CN101804978A - Preparation method of micro nano graphite nodule - Google Patents
Preparation method of micro nano graphite nodule Download PDFInfo
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- CN101804978A CN101804978A CN 201010146902 CN201010146902A CN101804978A CN 101804978 A CN101804978 A CN 101804978A CN 201010146902 CN201010146902 CN 201010146902 CN 201010146902 A CN201010146902 A CN 201010146902A CN 101804978 A CN101804978 A CN 101804978A
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Abstract
The invention belongs to the field of the inorganic non-metallic material, and relates to a preparation method of micro-nano graphite spheres, which adopts natural flake graphite as a source of elemental carbon, and comprises the following steps: heating pure nickel in a high-frequency induction melting furnace to be 1500-1900 DEG C, and placing a graphite flake into the molten nickel; pouring Ni-C alloy into a copper mold and cooling after 15 minutes; placing the Ni-C alloy into a glass tube for remelting, rapidly cooling the Ni-C alloy with a single-roller chilling device, and throwing the Ni-C alloy into a thin strip type object; and corroding the Ni-C alloy with hot concentrated hydrochloric acid in a clean small beaker, and drying obtained products for 30-50 minutes at the temperature of 60-80 DEG C, thereby obtaining black micro-nano graphite spheres. The invention has the advantages of simple process, low cost and high production efficiency. The prepared micro-nano graphite spheres have good stability, the particle sizes are 100nm to 1 mum, and 97 percent of the graphite particles are of a perfect spherical shape.
Description
Technical field
The invention belongs to the ceramic preparing technical field, relate to a kind of preparation method of micro nano graphite nodule.
Background technology
After soccerballene in 1985 was found, various new carbon materials such as carbon nanotube, carbon nanotrees, carbon micron bar, carbon ball etc. be subjected to people and have paid close attention to widely and study.Wherein, graphite pebbles has excellent thermal conducting performance, corrosion resistance, and thermostability and lubricity etc., therefore, it can be used as catalyzer, special rubber accelerator, conduction, wear-resisting, corrosion resistant material etc. are widely used in the various industries.For example, graphite is mainly used to make crucible in metallurgical industry, is used for metal smelting and precious metal and rare metal; In nuclear power, national defense industry, it is one of important structure material of building in nuclear reactor, makes shielding material and reflecting material, and it also can be used as the neutron moderator in the atomic reactor; Aspect lithium ion battery, graphite pebbles has better cycle ability and charge transport ability with respect to other carbon structure especially, so it is the main raw material as battery electrode.
At present, the method for preparing micro nano graphite nodule comprises: chemical Vapor deposition process, nanometer casting, hydrothermal method, thermolysis carbon source method, catalytic reduction method or the like.These method great majority adopt chemical process to prepare the micro-nano carbon ball, and the method that has needs relatively harsher reaction conditions, such as High Temperature High Pressure; The method that has needs expensive equipment and complicated operations, and cost is than higher and output is lower; Method that has such as nanometer casting, the pattern of the graphite pebbles of preparation and size are not easy control, or the like.This has just directly influenced the application of micro nano graphite nodule in scientific research and industry, so this just need be a kind of under the experiment condition of gentleness, can obtain high yield with low cost, and control the preparation method of the granularity of graphite pebbles easily.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of low-cost high yield, technological operation is simple, pollution-free and the manageable micro nano graphite nodule preparation method of granularity.
The present invention realizes in the following manner:
(1) at first according to a certain percentage (C 3-20wt%, Ni 80-97wt%) takes by weighing high-purity natural sheet stone
Ink powder and nickel, and Graphite Powder 99 is pressed into the thin slice that diameter is 3-5cm with omnipotent mechanical test machine;
(2) under the Ar gas shiled, the nickel block for preparing is placed on is heated to 1500-1900 ℃ in the high-frequency induction smelting furnace, then above-mentioned graphite flake is added in the fused nickel, and constantly slowly stir with carbon-point; After 15 minutes, the Ni-C alloy poured in the copper mould cool off;
(3) with the Ni-C alloy in glass tube for remelting, cool off the Ni-C alloy fast and get rid of into the thin ribbon shaped material with single roller chilling device;
(4) collect above-mentioned thin ribbon shaped material, corrode the Ni-C alloy at clean small beaker with hot concentrated hydrochloric acid; After treating to corrode fully, wash atrament 3-5 time respectively with deionized water and alcohol; Then gains were dried 30-50 minute down at 60-80 ℃, promptly get the micro nano graphite nodule of black.
The preparation method of above-mentioned micro nano graphite nodule is characterized in that: the rotating speed of single roller chilling device is 800-1200 rev/min in the step (3).
The micro nano graphite nodule thermostability height of this method preparation, size-grade distribution is at 100nm-1 μ m, and 97% graphite granule presents perfectly spherical.
The present invention has the following advantages: 1, cost is low, the production efficiency height; 2, stable preparation process, simple to operate, can utilize different speed of cooling to control the size of graphite pebbles; 3, pollution-free, do not need to use catalyzer; 4, be suitable for suitability for industrialized production and application.
Embodiment
Provide five most preferred embodiments of the present invention below:
Embodiment 1
(1) at first be ready to raw material by following mass percent: take by weighing the high-purity natural flake graphite in powder of massfraction 3% and 97% nickel, and with omnipotent mechanical test machine with Graphite Powder 99 be pressed into diameter be 3-5cm thin slice;
(2) under the Ar gas shiled, the nickel block for preparing is placed in the high-frequency induction smelting furnace 1500-1900 ℃ of heating, then above-mentioned graphite flake is put into fused nickel, and with carbon-point slowly stirring constantly.After 15 minutes, the Ni-C alloy poured in the copper mould cool off;
(3) with the Ni-C alloy in glass tube for remelting, cool off the Ni-C alloy fast and get rid of into the thin ribbon shaped material with single roller chilling device, rotating speed is 800 rev/mins;
(4) collect above-mentioned strip material, corrode the Ni-C alloy at clean small beaker with hot concentrated hydrochloric acid; After treating to corrode fully, wash atrament 3-5 time respectively with deionized water and alcohol; Then gains were dried 30-50 minute down at 60-80 ℃, promptly get the micro nano graphite nodule of black;
Above-mentioned prepared micro nano graphite nodule thermostability height, size-grade distribution is at 200nm-1 μ m, and 97% graphite granule presents perfectly spherical.
Embodiment 2
(1) at first be ready to raw material by following mass percent: take by weighing the high-purity natural flake graphite in powder of massfraction 5% and 95% nickel, and with omnipotent mechanical test machine with Graphite Powder 99 be pressed into diameter be 3-5cm thin slice;
(2) under the Ar gas shiled, the nickel block for preparing is placed in the high-frequency induction smelting furnace 1500-1900 ℃ of heating, then above-mentioned graphite flake is put into fused nickel, and with carbon-point slowly stirring constantly.After 15 minutes, the Ni-C alloy poured in the copper mould cool off;
(3) with the Ni-C alloy in glass tube for remelting, cool off the Ni-C alloy fast and get rid of into the thin ribbon shaped material with single roller chilling device, rotating speed is 1000 rev/mins;
(4) collect above-mentioned strip material, corrode the Ni-C alloy at clean small beaker with hot concentrated hydrochloric acid; After treating to corrode fully, wash atrament 3-5 time with deionized water and alcohol; Then gains were dried 30-50 minute down at 60-80 ℃, promptly get the micro nano graphite nodule of black;
Above-mentioned prepared micro nano graphite nodule thermostability height, size-grade distribution is at 150nm-1 μ m, and 98% graphite granule presents perfectly spherical.
Embodiment 3
(1) at first be ready to raw material by following mass percent: take by weighing the high-purity natural flake graphite in powder of massfraction 8% and 92% nickel, and with omnipotent mechanical test machine with Graphite Powder 99 be pressed into diameter be 3-5cm thin slice;
(2) under the Ar gas shiled, the nickel block for preparing is placed in the high-frequency induction smelting furnace 1500-1900 ℃ of heating, then above-mentioned graphite flake is put into fused nickel, and with carbon-point slowly stirring constantly.After 15 minutes, the Ni-C alloy poured in the copper mould cool off;
(3) with the Ni-C alloy in glass tube for remelting, cool off the Ni-C alloy fast and get rid of into the thin ribbon shaped material with single roller chilling device, rotating speed is 1200 rev/mins;
(4) collect above-mentioned strip material, corrode the Ni-C alloy at clean small beaker with hot concentrated hydrochloric acid; After treating to corrode fully, wash atrament 3-5 time respectively with deionized water and alcohol; Then gains were dried 30-50 minute down at 60-80 ℃, promptly get the micro nano graphite nodule of black;
Above-mentioned prepared micro nano graphite nodule thermostability height, size-grade distribution is at 100nm-800nm, and 98% graphite granule presents perfectly spherical.
Embodiment 4
(1) at first be ready to raw material by following mass percent: take by weighing the high-purity natural flake graphite in powder of massfraction 15% and 85% nickel, and with omnipotent mechanical test machine with Graphite Powder 99 be pressed into diameter be 3-5cm thin slice;
(2) under the Ar gas shiled, the nickel block for preparing is placed in the high-frequency induction smelting furnace 1500-1900 ℃ of heating, then above-mentioned graphite flake is put into fused nickel, and with carbon-point slowly stirring constantly.After 15 minutes, the Ni-C alloy poured in the copper mould cool off;
(3) with the Ni-C alloy in glass tube for remelting, cool off the Ni-C alloy fast and get rid of into the thin ribbon shaped material with single roller chilling device, rotating speed is 1000 rev/mins;
(4) collect above-mentioned strip material, corrode the Ni-C alloy at clean small beaker with hot concentrated hydrochloric acid; After treating to corrode fully, wash atrament 3-5 time respectively with deionized water and alcohol; Then gains were dried 30-50 minute down at 60-80 ℃, promptly get the micro nano graphite nodule of black;
Above-mentioned prepared micro nano graphite nodule thermostability height, size-grade distribution is at 300nm-1 μ m, and 96% graphite granule presents perfectly spherical.
Embodiment 5
(1) at first be ready to raw material by following mass percent: take by weighing the high-purity natural flake graphite in powder of massfraction 20% and 80% nickel, and with omnipotent mechanical test machine with Graphite Powder 99 be pressed into diameter be 3-5cm thin slice;
(2) under the Ar gas shiled, the nickel block for preparing is placed in the high-frequency induction smelting furnace 1500-1900 ℃ of heating, then above-mentioned graphite flake is put into fused nickel, and with carbon-point slowly stirring constantly.After 15 minutes, the Ni-C alloy poured in the copper mould cool off;
(3) with the Ni-C alloy in glass tube for remelting, cool off the Ni-C alloy fast and get rid of into the thin ribbon shaped material with single roller chilling device, rotating speed is 1200 rev/mins;
(4) collect above-mentioned strip material, corrode the Ni-C alloy at clean small beaker with hot concentrated hydrochloric acid; After treating to corrode fully, wash atrament 3-5 time respectively with deionized water and alcohol; Then gains were dried 30-50 minute down at 60-80 ℃, promptly get the micro nano graphite nodule of black;
Above-mentioned prepared micro nano graphite nodule thermostability height, size-grade distribution is at 500nm-1 μ m, and 97% graphite granule presents perfectly spherical.
Claims (2)
1. the preparation method of a micro nano graphite nodule is characterized in that may further comprise the steps:
(1) at first takes by weighing high-purity natural flake graphite in powder and nickel, and Graphite Powder 99 is pressed into the thin slice that diameter is 3-5cm with omnipotent mechanical test machine in the mass percent ratio of carbon 3-20%, nickel 97-80%;
(2) under the Ar gas shiled, the nickel for preparing is placed in the high-frequency induction smelting furnace 1500-1900 ℃ of heating, then above-mentioned graphite flake is put into fused nickel, and with carbon-point slowly stirring constantly; After 15 minutes, the Ni-C alloy poured in the copper mould cool off;
(3) with the Ni-C alloy in glass tube for remelting, cool off the Ni-C alloy fast and get rid of into the thin ribbon shaped material with single roller chilling device;
(4) collect above-mentioned thin ribbon shaped material, corrode the Ni-C alloy at clean small beaker with hot concentrated hydrochloric acid; After treating to corrode fully, wash atrament 3-5 time respectively with deionized water and alcohol; Then gains were dried 30-50 minute down at 60-80 ℃, promptly get the micro nano graphite nodule of black.
2. according to the preparation method of the described a kind of micro nano graphite nodule of claim 1, it is characterized in that: the rotating speed of single roller chilling device is 800-1200 rev/min in the step (3).
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102211005A (en) * | 2011-04-28 | 2011-10-12 | 山东大学 | Method for preparing magnetic graphite microspheres |
| CN102515144A (en) * | 2011-12-23 | 2012-06-27 | 哈尔滨工业大学 | Method for preparing porous carbon microspheres converted from graphene |
| CN102627275A (en) * | 2012-04-28 | 2012-08-08 | 郑州大学 | Method for preparing graphene by melting carbon-containing alloy to separate out carbon in solidification process |
| CN103924303A (en) * | 2014-04-09 | 2014-07-16 | 山东大学 | Method for preparing boron-enriched micro-nano wire |
| CN104112852A (en) * | 2014-06-14 | 2014-10-22 | 深圳市聚和源科技有限公司 | A preparing method of a lithium ion battery cathode material |
| CN104775147A (en) * | 2015-04-03 | 2015-07-15 | 余柯涵 | Method for preparing high-quality graphite monocrystal |
| CN106282650A (en) * | 2016-09-18 | 2017-01-04 | 山东大学 | A kind of boron-rich micro-nano ball strengthens Cu-base composites and preparation method thereof |
| CN106328987A (en) * | 2016-09-07 | 2017-01-11 | 马鞍山纽盟知识产权管理服务有限公司 | Novel graphite ball preparation method |
| CN107720735A (en) * | 2017-11-23 | 2018-02-23 | 西派克（厦门）科技有限公司 | A kind of preparation method of boron doped graphene |
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| CN101298326A (en) * | 2008-06-30 | 2008-11-05 | 洛阳市冠奇工贸有限责任公司 | Spherical graphitic corpuscule composite carbon material and preparation thereof |
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| CN1051154A (en) * | 1990-11-05 | 1991-05-08 | 鞍山市精制石墨厂 | The method of making refined grahite with dilute alkaline solution |
| US20090068470A1 (en) * | 2007-09-12 | 2009-03-12 | Samsung Electronics Co., Ltd. | Graphene shell and process of preparing the same |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102211005A (en) * | 2011-04-28 | 2011-10-12 | 山东大学 | Method for preparing magnetic graphite microspheres |
| CN102515144A (en) * | 2011-12-23 | 2012-06-27 | 哈尔滨工业大学 | Method for preparing porous carbon microspheres converted from graphene |
| CN102515144B (en) * | 2011-12-23 | 2014-04-02 | 哈尔滨工业大学 | Method for preparing porous carbon microspheres converted from graphene |
| CN102627275A (en) * | 2012-04-28 | 2012-08-08 | 郑州大学 | Method for preparing graphene by melting carbon-containing alloy to separate out carbon in solidification process |
| CN102627275B (en) * | 2012-04-28 | 2015-05-20 | 郑州大学 | Method for preparing graphene by melting carbon-containing alloy to separate out carbon in solidification process |
| CN103924303A (en) * | 2014-04-09 | 2014-07-16 | 山东大学 | Method for preparing boron-enriched micro-nano wire |
| CN103924303B (en) * | 2014-04-09 | 2016-03-30 | 山东大学 | A kind of preparation method of boron-rich micro-nano rice noodles |
| CN104112852A (en) * | 2014-06-14 | 2014-10-22 | 深圳市聚和源科技有限公司 | A preparing method of a lithium ion battery cathode material |
| CN104775147A (en) * | 2015-04-03 | 2015-07-15 | 余柯涵 | Method for preparing high-quality graphite monocrystal |
| CN106328987A (en) * | 2016-09-07 | 2017-01-11 | 马鞍山纽盟知识产权管理服务有限公司 | Novel graphite ball preparation method |
| CN106282650A (en) * | 2016-09-18 | 2017-01-04 | 山东大学 | A kind of boron-rich micro-nano ball strengthens Cu-base composites and preparation method thereof |
| CN107720735A (en) * | 2017-11-23 | 2018-02-23 | 西派克（厦门）科技有限公司 | A kind of preparation method of boron doped graphene |
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| CN101804978B (en) | 2011-09-21 |
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