CN102786800A - Method for preparing graphene nanosheet/nylon 66 high thermal conductivity composite material - Google Patents
Method for preparing graphene nanosheet/nylon 66 high thermal conductivity composite material Download PDFInfo
- Publication number
- CN102786800A CN102786800A CN2012102698803A CN201210269880A CN102786800A CN 102786800 A CN102786800 A CN 102786800A CN 2012102698803 A CN2012102698803 A CN 2012102698803A CN 201210269880 A CN201210269880 A CN 201210269880A CN 102786800 A CN102786800 A CN 102786800A
- Authority
- CN
- China
- Prior art keywords
- thermal conductivity
- composite material
- preparation
- ball
- high thermal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for preparing graphene nanosheet/nylon 66 high thermal conductivity composite material. The high thermal conductivity composite material is prepared in a simple method that a certain mass of graphene nanosheet obtained by ball-milling natural graphite, nylon 66 and a silane coupling agent KH550 are ball-milled and mixed uniformly to from high thermal conductivity composite material powder, and then the obtained composite material powder is hot-pressed for 4-10min at the temperature of 220-280 DEG C and the pressure of 10-20MPa to obtain the high thermal conductivity composite material. The high thermal conductivity composite material provided by the invention has excellent heat-conducting property, and is low in cost, and the preparation process is simple.
Description
Technical field
The present invention relates to a kind of preparation method based on ball milling graphene nanometer sheet/nylon 66 high-heat-conductive composite materials.
Background technology
Scatterer plays crucial effects in the LED illuminating device, it directly determines the performance and the work-ing life of led light source.Traditional radiator material is generally duraluminum or copper, and the thermoplastic composite of high heat conduction of new generation is expected to the substituted metal material, as the LED radiator material.
Macromolecular material has lightweight, resistance to chemical attack, easy machine-shaping, electrical insulation capability excellence, mechanics and anti-fatigue performance good characteristics.Yet the constructional feature of macromolecular material itself has determined that most macromolecular materials are the heat insulation body, thereby has limited macromolecular material in the thermally conductive material Application for Field.Adopting high heat conductive filler that polymer is carried out modification is the effective way that improves Polymer Thermal Conductivity.And the Si that makes heat conductive filler commonly used at present
3N
4, SiC, AlN and BN etc. be because of the thermal conductivity of itself is lower, determined only under high addition, just can get higher thermal conductivity, and this will inevitably reduce other performance of macromolecular material itself.
Graphene is as a kind of novel two-dimentional carbon nanomaterial, has excellent properties such as fabulous specific conductivity and thermal conductivity, high specific surface area and Young's modulus.Theoretical investigation shows that the room temperature thermal conductivity of single-layer graphene is 4840～5300W (mK)
-1, be the highest material of present thermal conductivity.These unique character make Graphene can be used as a kind of novel nano heat-conductive filler, thereby the heat conductivility of polymkeric substance is greatly improved.Existing research shows, adds the thermal conductivity that Graphene (nanometer sheet) can obviously improve the macromolecule matrix material.Yet the Graphene (nanometer sheet) that is adopted in the report is to obtain through redox graphene or expanded graphite interlayer compound mostly, in the preparation process of these heat conductive fillers, needs to use a large amount of poisonous and harmfuls and the chemical example of severe corrosive, like dense H
2SO
4, dense HNO
3Deng, the use of these chemical reagent is prone to cause environmental pollution, and the complex manufacturing of above-mentioned heat conductive filler, excessive cycle.
Summary of the invention
In order to solve the existing problem of prior art, the used heat conductive filler of the present invention is innovated on traditional heat conductive filler basis, used ball milling graphite after resulting graphene nanometer sheet be heat conductive filler.Because the two-dimentional laminated structure that it is unique, this graphene nanometer sheet more is prone in polymeric matrix, form the heat conduction network with respect to graphite, and its preparation process is simple, price is cheap more than Graphene.In the preparation process, also need not to adopt present chemical method to prepare the used poisonous and harmful chemical reagent of Graphene (nanometer sheet).
The preparation method who mainly utilizes graphene nanometer sheet as the high-heat-conductive composite material of filler provided by the invention has following steps:
(1) Graphite Powder 99 and WC ball are joined in the ball grinder, add a certain amount of absolute ethyl alcohol, behind the airtight rotating speed ball milling 4～8h of back, after oven dry is handled, just can obtain graphene nanometer sheet with 400～800 commentaries on classics/min as ball-milling medium;
(2) graphene nanometer sheet that obtains behind the ball milling, nylon 66 and silane coupling agent are joined in the ball grinder, and add a certain amount of absolute ethyl alcohol as ball-milling medium.Can obtain the high-heat-conductive composite material raw material with carrying out drying treatment behind the ball grinder sealing speed ball milling 1～2h of back with 400～600 commentaries on classics/min.
Compare with prior art, the present invention has following advantage:
1, high heat conductive filler provided by the invention has nano level laminated structure; Not only has good heat conductivility; And its unique two-dimentional laminated structure makes it in nylon 66 matrixes, form the heat conduction network easily, under low filling condition, just can reach high heat-conducting property.
2, the preparation technology of heat conductive filler provided by the invention is simple, and is with low cost, need not adopt dense H in the experimentation
2SO
4, dense HNO
3Deng the pharmaceutical chemicals of poisonous and harmful and severe corrosive and loaded down with trivial details subsequent processes.
3, high-heat-conductive composite material provided by the invention can adopt conventional blend method to make, and need not harsh synthesis condition, and preparation technology is simple.
Description of drawings
In order to be illustrated more clearly in the technical scheme of the embodiment of the invention, will do introduction simply to the accompanying drawing of required use among the embodiment below.
Fig. 1 is the electron scanning micrograph of gained graphene nanometer sheet different amplification behind the ball milling in the embodiment of the invention: (a) low multiple (10000 times), (b) high multiple (80000 times).
Fig. 2 be in the embodiment of the invention hot pressing with the three-dimensional decomposition texture synoptic diagram of mould.
Fig. 3 is used for the three-dimensional profile synoptic diagram of thermal conductivity test sample.
Embodiment
For a better understanding of the present invention, in the face of doing further, the present invention describes down.
The preparation of graphene nanometer sheet: 1.0～3.0g Graphite Powder 99 is joined in the ball grinder; Add 4～8mL absolute ethyl alcohol as ball-milling medium; The WC ball is a mill ball; Behind the airtight rotating speed ball milling 4～8h of back of ball grinder with 400～800 commentaries on classics/min, open ball grinder, sample, oven dry can be obtained graphene nanometer sheet after handling.
The preparation of graphene nanometer sheet/nylon 66 high-heat-conductive composite materials: dried graphene nanometer sheet is joined in the ball grinder by different mass ratio (4: 6～6: 4) with nylon 66; Add 4mL～10mL absolute ethyl alcohol and 20 μ L～50 μ L silane coupling agents (KH550) respectively as ball-milling medium and surface-modifying agent; The WC ball is as mill ball; Behind the airtight rotating speed ball milling 1～2h of back of ball grinder with 400～800 commentaries on classics/min; Open ball grinder, the composite powder that obtains behind the ball milling is carried out drying treatment under 40 ℃～80 ℃.
(die size is 90mm * 90nm * 2mm to have the stainless steel template 1 of diameter 12.7mm circular hole 11 in the middle of will the mixed powder after drying treatment putting into; Referring to Fig. 2); Upper and lower surface covers stainless steel steel disc 2 and 3, and hot pressing 4～10min can obtain the block finished product of high-heat-conductive composite material under 220～280 ℃, 10MPa～20MPa pressure then.
Thickness by we observe through the graphene nanometer sheet that obtains after the ball-milling processing among Fig. 1 mainly concentrates on below the 10nm.
Thermal Conductivity Determination: the thermal conductivity that adopts laser thermal conductivity appearance (NETZSCH LFA447) working sample of the anti-instrument Manufacturing Co., Ltd of speeding of Germany.Before the test, to reduce the scattering of sample to laser, each temperature spot replicate measurement three times is got its MV as net result at sample surfaces spraying one deck graphite.
The heat physical properties of the composite heat conducting material of the different graphene nanometer sheet content of table 1
Claims (8)
1. the preparation method of graphene nanometer sheet/nylon 66 high-heat-conductive composite materials is characterized in that following steps:
Step a) obtains graphene nanometer sheet with graphite ball milling in anhydrous ethanol medium;
The graphene nanometer sheet that step b) obtains after with ball milling mixes by a certain percentage with silane coupling agent KH550 with nylon 66 and obtains the high-heat-conductive composite material powder.
2. preparation method according to claim 1 is characterized in that, the ball milling speed of said step a) is 400～800 commentaries on classics/min.
3. preparation method according to claim 1 is characterized in that, the ball milling time of said step a) is 4～8h.
4. preparation method according to claim 1 is characterized in that, the massfraction of graphene nanometer sheet is 30～60% in the said step b).
5. preparation method according to claim 1 is characterized in that, the ball milling speed of said step b) is 300～600 commentaries on classics/min.
6. preparation method according to claim 1 is characterized in that, the ball milling time of said step b) is 1～2h.
7. preparation method according to claim 1 is characterized in that, used mill ball is the WC ball, and diameter is 10mm.
8. preparation method according to claim 1 is characterized in that, the material of used grinding pot is WC, and volume is 80ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102698803A CN102786800A (en) | 2012-08-01 | 2012-08-01 | Method for preparing graphene nanosheet/nylon 66 high thermal conductivity composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102698803A CN102786800A (en) | 2012-08-01 | 2012-08-01 | Method for preparing graphene nanosheet/nylon 66 high thermal conductivity composite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102786800A true CN102786800A (en) | 2012-11-21 |
Family
ID=47152399
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012102698803A Pending CN102786800A (en) | 2012-08-01 | 2012-08-01 | Method for preparing graphene nanosheet/nylon 66 high thermal conductivity composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102786800A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044906A (en) * | 2012-12-31 | 2013-04-17 | 广东高怡新工程塑料有限公司 | Nylon base composite material with heat conducting function, and preparation method of nylon base composite material |
| CN103044778A (en) * | 2012-12-31 | 2013-04-17 | 广东高怡新工程塑料有限公司 | High-thermal-conductivity PP (polypropylene)-based composite material and preparation method thereof |
| CN103073930A (en) * | 2013-01-30 | 2013-05-01 | 同济大学 | Preparation method and application of alkylated functional graphene |
| CN104788951A (en) * | 2015-05-04 | 2015-07-22 | 武汉轻工大学 | LED (light-emitting diode) high-thermal-conductivity composite material and preparation method thereof |
| CN104861645A (en) * | 2015-04-09 | 2015-08-26 | 浙江泰索科技有限公司 | Thermal-conductive flame-retardant nylon 66 and preparation method thereof |
| CN105860195A (en) * | 2016-04-19 | 2016-08-17 | 福建博大塑业新材料有限公司 | Preparation method of graphene-enhanced PE/PP polymer composite |
| CN107227019A (en) * | 2017-04-27 | 2017-10-03 | 宁波海雨新材料科技有限公司 | A kind of composite of graphene conductive modification of nylon 66 and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008208188A (en) * | 2007-02-26 | 2008-09-11 | Honda Motor Co Ltd | Method for producing filler for polyamide resin, and particle dispersion-reinforced polyamide resin |
| CN101704520A (en) * | 2009-11-05 | 2010-05-12 | 华侨大学 | Method for producing graphene |
| CN101928407A (en) * | 2009-06-25 | 2010-12-29 | 华东理工大学 | Preparation method of composition containing graphene |
-
2012
- 2012-08-01 CN CN2012102698803A patent/CN102786800A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008208188A (en) * | 2007-02-26 | 2008-09-11 | Honda Motor Co Ltd | Method for producing filler for polyamide resin, and particle dispersion-reinforced polyamide resin |
| CN101928407A (en) * | 2009-06-25 | 2010-12-29 | 华东理工大学 | Preparation method of composition containing graphene |
| CN101704520A (en) * | 2009-11-05 | 2010-05-12 | 华侨大学 | Method for producing graphene |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044906A (en) * | 2012-12-31 | 2013-04-17 | 广东高怡新工程塑料有限公司 | Nylon base composite material with heat conducting function, and preparation method of nylon base composite material |
| CN103044778A (en) * | 2012-12-31 | 2013-04-17 | 广东高怡新工程塑料有限公司 | High-thermal-conductivity PP (polypropylene)-based composite material and preparation method thereof |
| CN103044778B (en) * | 2012-12-31 | 2015-04-22 | 广东高怡新工程塑料有限公司 | High-thermal-conductivity PP (polypropylene)-based composite material and preparation method thereof |
| CN103073930A (en) * | 2013-01-30 | 2013-05-01 | 同济大学 | Preparation method and application of alkylated functional graphene |
| CN104861645A (en) * | 2015-04-09 | 2015-08-26 | 浙江泰索科技有限公司 | Thermal-conductive flame-retardant nylon 66 and preparation method thereof |
| CN104861645B (en) * | 2015-04-09 | 2017-07-11 | 浙江泰索科技有限公司 | A kind of heat conductive flame-retarding nylon66 fiber and preparation method thereof |
| CN104788951A (en) * | 2015-05-04 | 2015-07-22 | 武汉轻工大学 | LED (light-emitting diode) high-thermal-conductivity composite material and preparation method thereof |
| CN105860195A (en) * | 2016-04-19 | 2016-08-17 | 福建博大塑业新材料有限公司 | Preparation method of graphene-enhanced PE/PP polymer composite |
| CN107227019A (en) * | 2017-04-27 | 2017-10-03 | 宁波海雨新材料科技有限公司 | A kind of composite of graphene conductive modification of nylon 66 and preparation method thereof |
| CN107227019B (en) * | 2017-04-27 | 2019-09-20 | 宁波海雨新材料科技有限公司 | A kind of 66 composite material and preparation method of graphene conductive modification of nylon |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102786800A (en) | Method for preparing graphene nanosheet/nylon 66 high thermal conductivity composite material | |
| CN112175238B (en) | Preparation method of boron nitride nanosheet-carbon nanotube heat-conducting filler and heat-conducting composite material | |
| CN103627179A (en) | Graphene-containing silicone rubber composite material with high thermal conductivity and preparation method thereof | |
| CN103524825B (en) | A kind of preparation method of heat-conducting polymer-graphene composite material and goods | |
| CN104231624B (en) | A kind of modified cyanic acid ester resin heat-conductive composite material and preparation method thereof | |
| CN103627180B (en) | Carbon nanotube grafting cage-type silsesquioxane modified silicon rubber and preparation method thereof | |
| CN107892784B (en) | Polymer-based nanocomposite and preparation method thereof | |
| CN107474354A (en) | A kind of high dispersive graphene heat-conducting plastic preparation method and products thereof and application | |
| CN107325520B (en) | A kind of preparation method of antistatic modified plastics | |
| CN104532073A (en) | Aluminum-based composite radiating material for high strength LED | |
| CN103849120A (en) | Conductive composite material and its preparation method | |
| CN108485224A (en) | A kind of high bending modulus heat-conductivity polymer composite and preparation method thereof | |
| CN102584240A (en) | Sintering method of ZrB2-SiC superhigh temperature ceramics | |
| CN104045896B (en) | Heat conduction composite polyethylene material and preparation method thereof | |
| CN108727679A (en) | A kind of fire-retardant eva foam composite material of ammonium polyphosphate modifying/graphene | |
| CN106751198A (en) | Wood-plastic floor of negative oxygen ion and preparation method thereof | |
| CN106147204A (en) | A kind of preparation method of graphene/polyaniline/conductive polyurethane laminated film | |
| Li et al. | Boron nitride whiskers and nano alumina synergistically enhancing the vertical thermal conductivity of epoxy-cellulose aerogel nanocomposites | |
| CN105237948B (en) | A kind of moisture-proof phenolaldehyde moulding compound | |
| CN104194264B (en) | PCB high heat resistance POSS base epoxy nanocomposite and preparation method thereof | |
| CN102887665B (en) | Novel graphite powder and radiator made of novel graphite powder | |
| CN105789423B (en) | A kind of preparation method of the thermoelectric composite material of polyaniline in-situ polymerization cladding PEDOT modification nano-sized carbons | |
| CN105778134B (en) | A kind of graphene composite polymer film material and preparation method thereof | |
| CN103937146A (en) | Method for preparing graphene modified polyformaldehyde composite material | |
| CN104927736A (en) | Weather-proof epoxy resin glue and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20121121 |