CN102145888A - Preparation method of grapheme three-dimensional entity - Google Patents
Preparation method of grapheme three-dimensional entity Download PDFInfo
- Publication number
- CN102145888A CN102145888A CN 201110090764 CN201110090764A CN102145888A CN 102145888 A CN102145888 A CN 102145888A CN 201110090764 CN201110090764 CN 201110090764 CN 201110090764 A CN201110090764 A CN 201110090764A CN 102145888 A CN102145888 A CN 102145888A
- Authority
- CN
- China
- Prior art keywords
- graphene
- solution
- solid
- solid preparation
- preparation
- 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
Abstract
The invention discloses a method for preparing a grapheme three-dimensional entity with a hydrothermal reduction method. The method comprises the following steps of: mixing oxidized grapheme with water; stirring or ultrasonically dispersing to form an oxidized grapheme solution with the mass volume concentration between 1 mg/ml and 10 mg/ml; adding an alkali solution to adjust the pH value of the solution to 8-13; pouring the solution into a hydrothermal reaction kettle; putting the reaction kettle into a drying oven and raising the temperature to 100-400 DEG C for reacting for 3-48 hours; cooling; and taking the product out and drying to obtain the grapheme three-dimensional entity. The grapheme entity prepared with the method has a smooth surface, high density and high electric conductivity. The preparation method is convenient to operate, and is simple and practical.
Description
Technical field
The present invention relates to a kind of preparation method of Graphene 3D solid.
Background technology
Along with the discovery of Graphene, the electrical properties that it is excellent, mechanical property, thermal property and magnetic property have caused people's extensive concern, and the method for preparing Graphene simultaneously also emerges in an endless stream, mainly contain micromechanics and peel off method (Novoselov, K.S., Geim, A.K., Morozov, S.V., Jiang, D., Zhang Y., Dubonos, S.V.et al.Science 2004,306,666), chemical method (Stankovich, S., Dikin, D.A.et al.Carbon 2007,45,1558) and epitaxial growth method (Kim, K.S., Zhao, Y.et al.Nature 2009,457,706), the researchist has carried out the research of many-sided character to the Graphene that these methods make, and is the following graphene film of micron dimension but the object of research mostly is a thickness.The Graphene 3D solid is that the mixed and disorderly reunion of graphene film forms together, and the number of plies is more and in conjunction with more mixed and disorderly, thickness is more than 100 microns, in the prior art, few people study preparation (Park, the S.J. of Graphene 3D solid, An, J.H., Suk, J.W., Ruoff, R.S.Small 2009,6, and 210; Chen, H., Muller, M.B., Gilmore, K.J., Wallace, G.G., Li, D.Adv.Mater.2008,20,3557).Some researchist utilizes the hydrothermal reduction method to prepare Graphene 3D solid (Xu, Y.X., Sheng, K.X., Li, C.et al.ACS NANO 2010,4,4324), their power, electrical property have had large increase with respect to the entity performance of utilizing colloid self-assembly gained in the past, but these entities all are to obtain under the prerequisite that does not add basic solution, cause the surface of these entities very coarse, density is not high yet in addition, makes it can not satisfy the requirement in a lot of fields.
Summary of the invention
The invention provides a kind of method for preparing the Graphene 3D solid, prepared Graphene 3D solid smooth surface, the density height, intensity, density and specific conductivity have all obtained large increase simultaneously.
The present invention adopts the hydrothermal reduction method, prepare according to the method that may further comprise the steps: graphene oxide is mixed with water, stir or ultra-sonic dispersion, forming the quality volumetric concentration is the graphene oxide solution of 1mg/ml-10mg/ml, then add basic solution, and make the pH value of solution value be in the scope of 8-13; This solution is poured in the hydrothermal reaction kettle, placed loft drier to be warming up to 100 ℃ of-400 ℃ of reactions, continue 3h 48h, oven dry is taken out in cooling then, obtains the Graphene 3D solid.
As a kind of improvement of the present invention, the temperature of reaction of loft drier is set at 150 ℃-280 ℃, the product quality that makes like this is better.
A kind of improvement of the present invention, after solution was poured in the hydrothermal reaction kettle, the reaction times that places loft drier was for continuing 8h-24h, the same like this product quality that improves.
Used alkaline solution is any or several combination in ammoniacal liquor, sodium hydroxide, potassium hydroxide, the yellow soda ash in the preparation process of the present invention, can certainly be other similar alkaline solutions.
A kind of improvement of the present invention is modulated at the pH value of graphene oxide solution between the 9-11, adds the amount of various alkaline matters according to this value control, helps improving product quality.
A kind of improvement of the present invention, reactor place rate-controlling that loft drier heats up at 5 ℃/min-100 ℃/min.
Negative pressure or normal pressure oven dry are adopted in a kind of improvement of the present invention, the oven dry of Graphene 3D solid, and bake out temperature is controlled at 10 ℃-80 ℃.
The present invention places reactor with graphene oxide solution, utilize High Temperature High Pressure to obtain the Graphene after the reduction, in the process of reaction, utilize the colloidal property of Graphene and the character that reduction back hydrophobic is reunited, obtained the good Graphene 3D solid of power electrical property, the particularly adding of alkaline solution, played the effect of following two aspects: the one, alkali itself also can reduce to graphene oxide, so assisted the hydrothermal method redox graphene to a certain extent; The 2nd, the adding of alkali makes the particle size that is combined into the Graphene entity reduce.Comprehensive the two make the surface roughness of Graphene 3D solid decline to a great extent and density is greatly improved, mechanical property and electric property all are greatly increased simultaneously, have opened up a new road thereby the macroscopic view of Graphene used.The preparation method is easy to operate, and is simple.
Description of drawings
Fig. 1 is not for adding the scanning electron microscopy sheet of the prepared Graphene 3D solid of ammoniacal liquor.
Fig. 2 is the scanning electron microscopy sheet that adds the prepared Graphene 3D solid of ammoniacal liquor modulation pH=10.
Fig. 3 is the section low power scanning electron photomicrograph that adds the prepared Graphene 3D solid of ammoniacal liquor modulation pH=10.
Fig. 4 is the section high power scanning electron photomicrograph that adds the prepared Graphene 3D solid of ammoniacal liquor modulation pH=10.
Fig. 5 is the scanning electron microscopy sheet that adds the prepared Graphene 3D solid of ammoniacal liquor modulation pH=8.
Fig. 6 is the scanning electron microscopy sheet of the prepared Graphene 3D solid of hydro-oxidation sodium modulation pH=13.
Embodiment:
Embodiment 1: the first step, take by weighing the graphene oxide sheet of 55mg, and place beaker, in beaker, add the 33ml deionized water, then carry out ultra-sonic dispersion (40KHz, 15min), make solution not have obvious particle, adding ammoniacal liquor then, to make the pH value of solution value be 10;
Second step, solution in the beaker is poured in the interior cup of hydrothermal reaction kettle (volume 50ml), tightened outer cup/lid, erect and put into loft drier, temperature rise rate is set is 50 ℃/min, temperature of reaction and be 180 ℃, reaction times is 15h, and question response finishes the back naturally cooling.The scanning electron microscopy sheet of obtained Graphene 3D solid can be observed smooth surface as shown in Figure 2;
In the 3rd step, the entity that makes is carried out the drying of 15h under 45 ℃, normal pressure; The scanning electron photomicrograph of dried product exhibited as shown in Figure 3 and Figure 4.Fig. 3 is the low power scanning electron photomicrograph, has presented the entire profile of sample, does not see defectives such as hole crack from figure, in conjunction with fine and close; Fig. 4 is the high power scanning electron photomicrograph, proves that further the graphene film bonded is very fine and close.
Dry-eye disease has been carried out the measurement of density, specific conductivity and hardness, also compared simultaneously, referring to table 1 with the situation that does not add ammoniacal liquor.Because the raising of density makes the density of sample and specific conductivity improve a lot.
Table 1
Embodiment 2: the preparation method is substantially with embodiment 1, difference is: the dispersion of graphene oxide realizes that by stirring added less ammoniacal liquor simultaneously and made pH value of solution=8, Fig. 5 is the scanning electron microscopy sheet of gained Graphene 3D solid, as can be seen, the gained solid object surface is also very smooth.Table 2 compares for this Graphene 3D solid and the correlated performance that does not add ammoniacal liquor gained 3D solid.
| Sample | Density (g/cm 3) | Specific conductivity (S/cm) | Hardness (HV) |
| Do not add ammoniacal liquor | 1.43 | 6.3×10 -3 | 14.5 |
| Add ammoniacal liquor (pH=8) | 1.66 | 7.2×10 -2 | 15.3 |
Table 2
Embodiment 3: the preparation method is substantially with embodiment 1, and difference is: the loft drier temperature rise rate is set to 5 ℃/min, obtains similar results as shown in Figure 2 equally, and performance comparison is referring to table 3.
Embodiment 4: the preparation method is substantially with embodiment 1, and difference is: the loft drier temperature rise rate is made as 100 ℃/min, and the gained result is similar to shown in Figure 2, and the contrast of the performance perameter of preparing product sees Table 3 under the different temperature rise rates.
| Temperature rise rate | Density (g/cm 3) | Specific conductivity (S/cm) | Hardness (HV) |
| 5℃/min | 1.65 | 7.5×10 -2 | 15.6 |
| 50℃/min | 1.68 | 7.8×10 -2 | 15.8 |
| 100℃/min | 1.67 | 7.3×10 -2 | 15.4 |
Table 3
Embodiment 5: the preparation method is substantially with embodiment 1, difference is: basic solution is a sodium hydroxide solution, and modulating the pH value simultaneously is 13, has obtained result shown in Figure 6, Graphene 3D solid smooth surface, relevant surface sweeping electron photomicrograph is similar to Fig. 3, Fig. 4.
Embodiment 6: the preparation method is substantially with embodiment 1, and difference is: basic solution is a potassium hydroxide, and modulating the pH value simultaneously is 13, has obtained similar results as shown in Figure 6 equally.
Embodiment 7: the preparation method is substantially with embodiment 1, and difference is: basic solution is a sodium carbonate solution, has obtained similar results shown in Figure 2 equally.
Embodiment 8: the preparation method is substantially with embodiment 1, and difference is: the loft drier temperature of reaction is made as 100 ℃, obtains similar results as shown in Figure 2 equally, the similar Fig. 3 of scanning electron photomicrograph, and performance perameter contrasts referring to table 4.
Embodiment 9: the preparation method is substantially with embodiment 1, and difference is: the loft drier temperature of reaction is made as 400 ℃, obtains Fig. 2, similar results shown in Figure 3 equally, and performance perameter contrasts referring to table 4.
| The differential responses temperature (℃) | Density (g/cm 3) | Specific conductivity (S/cm) | Hardness (HV) |
| 100 | 1.63 | 7.2×10 -2 | 15.3 |
| 180 | 1.68 | 7.8×10 -2 | 15.8 |
| 400 | 1.71 | 7.9×10 -2 | 16.0 |
Table 4
Embodiment 10: the preparation method is substantially with embodiment 1, and difference is: duration of the reaction is 3h in loft drier, obtains equally as Fig. 2, similar results shown in Figure 3, and the correlated performance contrast sees Table 5.
Embodiment 11: the preparation method is substantially with embodiment 1, and difference is: duration of the reaction is 48h in loft drier, obtains Fig. 2, similar results shown in Figure 3 equally, and performance perameter contrasts referring to table 5.
| The differential responses time (h) | Density (g/cm 3) | Specific conductivity (S/cm) | Hardness (HV) |
| 3 | 1.64 | 7.4×10 -2 | 15.6 |
| 15 | 1.68 | 7.8×10 -2 | 15.8 |
| 48 | 1.70 | 8.0×10 -2 | 15.9 |
Table 5
Embodiment 12: the preparation method is substantially with embodiment 1, and difference is: the quality volumetric concentration of graphene oxide solution is mixed with 1mg/ml, and the oven dry of Graphene 3D solid is negative pressure oven dry, has obtained being similar to Fig. 3, result shown in Figure 4.
Embodiment 13: the preparation method is substantially with embodiment 1, and difference is: the concentration of graphene oxide solution is mixed with 10mg/ml, and bake out temperature is 10 ℃, obtains being similar to Fig. 3, result shown in Figure 4 equally.
Embodiment 14: the preparation method is substantially with embodiment 1, and difference is: bake out temperature is 80 ℃, obtains being similar to Fig. 3, result shown in Figure 4 equally.
Embodiment 15: the preparation method is substantially with embodiment 1, and difference is: the amount of regulating ammoniacal liquor makes pH=9, and temperature of reaction becomes 150 ℃ simultaneously, and the reaction times changes 24h into, and the gained result is similar to Fig. 2, Fig. 3.Relevant performance perameter contrast is referring to table 6.
Embodiment 16: the preparation method is substantially with example 5, and difference is: the amount of regulating sodium hydroxide makes pH=11, and temperature of reaction becomes 280 ℃ simultaneously, and the reaction times becomes 8h, and the gained result is similar to Fig. 4, Fig. 6.The correlated performance parameter comparison is referring to table 6.
| Sample | Density (g/cm 3) | Specific conductivity (S/cm) | Hardness (HV) |
| Embodiment 15 | 1.65 | 7.5×10 -2 | 16.0 |
| |
1.67 | 7.9×10 -2 | 15.7 |
Table 6
Claims (7)
1. a Graphene 3D solid preparation method is characterized in that, graphene oxide is mixed with water, stir or ultra-sonic dispersion, forming the quality volumetric concentration is the graphene oxide solution of 1mg/ml-10mg/ml, then adds basic solution, and makes the pH value of solution value be in 8-13 scope; This solution is poured in the hydrothermal reaction kettle, placed loft drier to be warming up to 100 ℃ of-400 ℃ of reactions, continue 3h-48h, oven dry is taken out in cooling then, obtains the Graphene 3D solid.
2. Graphene 3D solid preparation method according to claim 1 is characterized in that: described temperature of reaction is 150 ℃-280 ℃.
3. Graphene 3D solid preparation method according to claim 1 is characterized in that: the described reaction times is for continuing 8h-24h.
4. Graphene 3D solid preparation method according to claim 1 is characterized in that, described alkaline solution is any or several combination in ammoniacal liquor, sodium hydroxide, potassium hydroxide, the yellow soda ash.
5. Graphene 3D solid preparation method according to claim 1 is characterized in that described pH value is between 9-11.
6. according to the described arbitrary Graphene 3D solid preparation method of claim 1-5, it is characterized in that described reactor places speed that loft drier heats up at 5 ℃/min-100 ℃/min.
7. according to the described arbitrary Graphene 3D solid preparation method of claim 1-5, it is characterized in that the oven dry of described Graphene 3D solid is negative pressure or normal pressure oven dry, bake out temperature is controlled at 10 ℃-80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110090764 CN102145888A (en) | 2011-04-12 | 2011-04-12 | Preparation method of grapheme three-dimensional entity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110090764 CN102145888A (en) | 2011-04-12 | 2011-04-12 | Preparation method of grapheme three-dimensional entity |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102145888A true CN102145888A (en) | 2011-08-10 |
Family
ID=44420388
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110090764 Pending CN102145888A (en) | 2011-04-12 | 2011-04-12 | Preparation method of grapheme three-dimensional entity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102145888A (en) |
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500133A (en) * | 2011-10-15 | 2012-06-20 | 东南大学 | Application method of graphene sponge |
| CN102515144A (en) * | 2011-12-23 | 2012-06-27 | 哈尔滨工业大学 | Method for preparing porous carbon microspheres converted from graphene |
| CN102515148A (en) * | 2011-11-25 | 2012-06-27 | 东南大学 | Method for casting graphene cast body |
| CN102633257A (en) * | 2012-05-04 | 2012-08-15 | 东南大学 | Method for synthesizing less than 10 nm of single-layer graphene quantum dot biological imaging agent |
| CN102646810A (en) * | 2012-04-27 | 2012-08-22 | 宁波工程学院 | Preparation method for three-dimensional porous graphene doping and coating lithium titanate composite anode material |
| CN102897756A (en) * | 2012-09-19 | 2013-01-30 | 电子科技大学 | Preparation method of graphene |
| CN103420364A (en) * | 2013-07-13 | 2013-12-04 | 西南交通大学 | Preparation method of grapheme/hydroxyapatite composite material |
| CN103482612A (en) * | 2013-08-30 | 2014-01-01 | 西北工业大学 | Method for preparing graphene by reducing graphite oxide |
| CN103881278A (en) * | 2014-03-26 | 2014-06-25 | 东南大学 | Method for preparing three-dimensional porous nano composite material of graphene oxide-water soluble polymer |
| CN103896256A (en) * | 2012-12-26 | 2014-07-02 | 海洋王照明科技股份有限公司 | Preparation method for graphene gel |
| CN103924261A (en) * | 2014-04-18 | 2014-07-16 | 西南大学 | Preparation method for oxygen evolution electrode based on graphene oxide reduction |
| CN104016339A (en) * | 2014-06-20 | 2014-09-03 | 天津大学 | Preparation method of activated graphene material |
| CN104148663A (en) * | 2014-07-15 | 2014-11-19 | 东南大学 | Method for efficiently preparing silver nano particle-graphene three-dimensional composite structure |
| CN104591172A (en) * | 2015-01-22 | 2015-05-06 | 南京理工大学 | Preparation method for graphene |
| CN105107543A (en) * | 2015-09-30 | 2015-12-02 | 东南大学 | Nonmetal catalyst-doped reduced graphene oxide and preparing method and application thereof |
| CN105321724A (en) * | 2015-11-20 | 2016-02-10 | 中国科学技术大学 | Three-dimensional porous graphene, preparation method and application therefor |
| CN105645403A (en) * | 2016-03-28 | 2016-06-08 | 南京邮电大学 | Preparation method of high-performance nitrogen-doped three-dimensional graphene |
| CN105826523A (en) * | 2016-03-17 | 2016-08-03 | 北京理工大学 | Lithium-sulfur battery positive pole material and preparation method thereof |
| CN106315566A (en) * | 2016-08-15 | 2017-01-11 | 安徽师范大学 | Preparation method of graphene |
| CN106592007A (en) * | 2016-04-29 | 2017-04-26 | 北京纳米能源与系统研究所 | Graphene micron fibers and preparation method thereof, nerve tissue scaffold, and repair system |
| CN108144425A (en) * | 2018-03-03 | 2018-06-12 | 深圳市太鸟科技有限公司 | A kind of carbon-based composite sulfur removal material of three-dimensional grapheme and preparation method thereof |
| CN111900402A (en) * | 2020-07-29 | 2020-11-06 | 肇庆市华师大光电产业研究院 | Universal electrode material for lithium-sulfur battery and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090068470A1 (en) * | 2007-09-12 | 2009-03-12 | Samsung Electronics Co., Ltd. | Graphene shell and process of preparing the same |
| CN101837972A (en) * | 2010-05-28 | 2010-09-22 | 南京邮电大学 | Graphene three-dimensional structure and preparation method thereof |
| CN101857222A (en) * | 2010-05-28 | 2010-10-13 | 常州大学 | Preparation method of large-area and continuous graphen/zinc oxide composite structure |
| EP2256087A1 (en) * | 2009-05-26 | 2010-12-01 | Belenos Clean Power Holding AG | Stable dispersions of single and multiple graphene layers in solution |
| CN101982408A (en) * | 2010-10-20 | 2011-03-02 | 天津大学 | Graphene three-dimensional material as well as preparation method and application thereof |
-
2011
- 2011-04-12 CN CN 201110090764 patent/CN102145888A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090068470A1 (en) * | 2007-09-12 | 2009-03-12 | Samsung Electronics Co., Ltd. | Graphene shell and process of preparing the same |
| EP2256087A1 (en) * | 2009-05-26 | 2010-12-01 | Belenos Clean Power Holding AG | Stable dispersions of single and multiple graphene layers in solution |
| CN101837972A (en) * | 2010-05-28 | 2010-09-22 | 南京邮电大学 | Graphene three-dimensional structure and preparation method thereof |
| CN101857222A (en) * | 2010-05-28 | 2010-10-13 | 常州大学 | Preparation method of large-area and continuous graphen/zinc oxide composite structure |
| CN101982408A (en) * | 2010-10-20 | 2011-03-02 | 天津大学 | Graphene three-dimensional material as well as preparation method and application thereof |
Cited By (31)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500133A (en) * | 2011-10-15 | 2012-06-20 | 东南大学 | Application method of graphene sponge |
| WO2013075498A1 (en) * | 2011-11-25 | 2013-05-30 | 东南大学 | Method for casting a graphene cast body |
| CN102515148A (en) * | 2011-11-25 | 2012-06-27 | 东南大学 | Method for casting graphene cast body |
| CN102515148B (en) * | 2011-11-25 | 2013-12-25 | 东南大学 | Method for casting graphene cast body |
| CN102515144A (en) * | 2011-12-23 | 2012-06-27 | 哈尔滨工业大学 | Method for preparing porous carbon microspheres converted from graphene |
| CN102646810A (en) * | 2012-04-27 | 2012-08-22 | 宁波工程学院 | Preparation method for three-dimensional porous graphene doping and coating lithium titanate composite anode material |
| CN102633257A (en) * | 2012-05-04 | 2012-08-15 | 东南大学 | Method for synthesizing less than 10 nm of single-layer graphene quantum dot biological imaging agent |
| CN102897756A (en) * | 2012-09-19 | 2013-01-30 | 电子科技大学 | Preparation method of graphene |
| CN103896256A (en) * | 2012-12-26 | 2014-07-02 | 海洋王照明科技股份有限公司 | Preparation method for graphene gel |
| CN103420364A (en) * | 2013-07-13 | 2013-12-04 | 西南交通大学 | Preparation method of grapheme/hydroxyapatite composite material |
| CN103420364B (en) * | 2013-07-13 | 2016-02-03 | 西南交通大学 | A kind of preparation method of grapheme/hydroxyapatcomposite composite material |
| CN103482612A (en) * | 2013-08-30 | 2014-01-01 | 西北工业大学 | Method for preparing graphene by reducing graphite oxide |
| CN103482612B (en) * | 2013-08-30 | 2015-10-21 | 西北工业大学 | A kind of method of reduction-oxidation preparing graphite alkene |
| CN103881278A (en) * | 2014-03-26 | 2014-06-25 | 东南大学 | Method for preparing three-dimensional porous nano composite material of graphene oxide-water soluble polymer |
| CN103924261A (en) * | 2014-04-18 | 2014-07-16 | 西南大学 | Preparation method for oxygen evolution electrode based on graphene oxide reduction |
| CN103924261B (en) * | 2014-04-18 | 2017-03-01 | 西南大学 | Oxygen based on reduced graphene oxide serving separates out the preparation method of electrode |
| CN104016339A (en) * | 2014-06-20 | 2014-09-03 | 天津大学 | Preparation method of activated graphene material |
| CN104148663A (en) * | 2014-07-15 | 2014-11-19 | 东南大学 | Method for efficiently preparing silver nano particle-graphene three-dimensional composite structure |
| CN104591172A (en) * | 2015-01-22 | 2015-05-06 | 南京理工大学 | Preparation method for graphene |
| CN105107543A (en) * | 2015-09-30 | 2015-12-02 | 东南大学 | Nonmetal catalyst-doped reduced graphene oxide and preparing method and application thereof |
| CN105321724A (en) * | 2015-11-20 | 2016-02-10 | 中国科学技术大学 | Three-dimensional porous graphene, preparation method and application therefor |
| CN105826523A (en) * | 2016-03-17 | 2016-08-03 | 北京理工大学 | Lithium-sulfur battery positive pole material and preparation method thereof |
| CN105645403A (en) * | 2016-03-28 | 2016-06-08 | 南京邮电大学 | Preparation method of high-performance nitrogen-doped three-dimensional graphene |
| CN105645403B (en) * | 2016-03-28 | 2018-06-22 | 南京邮电大学 | A kind of preparation method of high-performance N doping three-dimensional grapheme |
| CN106592007A (en) * | 2016-04-29 | 2017-04-26 | 北京纳米能源与系统研究所 | Graphene micron fibers and preparation method thereof, nerve tissue scaffold, and repair system |
| CN106592007B (en) * | 2016-04-29 | 2019-03-15 | 北京纳米能源与系统研究所 | Graphene micrometer fibers, preparation method, nerve fiber bracket and repair system |
| CN106315566A (en) * | 2016-08-15 | 2017-01-11 | 安徽师范大学 | Preparation method of graphene |
| CN106315566B (en) * | 2016-08-15 | 2018-09-04 | 安徽师范大学 | A kind of preparation method of graphene |
| CN108144425A (en) * | 2018-03-03 | 2018-06-12 | 深圳市太鸟科技有限公司 | A kind of carbon-based composite sulfur removal material of three-dimensional grapheme and preparation method thereof |
| CN108144425B (en) * | 2018-03-03 | 2021-02-09 | 深圳市太鸟科技有限公司 | Three-dimensional graphene carbon-based composite desulfurization material and preparation method thereof |
| CN111900402A (en) * | 2020-07-29 | 2020-11-06 | 肇庆市华师大光电产业研究院 | Universal electrode material for lithium-sulfur battery and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102145888A (en) | Preparation method of grapheme three-dimensional entity | |
| Pham et al. | Covalent functionalization of graphene oxide with polyglycerol and their use as templates for anchoring magnetic nanoparticles | |
| CN106344937B (en) | monolayer molybdenum disulfide-cobalt ferrite nanocomposite and preparation method and application thereof | |
| Shen et al. | Facile synthesis of NiCo2O4-reduced graphene oxide nanocomposites with improved electrochemical properties | |
| Wen et al. | Organosilane-functionalized graphene quantum dots and their encapsulation into bi-layer hollow silica spheres for bioimaging applications | |
| CN104058392B (en) | A kind of preparation method of graphene colloid dispersion solution | |
| Shen et al. | Hydrothermal synthesis of magnetic reduced graphene oxide sheets | |
| CN102745752A (en) | Method of synthesizing mesoporous nickel cobalt oxide nanowire using hydrothermal method and application thereof | |
| CN110040724B (en) | Preparation method of folded graphene and electromagnetic shielding material thereof | |
| CN110527279B (en) | Material with high light-heat conversion efficiency and high heat conductivity coefficient and preparation method thereof | |
| CN104538145A (en) | Multi-scale uniform and single-dispersion magnetic microsphere and preparation method thereof | |
| CN106883818B (en) | Hud typed carbon ball/carbon nano tube composite wave-absorbing material and preparation method | |
| CN103723705A (en) | Graphene/nano-aluminum compound and preparation method thereof | |
| WO2017074086A1 (en) | Method for preparing magnetic iron oxide-graphene composite | |
| CN104439276B (en) | A kind of quick method and product preparing hollow porous silica/argentum nano composite material | |
| CN106145097A (en) | The preparation method of the redox graphene that a kind of hydrophilic and hydrophobic is controlled | |
| CN107161989A (en) | A kind of preparation method of cellular three-dimensional grapheme | |
| CN110092420A (en) | A kind of Fe3O4The preparation method of/porous graphene composite material | |
| Li et al. | Ultrasonic-assisted preparation of graphene oxide carboxylic acid polyvinyl alcohol polymer film and studies of thermal stability and surface resistivity | |
| CN103435037A (en) | Method for preparing graphene/Pt nanocomposite material by liquid phase reduction method | |
| Zheng et al. | Self-supported construction of three-dimensional NiCo2O4 hierarchical nanoneedles for high-performance microwave absorption | |
| Ma et al. | Lignin-derived hierarchical porous flower-like carbon nanosheets decorated with biomass carbon quantum dots for efficient oxygen reduction | |
| Shu et al. | High-efficient electromagnetic wave absorption of coral-like Co/CoO/RGO hybrid aerogels with good hydrophobic and thermal insulation properties | |
| CN102515147A (en) | Method for preparing tri-metal tetra-oxide/graphene nanocomposite material | |
| CN103641101A (en) | Two-dimensional structural carbon nanomaterial 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: 20110810 |