder is obtained;
After the material vacuum of composite is dried, it is well mixed, extrudes, granulates, is molded, heat conducting nano composite wood is made Material.
Preferably, in above-mentioned preparation method, galapectite powder, distilled water and the powdery calgon after crushing are taken with matter Amount is configured to mixed liquor than 5: 7: 0.005.
Preferably, in above-mentioned preparation method, galapectite powder, distilled water and the powdery calgon after crushing are taken with matter Amount is configured to mixed liquor than 2: 9: 0.03.
Preferably, in above-mentioned preparation method, extruder barrel mouthful temperature is 250 DEG C~260 DEG C, transportation section temperature is 260 DEG C~270 DEG C, compression section temperature be 270 DEG C~290 DEG C, metering section temperature be 290 DEG C~280 DEG C;Nozzle temperature be 275 DEG C~ 280℃;Screw speed is 180~200r/min;Rate of feeding is 15~20r/min.
Preferably, in above-mentioned preparation method, injection injecting machine material tube used mouthful temperature is 250 DEG C~260 DEG C, transportation section Temperature is 260 DEG C~270 DEG C, compression section temperature is 270 DEG C~290 DEG C, metering section temperature is 290 DEG C~295 DEG C;Nozzle temperature For 295 DEG C~300 DEG C;Mold temperature is 80 DEG C~100 DEG C;Screw speed is 100~120r/min;Inject back pressure be 60~ 80Mpa。
Preferably, in above-mentioned preparation method, it will granulate and dry 10~12h at 100 DEG C~110 DEG C in vacuum drying chamber It is cooled to room temperature afterwards and under sealing condition.
Detailed is made to the preparation method of the above-mentioned heat conducting nano composite material based on polyamide below by specific embodiment Explanation.
Embodiment 1
Prepare raw material by following components:Polyamide 66 45%;Silicone resin 12%;Thermotropic liquid crystal 13%;Nanoscale Galapectite powder 20%;Ethylene-propylene non-conjugated diene elastomer graft maleic anhydride 10%.
Contained brown part in natural galapectite is removed, preliminary crushing is first carried out, then the hot blast at 80 DEG C~100 DEG C Second of crushing after drying 6~9 hours;Galapectite powder, distilled water and the powdery calgon after crushing are taken with mass ratio 2-5: 7-10: 0.005~0.03 is configured to mixed liquor;50~66 hours are stood again after stirring 16~20 hours at normal temperatures;Take Settled solution after stratification at 80 DEG C~100 DEG C heated-air drying 11~14 hours to galapectite into bulk;By block angstrom Lip river stone is crushed, and crosses 50~1500 mesh sieves, obtains nano level pure galapectite powder;The material vacuum of composite is dried Afterwards, it is well mixed, extrudes, granulates, is molded, heat conducting nano composite material is made.
Embodiment 2
Prepare raw material by following components:Polyamide 66 40%;Silicone resin 15%;Thermotropic liquid crystal 20%;Nanoscale Galapectite powder 15%;Ethylene-propylene non-conjugated diene elastomer graft maleic anhydride 10%.
Contained brown part in natural galapectite is removed, preliminary crushing is first carried out, then the hot blast at 80 DEG C~100 DEG C Second of crushing after drying 6~9 hours;Galapectite powder, distilled water and the powdery calgon after crushing are taken with mass ratio 2-5: 7-10: 0.005~0.03 is configured to mixed liquor;50~66 hours are stood again after stirring 16~20 hours at normal temperatures;Take Settled solution after stratification at 80 DEG C~100 DEG C heated-air drying 11~14 hours to galapectite into bulk;By block angstrom Lip river stone is crushed, and crosses 50~1500 mesh sieves, obtains nano level pure galapectite powder;The material vacuum of composite is dried Afterwards, it is well mixed, extrudes, granulates, is molded, heat conducting nano composite material is made.
Embodiment 3
Prepare raw material by following components:Polyamide 66 42%;Silicone resin 13%;Thermotropic liquid crystal 13%;Nanoscale Galapectite powder 15%;Ethylene-propylene non-conjugated diene elastomer graft maleic anhydride 17%.
Contained brown part in natural galapectite is removed, preliminary crushing is first carried out, then the hot blast at 80 DEG C~100 DEG C Second of crushing after drying 6~9 hours;Galapectite powder, distilled water and the powdery calgon after crushing are taken with mass ratio 2-5: 7-10: 0.005~0.03 is configured to mixed liquor;50~66 hours are stood again after stirring 16~20 hours at normal temperatures;Take Settled solution after stratification at 80 DEG C~100 DEG C heated-air drying 11~14 hours to galapectite into bulk;By block angstrom Lip river stone is crushed, and crosses 50~1500 mesh sieves, obtains nano level pure galapectite powder;The material vacuum of composite is dried Afterwards, it is well mixed, extrudes, granulates, is molded, heat conducting nano composite material is made.
Embodiment 4
Prepare raw material by following components:Polyamide 66 44%;Silicone resin 13%;Thermotropic liquid crystal 13%;Nanoscale Galapectite powder 15%;Ethylene-propylene non-conjugated diene elastomer graft maleic anhydride 15%.
Contained brown part in natural galapectite is removed, preliminary crushing is first carried out, then the hot blast at 80 DEG C~100 DEG C Second of crushing after drying 6~9 hours;Galapectite powder, distilled water and the powdery calgon after crushing are taken with mass ratio 2-5: 7-10: 0.005~0.03 is configured to mixed liquor;50~66 hours are stood again after stirring 16~20 hours at normal temperatures;Take Settled solution after stratification at 80 DEG C~100 DEG C heated-air drying 11~14 hours to galapectite into bulk;By block angstrom Lip river stone is crushed, and crosses 50~1500 mesh sieves, obtains nano level pure galapectite powder;The material vacuum of composite is dried Afterwards, it is well mixed, extrudes, granulates, is molded, heat conducting nano composite material is made.
Embodiment 5
Prepare raw material by following components:Polyamide 66 44%;Silicone resin 15%;Thermotropic liquid crystal 15%;Nanoscale Galapectite powder 15%;Ethylene-propylene non-conjugated diene elastomer graft maleic anhydride 11%.
Contained brown part in natural galapectite is removed, preliminary crushing is first carried out, then the hot blast at 80 DEG C~100 DEG C Second of crushing after drying 6~9 hours;Galapectite powder, distilled water and the powdery calgon after crushing are taken with mass ratio 2-5: 7-10: 0.005~0.03 is configured to mixed liquor;50~66 hours are stood again after stirring 16~20 hours at normal temperatures;Take Settled solution after stratification at 80 DEG C~100 DEG C heated-air drying 11~14 hours to galapectite into bulk;By block angstrom Lip river stone is crushed, and crosses 50~1500 mesh sieves, obtains nano level pure galapectite powder;The material vacuum of composite is dried Afterwards, it is well mixed, extrudes, granulates, is molded, heat conducting nano composite material is made.
It should be appreciated that for those of ordinary skills, can according to the above description be improved or converted, And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.

Claims (10)

1. a kind of heat conducting nano composite material based on polyamide, it is characterised in that by weight percentage, including with the following group Point:
Wherein, the nanoscale galapectite powder is prepared via a method which:Contained brown part in natural galapectite is removed, Preliminary crushing is first carried out, then heated-air drying is crushed for second after 6~9 hours at 80 DEG C~100 DEG C;Take the Ai Luo after crushing Stone powder, distilled water and powdery calgon are configured to mixed liquor with mass ratio 2-5: 7-10: 0.005~0.03;In normal temperature Lower stirring stands 50~66 hours again after 16~20 hours;Take the hot blast at 80 DEG C~100 DEG C of the settled solution after stratification 11~14 hours are dried to galapectite into bulk;Block galapectite is crushed, and crosses 50~1500 mesh sieves, obtains nano level pure Net galapectite powder.
2. heat conducting nano composite material according to claim 1, it is characterised in that by weight percentage, including it is following Component:
3. heat conducting nano composite material according to claim 1, it is characterised in that by weight percentage, including it is following Component:
4. heat conducting nano composite material according to claim 1, it is characterised in that by weight percentage, including it is following Component:
5. a kind of preparation method of the heat conducting nano composite material based on polyamide, it is characterised in that comprise the following steps:
Contained brown part in natural galapectite is removed, preliminary crushing is first carried out, then the heated-air drying at 80 DEG C~100 DEG C Second of crushing after 6~9 hours;
Galapectite powder, distilled water and powdery calgon after crushing is taken to match somebody with somebody with mass ratio 2-5: 7-10: 0.005~0.03 Mixed liquor is made;
50~66 hours are stood again after stirring 16~20 hours at normal temperatures;
Take the settled solution after stratification at 80 DEG C~100 DEG C heated-air drying 11~14 hours to galapectite into bulk;
Block galapectite is crushed, and crosses 50~1500 mesh sieves, nano level pure galapectite powder is obtained;
After the material vacuum of composite is dried, it is well mixed, extrudes, granulates, is molded, heat conducting nano composite material is made.
6. preparation method according to claim 5, it is characterised in that take galapectite powder, distilled water and the powder after crushing Shape calgon is configured to mixed liquor with mass ratio 5: 7: 0.005.
7. preparation method according to claim 5, it is characterised in that take galapectite powder, distilled water and the powder after crushing Shape calgon is configured to mixed liquor with mass ratio 2: 9: 0.03.
8. preparation method according to claim 5, it is characterised in that extruder barrel mouthful temperature is 250 DEG C~260 DEG C, Transportation section temperature is 260 DEG C~270 DEG C, compression section temperature is 270 DEG C~290 DEG C, metering section temperature is 290 DEG C~280 DEG C;Spray Mouth temperature is 275 DEG C~280 DEG C;Screw speed is 180~200r/min;Rate of feeding is 15~20r/min.
9. preparation method according to claim 5, it is characterised in that injection injecting machine material tube used mouthful temperature is 250 DEG C~260 DEG C, transportation section temperature be 260 DEG C~270 DEG C, compression section temperature be 270 DEG C~290 DEG C, metering section temperature be 290 DEG C ~295 DEG C;Nozzle temperature is 295 DEG C~300 DEG C;Mold temperature is 80 DEG C~100 DEG C;Screw speed is 100~120r/min; Injection back pressure is 60~80Mpa.
10. preparation method according to claim 5, it is characterised in that will granulate in vacuum drying chamber 100 DEG C~ Dried at 110 DEG C after 10~12h and be cooled to room temperature under sealing condition.
CN201610114926.2A 2016-03-01 2016-03-01 Heat conducting nano composite material based on polyamide and preparation method thereof Pending CN107141784A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108727813A (en) * 2018-05-25 2018-11-02 郑州智锦电子科技有限公司 A kind of LED light sheathing material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102219994A (en) * 2011-05-24 2011-10-19 华南理工大学 Heat conducting nanometer material and preparation method and application thereof
CN104098890A (en) * 2013-04-10 2014-10-15 上海杰事杰新材料(集团)股份有限公司 HPN (high temperature resistant nylon)/(thermotropic liquid crystal polymer) / HNTs (halloysite nanotubes) composite material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102219994A (en) * 2011-05-24 2011-10-19 华南理工大学 Heat conducting nanometer material and preparation method and application thereof
CN104098890A (en) * 2013-04-10 2014-10-15 上海杰事杰新材料(集团)股份有限公司 HPN (high temperature resistant nylon)/(thermotropic liquid crystal polymer) / HNTs (halloysite nanotubes) composite material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108727813A (en) * 2018-05-25 2018-11-02 郑州智锦电子科技有限公司 A kind of LED light sheathing material

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Application publication date: 20170908