CN102583316A - Method for preparing carbon materials rich in nano diamond structure - Google Patents
Method for preparing carbon materials rich in nano diamond structure Download PDFInfo
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- CN102583316A CN102583316A CN2012100402782A CN201210040278A CN102583316A CN 102583316 A CN102583316 A CN 102583316A CN 2012100402782 A CN2012100402782 A CN 2012100402782A CN 201210040278 A CN201210040278 A CN 201210040278A CN 102583316 A CN102583316 A CN 102583316A
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Abstract
The invention relates to a method for preparing carbon materials rich in a nano diamond structure, which comprises the following steps: firstly, placing titanium carbide powder into a high-energy ball mill to carry out ball milling pretreatment, wherein in the ball milling process, the ratio of ball to powder is 4:1 to 6:1, the rotating speed of the ball mill is 180 to 220 revolutions per minute, the ball milling time is 5 to 20 hours and the titanium carbide powder is ground and refined to have the particle size of 0.5 to 2.0mum; and then, placing the titanium carbide powder subjected to ball milling into a fused quartz tube furnace, filling argon after vacuumizing to the pressure of 0.05 to 1Pa, heating the tube furnace to 900 to 1,200 DEG C, filling chlorine gas at a flow velocity of 20 to 30ml/min, carrying out chlorination for 1 to 2 hours, filling the argon again after the reaction is finished, and cooling to the room temperature along with the furnace. The method has the advantages that the method has simple synthesis process and high efficiency; and a great amount of carbon materials rich in nano diamond with the particle size of 5 to 10 nanometers can be prepared.
Description
Technical field
The present invention relates to field of novel carbon material, particularly a kind of preparation method of carbon material.
Background technology
Nano diamond has a extensive future at many key areas because of having high hardness and ultimate compression strength, good optical property, preferable excellent properties such as biocompatibility.Therefore, the technology of preparing of researchdevelopment Nano diamond and method receive much concern always.
Up to now; People have been developed the multiple method for preparing Nano diamond; Wherein mainly comprise: (1) explosive detonation synthesis method: be to make it become diamond through compressed graphite in the explosive detonation process, this is traditional method of utilizing the explosive detonation synthesizing nano diamond; (2) laser bombardment synthesis method: be to bombard through the high speed of laser to make carbon dust change diamond into, Sun Jing etc. utilize laser bombardment carbon dust suspension-s to synthesize Nano diamond; (3) high-current pulsed electron beam irradiation synthesis method: be to utilize the high-current pulsed electron beam irradiation to make graphite change diamond into, Gao Bo etc. utilize high-current pulsed electron beam irradiation graphite suspension to synthesize Nano diamond.Yet; Can be mixed with a large amount of metallic impurity in the tradition detonation method synthetic Nano diamond; These impurity have considerable influence to the quality of Nano diamond, further purification ratio difficulty, though and utilize the suspension-s of laser, strong pulse electron beam irradiation carbon can prepare than the pure nano diamond; But because laser, the strong pulse electron beam equipment involves great expense and synthesis rate is slower, is difficult to large-scale promotion application.
Summary of the invention
The object of the present invention is to provide simple, with low cost, the colory preparation method who is rich in the carbon material of Nano diamond structure of a kind of technology.
The present invention mainly is to be reaction raw materials with the titanium carbide, at first titanium carbide is carried out ball milling pretreatment, then the titanium carbide behind the ball milling is carried out that the high temperature halogenating reaction realizes.
Preparing method of the present invention is following:
(1) ball milling pretreatment of titanium carbide powder: the titanium carbide powder is put into high energy ball mill carry out ball milling pretreatment, make the fragmentation of titanium carbide powder particle diameter be refined to 0.5 ~ 2.0 μ m.Grinding element during ball milling is the GCr15 steel ball of bearing steel, and the mass ratio of steel ball and titanium carbide powder (being ball-to-powder weight ratio) is 4:1 ~ 6:1, and the rotating speed of ball mill is 180 ~ 220 rev/mins, and the ball milling time is 5 ~ 20 hours.Reunite for titanium carbide powder during preventing ball milling, select for use ethanol as dispersion agent.
(2) the high temperature halogenation treatment of titanium carbide powder: the titanium carbide powder behind the above-mentioned ball milling is put into fused quartz tubular type stove; Feed argon gas after being evacuated to 0.05 ~ 1Pa, tube furnace is warming up to 900 ~ 1200 ℃, feed chlorine again; Flow velocity is 20 ~ 30ml/min, and the time is 1 ~ 2 hour; Feed argon gas once more after reaction finishes, utilize the souring of argon gas stream to remove the residual muriates such as titanium tetrachloride in carbonized titanium powder surface, cool to the carbon material that can obtain to be rich in the Nano diamond structure after the room temperature with the furnace.
The present invention compared with prior art has following advantage: synthesis technique is simple, with low cost, resultant velocity is fast, efficient is high, and prepared carbon material is best in quality, contains the Nano diamond that a large amount of size distribution are 5 ~ 10 nanometers.
Description of drawings
Fig. 1 is the Electronic Speculum figure of the carbon material that obtained of the embodiment of the invention 1.
Fig. 2 is the high-resolution electron microscopy figure of stain shown in Fig. 1 (Nano diamond).
Fig. 3 is the Electronic Speculum figure of the carbon material that obtained of the embodiment of the invention 2.
Fig. 4 is the high-resolution electron microscopy figure of stain shown in Fig. 3 (Nano diamond).
Embodiment
Embodiment 1
Getting granularity is 800 purpose titanium carbide powder 20g, puts into high energy ball mill, puts into 80g GCr15 steel ball of bearing steel again; For titanium carbide powder during preventing ball milling is reunited; Put into 1ml ethanol as dispersion agent, the rotating speed of ball mill is 220 rev/mins, and the ball milling time is 5 hours.At this moment, titanium carbide powder particle diameter is about 2.0 μ m.Then the titanium carbide powder that obtains behind the above-mentioned ball milling is put into fused quartz tubular type stove, feed argon gas after being evacuated to 0.1Pa.The tube furnace temperature is risen to 900 ℃, feed chlorine, flow velocity is 30ml/min, and the time is 2 hours.Feed argon gas again after reaction finishes, remove the residual muriate in carbonized titanium powder surface, cool to room temperature with the furnace after, can obtain to be rich in the carbon material of Nano diamond structure.
As depicted in figs. 1 and 2, be rich in the Nano diamond that size distribution is 5 ~ 10 nanometers in the prepared carbon material.
Embodiment 2
Getting granularity is 800 purpose titanium carbide powder 20g, puts into high energy ball mill, puts into 120g GCr15 steel ball of bearing steel again; For titanium carbide powder during preventing ball milling is reunited; Put into 1ml ethanol as dispersion agent, the rotating speed of ball mill is 180 rev/mins, and the ball milling time is 20 hours.At this moment, titanium carbide powder particle diameter is about 0.5 μ m.Then the titanium carbide powder that obtains behind the above-mentioned ball milling is put into fused quartz tubular type stove, feed argon gas after being evacuated to 1Pa.The tube furnace temperature is risen to 1200 ℃, feed chlorine, flow velocity is 20ml/min, and the time is 1 hour.Reaction feeds argon gas after finishing again, removes the residual muriate in carbonized titanium powder surface.After cooling to room temperature with the furnace, can obtain to be rich in the carbon material of Nano diamond structure.
Like Fig. 3 and shown in Figure 4, to compare with embodiment 1, the Nano diamond that contains in the carbon material that present embodiment obtains is more.
Embodiment 3
Getting granularity is 800 purpose titanium carbide powder 20g, puts into high energy ball mill, puts into 100g GCr15 steel ball of bearing steel again; For titanium carbide powder during preventing ball milling is reunited; Put into 1ml ethanol as dispersion agent, the rotating speed of ball mill is 200 rev/mins, and the ball milling time is 15 hours.At this moment, titanium carbide powder particle diameter is about 0.9 μ m.Then the titanium carbide powder that obtains behind the above-mentioned ball milling is put into fused quartz tubular type stove, feed argon gas after being evacuated to 0.05Pa.The tube furnace temperature is risen to 1100 ℃, feed chlorine, flow velocity is 25ml/min, and the time is 1.5 hours.Reaction feeds argon gas after finishing again, removes the residual muriate in carbonized titanium powder surface.After cooling to room temperature with the furnace, can obtain to be rich in the carbon material of Nano diamond structure.
Claims (1)
1. preparation method who is rich in the carbon material of Nano diamond structure is characterized in that:
(1) the titanium carbide powder is put into high energy ball mill its particle diameter fragmentation is refined to 0.5 ~ 2.0 μ m; Grinding element during ball milling is the GCr15 steel ball of bearing steel; The mass ratio of steel ball and titanium carbide powder is 4:1 ~ 6:1, and the rotating speed of ball mill is 180 ~ 220 rev/mins, and the ball milling time is 5 ~ 20 hours; For titanium carbide powder during preventing ball milling is reunited, with ethanol as dispersion agent;
(2) the titanium carbide powder behind the above-mentioned ball milling is put into fused quartz tubular type stove, feed argon gas after being evacuated to 0.05 ~ 1Pa, tube furnace is warming up to 900 ~ 1200 ℃; Feed chlorine again; Flow velocity is 20 ~ 30ml/min, and time of chlorinating is 1 ~ 2h, and reaction feeds argon gas after finishing once more; Remove the residual muriates such as titanium tetrachloride in carbonized titanium powder surface, cool to room temperature with the furnace.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012100402782A CN102583316A (en) | 2012-02-22 | 2012-02-22 | Method for preparing carbon materials rich in nano diamond structure |
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| CN2012100402782A CN102583316A (en) | 2012-02-22 | 2012-02-22 | Method for preparing carbon materials rich in nano diamond structure |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017050264A1 (en) * | 2015-09-25 | 2017-03-30 | 郑州华晶金刚石股份有限公司 | Novel shape-controllable nano diamond-ene with layered structure |
| CN108840322A (en) * | 2018-07-10 | 2018-11-20 | 杭州高烯科技有限公司 | A kind of foaming carbon film and preparation method thereof |
| CN110577216A (en) * | 2019-10-10 | 2019-12-17 | 燕山大学 | method for preparing carbon material with nano diamond structure through normal pressure catalysis |
-
2012
- 2012-02-22 CN CN2012100402782A patent/CN102583316A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| RANJAN DASH ET AL.: "Titanium carbide derived nanoporous carbon for energy-related applications", 《CARBON》 * |
| YUFENG ZHAO ET AL.: "Titanium carbide derived nanoporous carbon for supercapacitor applications", 《INTERNATIONAL JOURNAL OF HYDROGEN ENERGY》 * |
| 张瑞军等: "一种新型碳材料_碳化物衍生碳的研究进展", 《燕山大学学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017050264A1 (en) * | 2015-09-25 | 2017-03-30 | 郑州华晶金刚石股份有限公司 | Novel shape-controllable nano diamond-ene with layered structure |
| CN108840322A (en) * | 2018-07-10 | 2018-11-20 | 杭州高烯科技有限公司 | A kind of foaming carbon film and preparation method thereof |
| CN110577216A (en) * | 2019-10-10 | 2019-12-17 | 燕山大学 | method for preparing carbon material with nano diamond structure through normal pressure catalysis |
| CN110577216B (en) * | 2019-10-10 | 2022-07-29 | 燕山大学 | Method for preparing carbon material with nano diamond structure through normal pressure catalysis |
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Application publication date: 20120718 |
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