CN106276879A - A kind of preparation method of Graphene fin - Google Patents
A kind of preparation method of Graphene fin Download PDFInfo
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- CN106276879A CN106276879A CN201610690056.3A CN201610690056A CN106276879A CN 106276879 A CN106276879 A CN 106276879A CN 201610690056 A CN201610690056 A CN 201610690056A CN 106276879 A CN106276879 A CN 106276879A
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Abstract
The invention discloses the preparation method of a kind of Graphene fin, the reduction system that the method uses metal iron powder compound with hydrochloric acid carrys out the graphene oxide water solution of reduction treatment dilute concentration, low raw-material cost, nontoxic, simple to operate, it is beneficial to batch production, can simply and effectively improve in Graphene the structural intergrity between carbon and carbon by N doping, and the organic or inorganic solid phase nitrogen source used has low cost and the advantage easily obtained, can effectively reduce manufacturing cost.
Description
Technical field
The present invention relates to electronic product radiating field, be specifically related to the preparation method of a kind of Graphene fin.
Background technology
For electronic product, its all parts effectively dispels the heat and obtains relatively low operating temperature and be used for the life-span
Extremely important impact can be produced with the speed of service.Development and progress, particularly computer chip multinuclear along with science and technology
Changing and have become as main flow, and the speed of service is constantly accelerated, power also increases, and effective heat radiation plays act to its speed of service
The effect of foot weight.At present, the heat radiation main product on market is graphite-like heat conducting film, but, its heat dispersion meets far away
The not radiating requirements of electronics and IT products radiating elements, becomes the heat radiation bottleneck of most electronic product.
Graphene (Graphene) be a kind of by carbon atom with sp2Hybrid orbital composition hexangle type is honeycomb lattice
The monolayer flat film that (honeycomb crystal lattice) is arranged to make up, the two-dimentional material of only one of which carbon atom thickness
Material.It is the hardest nano material also that Graphene is currently the thinnest, and it is almost fully transparent, only absorbs 2.3%
Light；Heat conductivity is up to 5300W/m K, and higher than CNT and diamond, under room temperature, its electron mobility exceedes
15000cm2/ (V s), again ratio CNT or silicon wafer height, and resistivity about 10-6Ω cm, lower than copper or silver, for
The material that resistivity is minimum in the world.Graphene has the most excellent physical and chemical performance, has been gradually available for transparent conductive film,
Nano electron device (transistor, transistor circuit interconnection memory semiconductor), conductive ink, solaode, lithium battery, super
The fields such as capacitor, sensor and biological medicine.
Graphene can usually be adjusted material internal conductivity and the character of conduction of heat by the different unit of doping further, passed in the past
System can be prepared the composite for electronic component by nitrogen-doped graphene.
Summary of the invention
The present invention provides the preparation method of a kind of Graphene fin, and the method uses compound the going back of metal iron powder and hydrochloric acid
Substance system carrys out the graphene oxide water solution of reduction treatment dilute concentration, and low raw-material cost is nontoxic, simple to operate, is beneficial to batch
Produce, can simply and effectively improve in Graphene the structural intergrity between carbon and carbon, and the organic or nothing used by N doping
Machine solid phase nitrogen source has low cost and the advantage easily obtained, and can effectively reduce manufacturing cost.
To achieve these goals, the invention provides the preparation method of a kind of Graphene fin, the method include as
Lower step:
(1) Graphene is prepared
In 250g native graphite and the 5L nitration mixture that is made up of 4.5L concentrated sulphuric acid and 0.5L strong phosphoric acid are mixed in reactor and electricity consumption
Control magnetic stirrer is uniform, is slowly added to 500g potassium permanganate in the case of less than 20 DEG C；Afterwards, sealed reactor is also
It is warming up to 85-90 DEG C react 2-3 hour, product is taken out from reactor lower end, be diluted to 40L solution, add 0.6L hydrogen peroxide
Obtain glassy yellow graphite oxide solution；Then, wash with acid and water alternating centrifugal, to pH value of solution=5-6, remove foreign ion；?
After, ultrasonic disperse graphite oxide, configure certain density graphene oxide solution；
The 0.5mg/mL graphene oxide solution of 2L is transferred in reactor, under magnetic stirring add 12-36g iron powder and
The concentrated hydrochloric acid of 0.8-1.8L, 75-90 DEG C is reacted 4-5 hour；Then stand, remove the iron powder of residual by hydrochloric acid filtering and washing, then
Washing sucking filtration deacidification；Last lyophilization, grinds the graphene powder that sieves to obtain；
(2) nitrogen-doped graphene
Solid phase nitrogen-containing precursor and above-mentioned graphene powder solid phase mixing form this mixture, and solid phase nitrogen source is selected from C6H12N4、
C6H5COONH4、(NH4)2CO3、HOC(CO2NH4)(CH2CO2NH4)2、HCO2NH4、C3H3N6、C11H7N、C10H6(CN)2And
C12H7NO2In at least one；The part by weight that Graphene mixes with solid phase nitrogen-containing precursor is 1:2 to 1:10；By described mixed
Compound is sintered at a temperature of 500 DEG C to 700 DEG C, and the time of sintering is 4～7 hours, obtains nitrogen-doped graphene；
(3) Graphene fin is prepared
Nitrogen-doped graphene obtained by said method is mixed with high polymer binder, to form slurry mix, will
This slurry mix is coated at least one surface of metal base, to form composite；This composite is inserted high temperature
Baking oven is dried formation fin.
Preferably, in step (1), iron powder purity > 99.0%, concentrated hydrochloric acid mass fraction concentration be 36%, described
In step (4), this high polymer binder is carboxymethyl cellulose (CMC), and the nitrogen-doped graphene content in slurry mix is
65-86wt%, this metal base is native silver.
It is an advantage of the current invention that the reduction system using metal iron powder compound with hydrochloric acid carrys out the oxygen of reduction treatment dilute concentration
Functionalized graphene aqueous solution, low raw-material cost, nontoxic, simple to operate, it is beneficial to batch production, can simply, effectively by N doping
Ground improves the structural intergrity in Graphene between carbon and carbon, and the organic or inorganic solid phase nitrogen source used has low cost and easily takes
The advantage obtained, can effectively reduce manufacturing cost.
Detailed description of the invention
Embodiment one
In 250g native graphite and the 5L nitration mixture that is made up of 4.5L concentrated sulphuric acid and 0.5L strong phosphoric acid are mixed in reactor and electricity consumption
Control magnetic stirrer is uniform, is slowly added to 500g potassium permanganate in the case of less than 20 DEG C；Afterwards, sealed reactor is also
It is warming up to 85 DEG C react 2-3 hour, product is taken out from reactor lower end, be diluted to 40L solution, add 0.6L hydrogen peroxide and obtain bright
Oxide yellow graphite solution；Then, wash with acid and water alternating centrifugal, to pH value of solution=5-6, remove foreign ion；Finally, super
Sound dispersion graphite oxide, configures certain density graphene oxide solution；
The 0.5mg/mL graphene oxide solution of 2L is transferred in reactor, adds 12g iron powder and 0.8L under magnetic stirring
Concentrated hydrochloric acid, 75 DEG C react 4 hours；Then stand, remove the iron powder of residual by hydrochloric acid filtering and washing, then wash sucking filtration deacidification；
Last lyophilization, grinds the graphene powder that sieves to obtain；Iron powder purity > 99.0%, concentrated hydrochloric acid mass fraction concentration be 36%.
Solid phase nitrogen-containing precursor and above-mentioned graphene powder solid phase mixing form this mixture, and solid phase nitrogen source is selected from
C6H12N4、C6H5COONH4、(NH4)2CO3、HOC(CO2NH4)(CH2CO2NH4)2、HCO2NH4、C3H3N6、C11H7N、C10H6(CN)2
And C12H7NO2In at least one；The part by weight that Graphene mixes with solid phase nitrogen-containing precursor is 1:2；By described mixture
Being sintered at a temperature of 500 DEG C, the time of sintering is 4 hours, obtains nitrogen-doped graphene.
Nitrogen-doped graphene obtained by said method is mixed with high polymer binder, to form slurry mixing
Thing, coats this slurry mix at least one surface of metal base, to form composite；This composite is inserted
High temperature oven is dried formation fin.This high polymer binder is carboxymethyl cellulose (CMC), the nitrogen in slurry mix
Doped graphene content is 65wt%, and this metal base is native silver.
Embodiment two
In 250g native graphite and the 5L nitration mixture that is made up of 4.5L concentrated sulphuric acid and 0.5L strong phosphoric acid are mixed in reactor and electricity consumption
Control magnetic stirrer is uniform, is slowly added to 500g potassium permanganate in the case of less than 20 DEG C；Afterwards, sealed reactor is also
It is warming up to 90 DEG C react 3 hours, product is taken out from reactor lower end, be diluted to 40L solution, add 0.6L hydrogen peroxide and obtain bright orange
Color graphite oxide solution；Then, wash with acid and water alternating centrifugal, to pH value of solution=5-6, remove foreign ion；Finally, ultrasonic
Dispersion graphite oxide, configures certain density graphene oxide solution；
The 0.5mg/mL graphene oxide solution of 2L is transferred in reactor, adds 36g iron powder and 1.8L under magnetic stirring
Concentrated hydrochloric acid, 90 DEG C react 5 hours；Then stand, remove the iron powder of residual by hydrochloric acid filtering and washing, then wash sucking filtration deacidification；
Last lyophilization, grinds the graphene powder that sieves to obtain；Iron powder purity > 99.0%, concentrated hydrochloric acid mass fraction concentration be 36%.
Solid phase nitrogen-containing precursor and above-mentioned graphene powder solid phase mixing form this mixture, and solid phase nitrogen source is selected from
C6H12N4、C6H5COONH4、(NH4)2CO3、HOC(CO2NH4)(CH2CO2NH4)2、HCO2NH4、C3H3N6、C11H7N、C10H6(CN)2
And C12H7NO2In at least one；The part by weight that Graphene mixes with solid phase nitrogen-containing precursor is 1:10；By described mixture
Being sintered at a temperature of 700 DEG C, the time of sintering is 7 hours, obtains nitrogen-doped graphene.
Nitrogen-doped graphene obtained by said method is mixed with high polymer binder, to form slurry mixing
Thing, coats this slurry mix at least one surface of metal base, to form composite；This composite is inserted
High temperature oven is dried formation fin.This high polymer binder is carboxymethyl cellulose (CMC), the nitrogen in slurry mix
Doped graphene content is 86wt%, and this metal base is native silver.
Claims (2)
1. a preparation method for Graphene fin, the method comprises the steps:
(1) Graphene is prepared
In 250g native graphite and the 5L nitration mixture that is made up of 4.5L concentrated sulphuric acid and 0.5L strong phosphoric acid are mixed in reactor and electricity consumption
Control magnetic stirrer is uniform, is slowly added to 500g potassium permanganate in the case of less than 20 DEG C；Afterwards, sealed reactor is also
It is warming up to 85-90 DEG C react 2-3 hour, product is taken out from reactor lower end, be diluted to 40L solution, add 0.6L hydrogen peroxide
Obtain glassy yellow graphite oxide solution；Then, wash with acid and water alternating centrifugal, to pH value of solution=5-6, remove foreign ion；?
After, ultrasonic disperse graphite oxide, configure certain density graphene oxide solution；
The 0.5mg/mL graphene oxide solution of 2L is transferred in reactor, under magnetic stirring add 12-36g iron powder and
The concentrated hydrochloric acid of 0.8-1.8L, 75-90 DEG C is reacted 4-5 hour；Then stand, remove the iron powder of residual by hydrochloric acid filtering and washing, then
Washing sucking filtration deacidification；Last lyophilization, grinds the graphene powder that sieves to obtain；
(2) nitrogen-doped graphene
Solid phase nitrogen-containing precursor and above-mentioned graphene powder solid phase mixing form this mixture, and solid phase nitrogen source is selected from C6H12N4、
C6H5COONH4、(NH4)2CO3、HOC(CO2NH4)(CH2CO2NH4)2、HCO2NH4、C3H3N6、C11H7N、C10H6(CN)2And
C12H7NO2In at least one；The part by weight that Graphene mixes with solid phase nitrogen-containing precursor is 1:2 to 1:10；By described mixed
Compound is sintered at a temperature of 500 DEG C to 700 DEG C, and the time of sintering is 4～7 hours, obtains nitrogen-doped graphene；
(3) Graphene fin is prepared
Nitrogen-doped graphene obtained by said method is mixed with high polymer binder, to form slurry mix, will
This slurry mix is coated at least one surface of metal base, to form composite；This composite is inserted high temperature
Baking oven is dried formation fin.
2. the method for claim 1, it is characterised in that in step (1), iron powder purity > 99.0%, concentrated hydrochloric acid
Mass fraction concentration is 36%, and in described step (4), this high polymer binder is carboxymethyl cellulose (CMC), and slurry mixes
Nitrogen-doped graphene content in thing is 65-86wt%, and this metal base is native silver.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106702195A (en) * | 2017-01-12 | 2017-05-24 | 苏州思创源博电子科技有限公司 | Preparation method for graphene and copper composite conductor |
| CN106735250A (en) * | 2017-01-12 | 2017-05-31 | 苏州思创源博电子科技有限公司 | A kind of preparation method of compound titanium alloy material |
| CN106756176A (en) * | 2017-01-26 | 2017-05-31 | 苏州思创源博电子科技有限公司 | A kind of preparation method of Al-alloy material |
| CN106957053A (en) * | 2017-04-13 | 2017-07-18 | 山东玉皇新能源科技有限公司 | A kind of iron powder is the method for the quick macroscopic preparation of graphene of reducing agent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626158A (en) * | 2012-08-23 | 2014-03-12 | 中国科学院宁波材料技术与工程研究所 | Preparation method of nitrogen doped graphene and application of nitrogen doped graphene |
| CN104150470A (en) * | 2014-07-31 | 2014-11-19 | 山东玉皇新能源科技有限公司 | Metal-solution reduction method for preparing graphene |
-
2016
- 2016-08-19 CN CN201610690056.3A patent/CN106276879A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626158A (en) * | 2012-08-23 | 2014-03-12 | 中国科学院宁波材料技术与工程研究所 | Preparation method of nitrogen doped graphene and application of nitrogen doped graphene |
| CN104150470A (en) * | 2014-07-31 | 2014-11-19 | 山东玉皇新能源科技有限公司 | Metal-solution reduction method for preparing graphene |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106702195A (en) * | 2017-01-12 | 2017-05-24 | 苏州思创源博电子科技有限公司 | Preparation method for graphene and copper composite conductor |
| CN106735250A (en) * | 2017-01-12 | 2017-05-31 | 苏州思创源博电子科技有限公司 | A kind of preparation method of compound titanium alloy material |
| CN106756176A (en) * | 2017-01-26 | 2017-05-31 | 苏州思创源博电子科技有限公司 | A kind of preparation method of Al-alloy material |
| CN106957053A (en) * | 2017-04-13 | 2017-07-18 | 山东玉皇新能源科技有限公司 | A kind of iron powder is the method for the quick macroscopic preparation of graphene of reducing agent |
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Application publication date: 20170104 |