CN1314584C - Process for preparing nanometer carbon particles - Google Patents
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- CN1314584C CN1314584C CNB2005100268872A CN200510026887A CN1314584C CN 1314584 C CN1314584 C CN 1314584C CN B2005100268872 A CNB2005100268872 A CN B2005100268872A CN 200510026887 A CN200510026887 A CN 200510026887A CN 1314584 C CN1314584 C CN 1314584C
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Abstract
The present invention relates to a method for preparing nano carbon microparticles, which belongs to the technical field of the preparation of cold cathodes of field emission devices. Carbon nano tubes or carbon nano fibers prepared by a chemical vapor phase deposition method or a vacuum arc method are used as raw materials; the raw materials are firstly processed through high energy mechanical ball milling; the raw materials processed by ball milling are cleaned by ultrasonic, filtered by a filter screen and centrifugally filtered. Consequently, the particle uniformity of nano carbon microparticles as products is enhanced, and the nano carbon microparticles as products can be used for preparing screen printing slurry used for the preparation of high performance field emission cold cathodes. The method has the advantages of simple technology, easy enforcement, low cost, and favorable uniformity of prepared particles as products.
Description
Technical field
The present invention relates to a kind of method for preparing nanometer carbon particles, the product nanometer carbon particles of this method is suitable for being used for preparing the cold cathode of feds, belongs to the cold cathode preparing technical field of feds.
Background technology
Cold cathode will become the key part of flat-panel screens of new generation, transmitter, cold light source and vacuum microelectronic device etc.What just developing at present is to adopt the cold cathode of carbon-base film as electron emitter, the structure of this negative electrode and preparation process are simpler and cost is much lower than traditional awl point type cold cathode, carbon-base film vacuum tightness to the device that adopts this negative electrode when emitting electrons is less demanding, thereby greatly reduces the manufacturing cost of device.The carbon material of nanostructure such as carbon nanotube (carbon nanotube-CNT) and carbon nanofiber (carbon nanofiber-CNF) are the critical materials of making cold cathode in the feds, this type of material not only has high thermostability and chemical stability, also has excellent field emission performance, as very low electron emission threshold field and very high emission, be ideal field emission cold-cathode material.Therefore be considered to the optimum substituent that metal and silicon are bored sharp type field-transmitting cathode, it not only can improve the field emission planar display performance, and is expected to reduce greatly the manufacturing cost of indicating meter.The carbon material of this class nanostructure adopts vacuum arc method or chemical Vapor deposition process preparation usually, and the length distribution scope of prepared carbon nanotube or carbon nanofiber is very wide, between tens nanometers～hundreds of micron.Employing is suitable for preparing the thin-film technique of large area display spare, i.e. silk screen printing or imprint process are the inevitable approach of this type of device productsization, the marketization.Adopt the cold cathode of silk screen printing or imprint process preparation,, have the carbon nanotube of length or carbon nanofiber to give prominence to shortcoming on the cold cathode surface because carbon nanotube or carbon nanofiber itself are different in size.When such cold cathode is worked, under electric field action, long or outstanding carbon nanotube or carbon nanofiber are easy to emitting electrons, these carbon nanotubes or carbon nanofiber can be burnt because of current density is excessive, make the field emission performance instability of cold cathode, field transmitting uniformity also is difficult to be guaranteed.In brief, when adopting the cold cathode of silk screen printing or impression preparation feds, uniform particles to the carbon particulate in the slurry of printing cold cathode has higher requirement, the uniform particles of the carbon particulate in the used slurry of background technology reaches above-mentioned requirements far away, make the field emission performance of cold cathode of preparation such as homogeneity, stability, repeatability etc. all relatively poor, seriously have influence on the performance and the application of feds.
If the carbon nanotube of employing oriented growth or carbon nanofiber are as field emission cold-cathode, as patent (application number 02159948.3, publication number CN1417829A) described, the difficult control of the consistence of carbon nanotube or carbon nanofibers grow length, large area deposition is difficult to realize, and excessive because of axial carbon nanotube or carbon nanofiber density, electron emission time space electric charge restriction effect is obvious, makes the degradation of the feds that adopts this cold cathode.
Summary of the invention
At the problem that exists in the above-mentioned technology, the objective of the invention is to release a kind of method for preparing nanometer carbon particles.The advantage of this method is that this method can prepare evengranular nanometer carbon particles, and such nanometer carbon particles is suitable for being used for preparing the field emission cold-cathode with superior performance.The product nanometer carbon particles of this method can be evengranular Powdered, is particularly suitable for being used for preparing carbon back silk screen printing slurry, again with this slurry coating carbon-base film, as the cold cathode of feds; The product nanometer carbon particles of this method also can be the form that is stored in the silk screen printing slurry, and like this, this silk screen printing slurry is exactly a carbon back silk screen printing slurry, can be directly used in the coating carbon-base film, as the cold cathode of feds.
The technical scheme that the present invention adopts for achieving the above object is, prepare the carbon nanotube, carbon nanofiber of gained or both are raw material by the mixed mixed powder of any mass ratio with vacuum arc method or chemical Vapor deposition process, by high-energy ball milling raw material is ground to form evengranular product, the carbon nanoparticle, high-energy ball milling is Powdered or pulpous state respectively for dry grinding or wet-milling, the product of dry grinding or wet-milling correspondence.
Technical scheme of the present invention now is described in detail in detail.
A kind of method for preparing nanometer carbon particles is characterized in that, the concrete operations step comprises:
The first step raw material is prepared
With the prepared carbon nanotube of vacuum arc method or chemical Vapor deposition process, carbon nanofiber or both by the mixed mixed powder of any mass ratio as raw material;
The second step dry ball milling
Raw material and large and small abrading-ball are put into the mill jar of ball mill, big abrading-ball: little abrading-ball: the mass ratio of raw material is 12～30: 25～50: 1, be respectively at mill jar internal pressure and drum's speed of rotation under the condition of 1 normal atmosphere and 100～800 rev/mins and carry out dry ball milling, time is 0.5～4 hour, naturally after being cooled to room temperature, will take out through the raw material that dry ball milling is handled;
The 3rd step cleaned, filters, volatilizees
To be blended into filtrate through raw material and the volatile organic solvent after the second step dry ball milling is handled, the mass ratio of the former with the latter is 1: 8～24, ultrasonic cleaning 2～6 minutes, gauze filters, the macrobead in the elimination filtrate, volatilization organic solvent, get product, nanometer carbon particles.
Technical scheme of the present invention is further characterized in that, between " macrobead in the elimination filtrate " and " volatilization organic solvent " in the 3rd step, inserts the operation of filtrate being carried out centrifuging, and the time is 1～3 minute.
The nanometer carbon particles of above method preparation, uniform particles is good, is suitable for being used for preparing the silk screen printing slurry.Can prepare homogeneity, stability, repeated superior cold cathode with such slurry.
A kind of method for preparing nanometer carbon particles is characterized in that, the concrete operations step comprises:
The first step raw material is prepared
With the prepared carbon nanotube of vacuum arc method or chemical Vapor deposition process, carbon nanofiber or both by the mixed mixed powder of any mass ratio as raw material;
The second step wet ball grinding
Raw material, silk screen printing slurry and large and small abrading-ball are put into the mill jar of ball mill, big abrading-ball: little abrading-ball: the mass ratio of raw material is 12～30: 25～50: 1, the mass ratio of raw material and silk screen printing slurry is 1: 5～10, be respectively at mill jar internal pressure and drum's speed of rotation under the condition of 1 normal atmosphere and 100～800 rev/mins and carry out wet ball grinding, time is 0.5～4 hour, naturally after being cooled to room temperature, the raw material that will handle through wet ball grinding and the mixed slurry of silk screen printing slurry take out;
The 3rd step cleaned, filters
Will be through the mixed slurry after second step, wet ball grinding was handled through ultrasonic cleaning, the time is 2～6 minutes, warp thread net filtration again, the macrobead in the elimination mixed slurry, product, nanometer carbon particles, product is stored in the mixed slurry.
Technical scheme of the present invention is further characterized in that, between " macrobead in the elimination mixed slurry " and " getting product " in the 3rd step, inserts the operation of mixed slurry being carried out centrifuging, and the time of centrifuging is 10～20 minutes.
The nanometer carbon particles of above method preparation is stored in the mixed slurry, and uniform particles is good, and such mixed slurry is exactly a carbon back silk screen printing slurry, can directly be used for preparing homogeneity, stability, repeated superior cold cathode.
Compare with background technology, the present invention has following advantage:
1, technology is simple, and is easy to implement, and preparation cost is low.
2, with the product of method preparation of the present invention, have good field transmitting uniformity and stability, and good repetitiveness.
Embodiment
Now describe technical scheme of the present invention in detail by embodiment.All embodiment operate according to above-mentioned preparation method's operation steps fully.
Embodiment 1 dry ball milling prepares one of nanometer carbon particles
The concrete operations step comprises:
The first step raw material is prepared
With the prepared carbon nanotube of vacuum arc method or chemical Vapor deposition process, carbon nanofiber or both by the mixed mixed powder of any mass ratio as raw material, the quality of raw material is 2g;
The second step dry ball milling
Raw material and large and small abrading-ball are put into the mill jar of ball mill, ball mill is a planetary ball mill, the mill jar is a cylinder of steel, abrading-ball is a steel ball, the quality of big steel ball and little steel ball is respectively 4g and 2g, the quantity of big steel ball and little steel ball is respectively 13 and 45, big abrading-ball: little abrading-ball: the mass ratio of raw material is 26: 45: 1, be respectively at mill jar internal pressure and drum's speed of rotation under the condition of 1 normal atmosphere and 200 rev/mins and carry out dry ball milling, time is 2 hours, naturally after being cooled to room temperature, will take out through the raw material that dry ball milling is handled;
The 3rd step cleaned, filters, volatilizees
To be blended into filtrate through raw material and the volatile organic solvent after the second step dry ball milling is handled, volatile organic solvent is an acetone, and the quality of acetone is 20g, ultrasonic cleaning 5 minutes, gauze filters, the macrobead in the elimination filtrate, volatilization acetone, get product, nanometer carbon particles is Powdered.
Embodiment 2 dry ball millings prepare two of nanometer carbon particles
Except for the following differences, remaining operation steps is identical with embodiment 1 all: between " macrobead in the elimination filtrate " and " volatilization acetone " in the 3rd step of embodiment 1, the operation of centrifuging is carried out in insertion to filtrate: the filtrate that filtration obtains is put into whizzer, centrifuging 2 minutes.
More than the nanometer carbon particles uniform particles of two embodiment preparation, be Powdered, be particularly suitable for being used for preparing carbon back silk screen printing slurry, again with this slurry coating carbon-base film, preparation homogeneity, stability, repeated superior cold cathode.
Embodiment 3 wet ball grindings prepare one of nanometer carbon particles
The concrete operations step comprises:
The first step raw material is prepared
Is raw material with vacuum arc method or prepared carbon nanotube and the carbon nanofiber of chemical Vapor deposition process by the mixed mixed powder of any mass ratio, and the quality of raw material is 3g;
The second step wet ball grinding
With raw material, the silk screen printing slurry is with big, little abrading-ball is put into the mill jar of ball mill, ball mill is a planetary ball mill, the mill jar is the agate jar, abrading-ball is big, little agate bead, the quality of big agate bead and little agate bead is respectively 4g and 2g, the quantity of big agate bead and little agate bead is respectively 12 and 45, big abrading-ball: little abrading-ball: the mass ratio of raw material is 16: 30: 1, the silk screen printing slurry is 18g, the mass ratio of raw material and silk screen printing slurry is 1: 6, be respectively at mill jar internal pressure and drum's speed of rotation under the condition of 1 normal atmosphere and 600 rev/mins and carry out wet ball grinding, time is 2.5 hours, naturally after being cooled to room temperature, the raw material that will handle through wet ball grinding and the mixed slurry of silk screen printing slurry take out;
The 3rd step cleaned, filters
Will be through the mixed slurry after second step, wet ball grinding was handled through ultrasonic cleaning, the time is 3 minutes, warp thread net filtration again, the macrobead in the elimination mixed slurry, product, nanometer carbon particles, product is stored in the mixed slurry.
Embodiment 4 wet ball grindings prepare two of nanometer carbon particles
Except for the following differences, remaining operation steps is identical with embodiment 3 all: between " macrobead in the elimination mixed slurry " in the 3rd step of embodiment 3 and " must product ", insertion is carried out the operation of centrifuging to mixed slurry, and the time of centrifuging is 15 minutes.
More than the nanometer carbon particles of two embodiment preparation, uniform particles is stored in the mixed slurry, this slurry is exactly a carbon back silk screen printing slurry, can be directly used in the coating carbon-base film, preparation homogeneity, stability, the cold cathode that repeatability is superior.
Claims (4)
1, a kind of method for preparing nanometer carbon particles is characterized in that, the concrete operations step comprises:
The first step raw material is prepared
With the prepared carbon nanotube of vacuum arc method or chemical Vapor deposition process, carbon nanofiber or both by the mixed mixed powder of any mass ratio as raw material;
The second step dry ball milling
Raw material and large and small abrading-ball are put into the mill jar of ball mill, big abrading-ball: little abrading-ball: the mass ratio of raw material is 12～30: 25～50: 1, be respectively at mill jar internal pressure and drum's speed of rotation under the condition of 1 normal atmosphere and 100～800 rev/mins and carry out dry ball milling, time is 0.5～4 hour, naturally after being cooled to room temperature, will take out through the raw material that dry ball milling is handled;
The 3rd step cleaned, filters, volatilizees
To be blended into filtrate through raw material and the volatile organic solvent after the second step dry ball milling is handled, the mass ratio of the former with the latter is 1: 8～24, ultrasonic cleaning 2～6 minutes, gauze filters, the macrobead in the elimination filtrate, volatilization organic solvent, get product, nanometer carbon particles.
2, the method for preparing nanometer carbon particles according to claim 1 is characterized in that, between " macrobead in the elimination filtrate " and " volatilization organic solvent " in the 3rd step, inserts the operation of filtrate being carried out centrifuging, and the time is 1～3 minute.
3, a kind of method for preparing nanometer carbon particles is characterized in that, the concrete operations step comprises:
The first step raw material is prepared
With the prepared carbon nanotube of vacuum arc method or chemical Vapor deposition process, carbon nanofiber or both by the mixed mixed powder of any mass ratio as raw material;
The second step wet ball grinding
Raw material, silk screen printing slurry and large and small abrading-ball are put into the mill jar of ball mill, big abrading-ball: little abrading-ball: the mass ratio of raw material is 12～30: 25～50: 1, the mass ratio of raw material and silk screen printing slurry is 1: 5～10, be respectively at mill jar internal pressure and drum's speed of rotation under the condition of 1 normal atmosphere and 100～800 rev/mins and carry out wet ball grinding, time is 0.5～4 hour, naturally after being cooled to room temperature, the raw material that will handle through wet ball grinding and the mixed slurry of silk screen printing slurry take out;
The 3rd step cleaned, filters
Will be through the mixed slurry after second step, wet ball grinding was handled through ultrasonic cleaning, the time is 2～6 minutes, warp thread net filtration again, the macrobead in the elimination mixed slurry, product, nanometer carbon particles, product is stored in the mixed slurry.
4, the method for nanometer carbon particles according to claim 3, it is characterized in that, between " macrobead in the elimination mixed slurry " and " getting product " in the 3rd step, insert the operation of mixed slurry being carried out centrifuging, the time of centrifuging is 10～20 minutes.
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| CNB2005100268872A CN1314584C (en) | 2005-06-17 | 2005-06-17 | Process for preparing nanometer carbon particles |
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| CNB2005100268872A CN1314584C (en) | 2005-06-17 | 2005-06-17 | Process for preparing nanometer carbon particles |
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| CN1314584C true CN1314584C (en) | 2007-05-09 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP5062593B2 (en) * | 2007-12-03 | 2012-10-31 | 独立行政法人産業技術総合研究所 | Carbon fine particles using lignin as raw material and method for producing the same |
| CN101250059B (en) * | 2008-01-25 | 2011-05-04 | 上海纳晶科技有限公司 | Method for preparing light highly-conductive hot carbon nano composite material |
| CN103203265B (en) * | 2012-01-13 | 2015-09-30 | 谢小飞 | A kind of ultrasonic wave high-energy-density ball mill for biological cell broken wall |
| CN103896249B (en) * | 2014-03-25 | 2016-09-07 | 深圳市纳米港有限公司 | Spherical Carbon nanotube group and its production and use |
| CN103922303B (en) * | 2014-03-25 | 2016-06-08 | 深圳市纳米港有限公司 | Spherical Carbon nanotube coacervate and its production and use |
| CN104988451B (en) * | 2015-07-17 | 2018-03-16 | 中南大学 | A kind of preparation method of ultrafine tungsten carbide base ball shaped thermal spray coating powder |
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| CN1374250A (en) * | 2002-04-19 | 2002-10-16 | 清华大学 | Method of utilizing external force to crush, wash and purify slender carbon nanotube |
| US20050008560A1 (en) * | 2003-05-20 | 2005-01-13 | Futaba Corporation | Ultra-dispersed nanocarbon and method for preparing the same |
| CN1613754A (en) * | 2003-11-07 | 2005-05-11 | 中国科学院金属研究所 | Preparation of high-specific surface area nanometer carbon tube |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1374250A (en) * | 2002-04-19 | 2002-10-16 | 清华大学 | Method of utilizing external force to crush, wash and purify slender carbon nanotube |
| US20050008560A1 (en) * | 2003-05-20 | 2005-01-13 | Futaba Corporation | Ultra-dispersed nanocarbon and method for preparing the same |
| CN1613754A (en) * | 2003-11-07 | 2005-05-11 | 中国科学院金属研究所 | Preparation of high-specific surface area nanometer carbon tube |
Non-Patent Citations (1)
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| 碳纳米管的球磨处理及其对储氢性能的影响 刘芙等，太阳能学报，第24卷第1期 2003 * |
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