CN107325648A - A kind of preparation method of graphene heat conducting film - Google Patents
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Abstract
The invention discloses a kind of preparation method of graphene heat conducting film, belong to Heat Conduction Material preparing technical field.The crosslinking toughening effect that the present invention is produced using the splendid film forming of fish glue and glutinous rice starch through thermodynamic activity is come composite modified with graphene oxide solution, while graphene oxide film forming ability is improved, the toughness of heat conducting film is added again, after finally by KI, graphene oxide is reduced under vacuum, by thermodynamic activity further to film deoxygenation, finally give graphene heat conducting film, graphene heat conducting film mechanical performance produced by the present invention is splendid, it is hot good to spread, and with preferable filming performance, the resistance to number of times of bending repeatedly of heat conducting film is up to more than 1300 times.
Description
Technical field
The invention discloses a kind of preparation method of graphene heat conducting film, belong to Heat Conduction Material preparing technical field.
Background technology
For electronic product, effectively radiated by all parts and be used for the longevity to obtain relatively low operating temperature
Life and the speed of service can produce extremely important influence.With continuing to develop and progressive for science and technology, particularly computer chip is more
Coring has become main flow, and the computer speed of service is constantly accelerated, and power is also increased, and effective radiating runs speed to it
Degree plays very important effect.Wherein, radiating main product is graphite-like heat conducting film.
Graphene heat conducting film is also known as conductive graphite piece, is a kind of new heat conduction and heat radiation material new in recent years,
It is applied to many fields such as electronics, communication, illumination, aviation and defence and military extensively.Graphene heat conducting film has the following advantages that：
（1）High thermal conductivity coefficient, can reach 1200~1800W/（m·K）, higher than CNT and diamond, resistivity is about 10-6Ω·
Cm, and the speed of electron transfer is exceedingly fast；（2）Low thermal resistance, lightweight, its thermal resistance is lower than aluminium by 40%, and lower than copper by 20%, weight compares aluminium
It is light by 25%, it is lighter than copper by 75%；（3）Graphene heat conducting film surface can be combined to meet with the other materials such as metal, plastic cement, adhesive sticker
More design functions and needs, can also need to carry out cutting cutting to graphene heat conducting film according to true form.
The preparation method of current graphene heat conducting film mainly has dilatometry and macromolecule thermal decomposition method.Utilize dilatometry
Obtained graphene heat conducting film, its crystal property is poor, and resist bending poor performance, heat diffusivity is not good, and thermal conductivity factor is low, normally only
For 200~500W/（m·K）, and the graphene heat conducting film of better performances can be arrived using macromolecule pyrolysismethod, but technique is cumbersome,
The graphene heat conducting film of sheet, low production efficiency are can only obtain every time.Therefore, a kind of preparation technology letter is urgently developed in this area
Single, production efficiency is high, and the graphene heat conducting film of excellent combination property.
The content of the invention
Present invention mainly solves technical problem：There is heat diffusivity for common graphene heat conducting film at present not good,
Causing property of film forming ability deficiency is crisp easily to be split, and there is provided a kind of preparation method of graphene heat conducting film for the defect of resist bending poor performance.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）Weigh 2~3kg glutinous rice and soak 5~8h with 8~10L clear water, ground after the glutinous rice after immersion and water are mixed with stone mill
3~5 times, the milky sticky rice syrup that is flowed out from stone mill is collected, sticky rice syrup was staticly settled after 3~5 days and absorbed with syringe
Layer clear liquid, obtains the sticky glutinous rice starch slurry of lower floor；
（2）Weigh 500~600g fishes fat and 400~500g grass carp skins and crush 20~30min, obtain crushed material, by crushed material and
It is put into after water mixing in pot and is heated to boiling, 1~2h of boiling treats filtering after the completion of boiling, obtains filtrate, then concentrate the filtrate to
The 1/5 of filtrate original volume, is obtained making fish glue concentrate by oneself, and above-mentioned glutinous rice starch slurry, self-control fish glue concentrate and peach gum are mixed
Heating stirring, obtains self-control toughness reinforcing into film liquid afterwards, standby；
（3）Weigh 100~200g crystalline flake graphites to be put into reactor, then 1.0~2.0L mass fractions are added into reactor and be
75% sulfuric acid solution and 0.5~1.0L mass fractions are 85% concentrated phosphoric acid, start reactor agitator and are stirred at 20~30 DEG C
Mix after 15~20min of mixing, then 300~500g potassium permanganate is added into reactor, improve temperature of reaction kettle to 90~100
DEG C, continue insulated and stirred and react 4~6h；
（4）After above-mentioned reaction terminates, taking-up reaction product, which is separated by filtration, to be precipitated, and is with concentration successively by gained precipitation
1mol/L hydrochloric acid and deionized water wash 10~12h respectively, then the precipitation after washing and deionized water are mixed, after ultrasonic disperse
Obtain graphene oxide suspension；
（5）By above-mentioned graphene oxide suspension and step（2）Standby self-control toughness reinforcing is heated to 70~80 after being mixed into film liquid
DEG C, spray film liquid is obtained, then spray film liquid is obtained into wet heat conducting film by hot spray process spraying, wet heat conducting film is moved into baking oven, dried,
Dry heat conducting film is obtained, then dry heat conducting film is immersed mass concentration in 40~50mg/L liquor kalii iodide, to soak at 2~4 DEG C
Stain reduces 4~6h, and reduction takes out heat conducting film after terminating, and graphene heat conducting film is can obtain after vacuum drying.
Step（1）Described in glutinous rice and water mass ratio be 1:2.
Step（2）Described in crushed material and water mass ratio be 1:5.
Step（2）Described in glutinous rice starch slurry, self-control fish glue concentrate and peach gum mass ratio be 1:3:1, heating temperature
Spend for 110~120 DEG C, mixing time is 15~20min.
Step（4）Described in washing after precipitation and deionized water mass ratio be 1:5, ultrasonic disperse power is 200
~300W, supersonic frequency is 40~50KHz.
Step（5）Described in graphene oxide suspension and self-control toughness reinforcing into film liquid mass ratio be 5:1, hot spray process
Specific operation process be：Will spray film liquid at 100~120 DEG C apart from polyvinyl chloride film height 40~50cm at be sprayed on it is poly-
On vinyl chloride film, it is 200~300 μm to control coating thickness.
The beneficial effects of the invention are as follows：
（1）The present invention mixes glutinous rice starch and fish glue concentrate as toughness reinforcing into film liquid, using the splendid film forming of fish glue and
Graphene oxide suspension is composite modified, improves the film forming ability of graphene oxide；
（2）The crosslinking toughening effect that the present invention is produced using glutinous rice starch through thermodynamic activity adds the toughness of heat conducting film, leads to again
Cross after KI reduces graphene oxide under vacuum, by thermodynamic activity to film deoxygenation, further improve heat conduction
The toughness of film, and heat conducting film is improved into the compatibility between film liquid and graphene, the cross-linked structure of formation can be bridged effectively
Heat transfer process between graphene so that heat conducting film diffusion is hot to improve, and improves conventional graphene heat conducting film film forming ability
The crisp shortcoming easily split of causing property of deficiency, after testing, graphene heat conducting film thermal conductivity factor produced by the present invention are 1160~1680W/
（m·K）, tensile strength is resistant to bend repeatedly more than 1300 times up to 48.5~52.3MPa.
Embodiment
2~3kg glutinous rice is weighed first and soaks 5~8h with 8~10L clear water, is in mass ratio by the glutinous rice and water after immersion
1:Ground 3~5 times with stone mill after 2 mixing, collect the milky sticky rice syrup flowed out from stone mill, sticky rice syrup is moved into wooden barrel,
Staticly settle after 3~5 days and to absorb wooden barrel clear liquid at the middle and upper levels with syringe, obtain the sticky glutinous rice starch slurry of lower floor, weigh 500~
600g fishes fat and 400~500g grass carp skins are put into tissue pulverizer 20~30min of crushing, obtain crushed material, by crushed material and
Water is 1 in mass ratio:It is put into after 5 mixing in pot and is heated to boiling, 1~2h of boiling, filtering removes filter residue after the completion for the treatment of boiling, obtains
Rotary Evaporators are put into filtrate, then by filtrate, concentrated by rotary evaporation obtains making fish glue concentrate by oneself to the 1/5 of filtrate original volume, then
Glutinous rice starch is starched, fish glue concentrate and peach gum in mass ratio 1 is made by oneself:3:It is put into after 1 mixing in beaker, beaker is moved into oil bath
In pot, rise oil bath pot temperature is to 110~120 DEG C, and 15~20min of insulated and stirred obtains self-control toughness reinforcing into film liquid, then weigh
100~200g crystalline flake graphites are put into reactor, then it is 75% sulfuric acid solution to add 1.0~2.0L mass fractions into reactor
With 0.5~1.0L mass fractions be 85% concentrated phosphoric acid, start reactor agitator stir at 20~30 DEG C mix 15~
After 20min, then addition 300~500g potassium permanganate into reactor, temperature of reaction kettle is improved to 90~100 DEG C, continues to be incubated
4~6h of stirring reaction, after question response terminates, taking-up reaction product, which is separated by filtration, to be precipitated, and gained precipitation is used into concentration successively
10~12h is washed respectively for 1mol/L hydrochloric acid and deionized water, then by the precipitation after washing is 1 in mass ratio:5 be added to from
In sub- water, graphene oxide is obtained after disperseing through ultrasonic disperse instrument with 200~300W power and 40~50KHz frequency ultrasound and is hanged
Supernatant liquid, then be 5 in mass ratio:1 by graphene oxide suspension with self-control toughness reinforcing into film liquid mix after be heated to 70~80 DEG C, obtain
To spray film liquid, then will the spray at 40~50cm of polyvinyl chloride film height at 100~120 DEG C by hot spray process of spray film liquid
It is coated on polyvinyl chloride film, it is 200~300 μm to control coating thickness, obtains wet heat conducting film, finally wet heat conducting film is moved into and dried
Case, dries 1~2h at 60~70 DEG C, obtains dry heat conducting film, then it is 40~50mg/L's that dry heat conducting film is immersed into mass concentration
In liquor kalii iodide, 4~6h of dipping reduction at 2~4 DEG C, reduction is taken out heat conducting film after terminating, is put into vacuum desiccator,
Dried at 100~105 DEG C after 30~40min and can obtain graphene heat conducting film.
Example 1
2kg glutinous rice 8L clear water immersion 5h is weighed first, is 1 in mass ratio by the glutinous rice and water after immersion:Stone mill is used after 2 mixing
Grinding 3 times, collects the milky sticky rice syrup flowed out from stone mill, and sticky rice syrup is moved into wooden barrel, staticly settles after 3 days with injection
Device absorbs wooden barrel clear liquid at the middle and upper levels, obtains the sticky glutinous rice starch slurry of lower floor, weighs 500g fishes fat and 400g grass carp skins are put into group
Knit and 20min is crushed in pulverizer, obtain crushed material, be 1 in mass ratio by crushed material and water:It is put into pot and is heated to after 5 mixing
Boiling, boiling 1h, filtering removes filter residue after the completion for the treatment of boiling, obtains filtrate, then filtrate is put into Rotary Evaporators, concentrated by rotary evaporation
To the 1/5 of filtrate original volume, obtain making fish glue concentrate by oneself, then glutinous rice starch is starched, fish glue concentrate and peach gum is made by oneself by matter
Amount compares 1:3:It is put into after 1 mixing in beaker, beaker is moved into oil bath pan, rise oil bath pot temperature to 110 DEG C, insulated and stirred
15min, obtains self-control toughness reinforcing into film liquid, then weighs 100g crystalline flake graphites and be put into reactor, then adds into reactor 1.0L
Mass fraction is 75% sulfuric acid solution and 0.5L mass fractions are 85% concentrated phosphoric acid, starts reactor agitator and is stirred at 20 DEG C
Mix after mixing 15min, then 300g potassium permanganate is added into reactor, improve temperature of reaction kettle to 90 DEG C, continue insulated and stirred
4h is reacted, after question response terminates, taking-up reaction product, which is separated by filtration, to be precipitated, and is successively 1mol/L with concentration by gained precipitation
Hydrochloric acid and deionized water wash 10h respectively, then by the precipitation after washing are 1 in mass ratio:5 are added in deionized water, through super
Sound separating apparatus obtains graphene oxide suspension after disperseing with 200W power and 40KHz frequency ultrasound, then is 5 in mass ratio:1
70 DEG C are heated to after graphene oxide suspension is mixed with self-control toughness reinforcing into film liquid, obtains spraying film liquid, then spray film liquid is passed through
Hot spray process is sprayed on polyvinyl chloride film at 100 DEG C at polyvinyl chloride film height 40cm, controls coating thickness
For 200 μm, wet heat conducting film is obtained, wet heat conducting film is finally moved into baking oven, 1h is dried at 60 DEG C, dry heat conducting film is obtained, then will
Dry heat conducting film immersion mass concentration is in 40mg/L liquor kalii iodide, the dipping reduction 4h at 2 DEG C, reduction is taken out and led after terminating
Hotting mask, is put into vacuum desiccator, is dried at 100 DEG C and can obtain graphene heat conducting film after 30min.
Example 2
2kg glutinous rice 9L clear water immersion 7h is weighed first, is 1 in mass ratio by the glutinous rice and water after immersion:Stone mill is used after 2 mixing
Grinding 4 times, collects the milky sticky rice syrup flowed out from stone mill, and sticky rice syrup is moved into wooden barrel, staticly settles after 4 days with injection
Device absorbs wooden barrel clear liquid at the middle and upper levels, obtains the sticky glutinous rice starch slurry of lower floor, weighs 550g fishes fat and 450g grass carp skins are put into group
Knit and 25min is crushed in pulverizer, obtain crushed material, be 1 in mass ratio by crushed material and water:It is put into pot and is heated to after 5 mixing
Boiling, boiling 1h, filtering removes filter residue after the completion for the treatment of boiling, obtains filtrate, then filtrate is put into Rotary Evaporators, concentrated by rotary evaporation
To the 1/5 of filtrate original volume, obtain making fish glue concentrate by oneself, then glutinous rice starch is starched, fish glue concentrate and peach gum is made by oneself by matter
Amount compares 1:3:It is put into after 1 mixing in beaker, beaker is moved into oil bath pan, rise oil bath pot temperature to 115 DEG C, insulated and stirred
18min, obtains self-control toughness reinforcing into film liquid, then weighs 150g crystalline flake graphites and be put into reactor, then adds into reactor 1.5L
Mass fraction is 75% sulfuric acid solution and 0.8L mass fractions are 85% concentrated phosphoric acid, starts reactor agitator and is stirred at 25 DEG C
Mix after mixing 18min, then 400g potassium permanganate is added into reactor, improve temperature of reaction kettle to 95 DEG C, continue insulated and stirred
5h is reacted, after question response terminates, taking-up reaction product, which is separated by filtration, to be precipitated, and is successively 1mol/L with concentration by gained precipitation
Hydrochloric acid and deionized water wash 11h respectively, then by the precipitation after washing are 1 in mass ratio:5 are added in deionized water, through super
Sound separating apparatus obtains graphene oxide suspension after disperseing with 250W power and 45KHz frequency ultrasound, then is 5 in mass ratio:1
75 DEG C are heated to after graphene oxide suspension is mixed with self-control toughness reinforcing into film liquid, obtains spraying film liquid, then spray film liquid is passed through
Hot spray process is sprayed on polyvinyl chloride film at 110 DEG C at polyvinyl chloride film height 45cm, controls coating thickness
For 250 μm, wet heat conducting film is obtained, wet heat conducting film is finally moved into baking oven, 1h is dried at 65 DEG C, dry heat conducting film is obtained, then will
Dry heat conducting film immersion mass concentration is in 45mg/L liquor kalii iodide, the dipping reduction 5h at 3 DEG C, reduction is taken out and led after terminating
Hotting mask, is put into vacuum desiccator, is dried at 103 DEG C and can obtain graphene heat conducting film after 35min.
Example 3
3kg glutinous rice 10L clear water immersion 8h is weighed first, is 1 in mass ratio by the glutinous rice and water after immersion:Stone is used after 2 mixing
Mill grinding 5 times, collects the milky sticky rice syrup flowed out from stone mill, and sticky rice syrup is moved into wooden barrel, staticly settles after 5 days with note
Emitter absorbs wooden barrel clear liquid at the middle and upper levels, obtains the sticky glutinous rice starch slurry of lower floor, weighs 600g fishes fat and 500g grass carp skins are put into
30min is crushed in tissue pulverizer, crushed material is obtained, is 1 in mass ratio by crushed material and water:It is put into pot and heats after 5 mixing
To seething with excitement, boiling 2h treats filtering removal filter residue after the completion of boiling, obtains filtrate, then filtrate is put into Rotary Evaporators, rotates dense
The 1/5 of filtrate original volume is reduced to, obtains making by oneself fish glue concentrate, then glutinous rice starch starched, fish glue concentrate is made by oneself and peach gum is pressed
Mass ratio 1:3:It is put into after 1 mixing in beaker, beaker is moved into oil bath pan, rise oil bath pot temperature to 120 DEG C, insulated and stirred
20min, obtains self-control toughness reinforcing into film liquid, then weighs 200g crystalline flake graphites and be put into reactor, then adds into reactor 2.0L
Mass fraction is 75% sulfuric acid solution and 1.0L mass fractions are 85% concentrated phosphoric acid, starts reactor agitator and is stirred at 30 DEG C
Mix after mixing 20min, then 500g potassium permanganate is added into reactor, improve temperature of reaction kettle to 100 DEG C, continue insulated and stirred
6h is reacted, after question response terminates, taking-up reaction product, which is separated by filtration, to be precipitated, and is successively 1mol/L with concentration by gained precipitation
Hydrochloric acid and deionized water wash 12h respectively, then by the precipitation after washing are 1 in mass ratio:5 are added in deionized water, through super
Sound separating apparatus obtains graphene oxide suspension after disperseing with 300W power and 50KHz frequency ultrasound, then is 5 in mass ratio:1
80 DEG C are heated to after graphene oxide suspension is mixed with self-control toughness reinforcing into film liquid, obtains spraying film liquid, then spray film liquid is passed through
Hot spray process is sprayed on polyvinyl chloride film at 120 DEG C at polyvinyl chloride film height 50cm, controls coating thickness
For 300 μm, wet heat conducting film is obtained, wet heat conducting film is finally moved into baking oven, 2h is dried at 70 DEG C, dry heat conducting film is obtained, then will
Dry heat conducting film immersion mass concentration is in 50mg/L liquor kalii iodide, the dipping reduction 6h at 4 DEG C, reduction is taken out and led after terminating
Hotting mask, is put into vacuum desiccator, is dried at 105 DEG C and can obtain graphene heat conducting film after 40min.
Performance test is carried out to graphene heat conducting film made from example 1~3 and commercially available common graphite alkene heat conducting film, it is detected
As a result such as following table：
| Detection project | Common graphite alkene heat conducting film | Example 1 | Example 2 | Example 3 |
| Thermal conductivity factor W/（m·K） | 1800 | 1980 | 1820 | 1960 |
| Tensile strength（MPa） | 45.2 | 48.5 | 50.8 | 52.3 |
| It is resistance to bend repeatedly（It is secondary） | 800 | 1300 | 1400 | 1500 |
Above-described embodiment is not limited for the present invention preferably embodiment, but embodiments of the present invention by above-described embodiment
System, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (6)
1. a kind of preparation method of graphene heat conducting film, it is characterised in that specifically preparation process is：
（1）Weigh 2~3kg glutinous rice and soak 5~8h with 8~10L clear water, ground after the glutinous rice after immersion and water are mixed with stone mill
3~5 times, the milky sticky rice syrup that is flowed out from stone mill is collected, sticky rice syrup was staticly settled after 3~5 days and absorbed with syringe
Layer clear liquid, obtains the sticky glutinous rice starch slurry of lower floor；
（2）Weigh 500~600g fishes fat and 400~500g grass carp skins and crush 20~30min, obtain crushed material, by crushed material and
It is put into after water mixing in pot and is heated to boiling, 1~2h of boiling treats filtering after the completion of boiling, obtains filtrate, then concentrate the filtrate to
The 1/5 of filtrate original volume, is obtained making fish glue concentrate by oneself, and above-mentioned glutinous rice starch slurry, self-control fish glue concentrate and peach gum are mixed
Heating stirring, obtains self-control toughness reinforcing into film liquid afterwards, standby；
（3）Weigh 100~200g crystalline flake graphites to be put into reactor, then 1.0~2.0L mass fractions are added into reactor and be
75% sulfuric acid solution and 0.5~1.0L mass fractions are 85% concentrated phosphoric acid, start reactor agitator and are stirred at 20~30 DEG C
Mix after 15~20min of mixing, then 300~500g potassium permanganate is added into reactor, improve temperature of reaction kettle to 90~100
DEG C, continue insulated and stirred and react 4~6h；
（4）After above-mentioned reaction terminates, taking-up reaction product, which is separated by filtration, to be precipitated, and is with concentration successively by gained precipitation
1mol/L hydrochloric acid and deionized water wash 10~12h respectively, then the precipitation after washing and deionized water are mixed, after ultrasonic disperse
Obtain graphene oxide suspension；
（5）By above-mentioned graphene oxide suspension and step（2）Standby self-control toughness reinforcing is heated to 70~80 after being mixed into film liquid
DEG C, spray film liquid is obtained, then spray film liquid is obtained into wet heat conducting film by hot spray process spraying, wet heat conducting film is moved into baking oven, dried,
Dry heat conducting film is obtained, then dry heat conducting film is immersed mass concentration in 40~50mg/L liquor kalii iodide, to soak at 2~4 DEG C
Stain reduces 4~6h, and reduction takes out heat conducting film after terminating, and graphene heat conducting film is can obtain after vacuum drying.
2. a kind of preparation method of graphene heat conducting film according to claim 1, it is characterised in that：Step（1）Described in
Glutinous rice and water mass ratio be 1:2.
3. a kind of preparation method of graphene heat conducting film according to claim 1, it is characterised in that：Step（2）Described in
Crushed material and water mass ratio be 1:5.
4. a kind of preparation method of graphene heat conducting film according to claim 1, it is characterised in that：Step（2）Described in
Glutinous rice starch slurry, self-control fish glue concentrate and peach gum mass ratio be 1:3:1, heating-up temperature is 110~120 DEG C, during stirring
Between be 15~20min.
5. a kind of preparation method of graphene heat conducting film according to claim 1, it is characterised in that：Step（4）Described in
Washing after precipitation and deionized water mass ratio be 1:5, ultrasonic disperse power be 200~300W, supersonic frequency be 40~
50KHz。
6. a kind of preparation method of graphene heat conducting film according to claim 1, it is characterised in that：Step（5）Described in
Graphene oxide suspension and self-control toughness reinforcing into film liquid mass ratio be 5:1, the specific operation process of hot spray process is：Will spray
Film liquid is sprayed on polyvinyl chloride film at 100~120 DEG C at 40~50cm of polyvinyl chloride film height, control spraying
Thickness is 200~300 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710460173.5A CN107325648A (en) | 2017-06-17 | 2017-06-17 | A kind of preparation method of graphene heat conducting film |
Applications Claiming Priority (1)
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