CN101214959A - Process for preparing nano boron carbide powder - Google Patents
Process for preparing nano boron carbide powder Download PDFInfo
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- CN101214959A CN101214959A CNA2008100490359A CN200810049035A CN101214959A CN 101214959 A CN101214959 A CN 101214959A CN A2008100490359 A CNA2008100490359 A CN A2008100490359A CN 200810049035 A CN200810049035 A CN 200810049035A CN 101214959 A CN101214959 A CN 101214959A
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Abstract
The invention provides a process for preparing nanometer boron carbide powder body. The character that carbon source absorbs microwave energy and transforms the microwave energy into heat is employed, the carbon source and boron source are mixed according to certain proportion as initial reaction mass, under the protection of argon gas or nitrogen, the reaction mass is heated to 1650 DEG C to 1800 DEG C with a method of microwave heating, then the reaction mass undergoes thermal retardation 10-30 minutes and is cooled, and the nanometer boron carbide powder body is obtained, wherein the carbon source absorbs microwave in microwave field and transforms the microwave energy into heat, the carbon source provides heat required by the boron carbide generating reaction in the entire processing technique. The invention employs the method of microwave heating, the reaction mass can be heated in a short time and generate reaction, thereby energy resource is largely saved and the working efficiency is increased. The invention has the advantages of low reaction temperature, high efficiency, energetic saving, low cost and the like.
Description
Technical field
The present invention relates to the norbide production technology, mainly propose a kind of preparation method of nano boron carbide powder.
Background technology
Norbide has characteristics such as high rigidity, high chemical potential, neutron absorb, wear-resisting and semi-conductor electroconductibility, and with acid, alkaline solution Fails To Respond, be widely used in fields such as refractory materials, engineering ceramics, nuclear industry, space flight and aviation.
The preparation method who can be used for boron carbide powder at present mainly contains following two kinds: 1, adopt electric arc furnace, boric acid powder, carbon black and petroleum coke powder were smelted 10～14 hours under 2350 ℃～2500 ℃ temperature, make it to generate block norbide, again it is ground into varigrained powder (CN1421386 patent).2, adopt carbon tube furnace, boric acid and carbon black are reacted under 2000 ℃～3000 ℃ high temperature generate boron carbide powder, synthetic powder median size is 20～40 μ m[Pei Li residences, the technology of preparing of boron carbide material, Foshan pottery, 2007 the 4th phases], can be directly used in abrasive material, but also need a large amount of break process operations as the raw material of sintering boron carbide.
From the above mentioned, existing norbide technology of preparing selects for use boric acid, carbon black and refinery coke as raw material substantially, and this is the reason of higher owing to the industrial goods purity of these raw materials, active good, relative low price.But the prepared norbide that goes out of these technologies all is big block or big crystal grain powder, needs through pulverizing and post-processing steps such as fragmentation could form the fine powder product.Because norbide is a kind of high hardness material, its broken crushing process power consumption is huge, seriously polluted, has extending manufacture cycle again and has improved shortcoming such as cost.
Summary of the invention
Task of the present invention be propose a kind of fast, power consumption less, the preparation method of nano boron carbide powder that cost is low.
Preparation method proposed by the invention is: utilize carbon source to the absorption of microwave energy and convert the characteristic of heat to; carbon source and boron source are mixed by a certain percentage as the initial reaction material; under argon gas or protection of nitrogen gas; adopt microwave heating method that reaction mass is heated to 1650 ℃～1800 ℃; be incubated and cool off after 10～30 minutes; obtain nano boron carbide powder; described carbon source absorbs microwave and the energy transformation of microwave is become heat in microwave field, carbon source provides the required heat of formation reaction of norbide in whole technological process.
Carbon source described in the preparation method of the present invention is one or both the combination in carbon black, the refinery coke, its granularity＜300 orders, purity＞99%; Described boron source is one or both the combination in boric acid, the boron oxide, its granularity＜50 orders, purity＞98%.
The weight percent of carbon source is 25%～35% among the preparation method of the present invention, and the weight percent in boron source is 65%～75%.
Among the preparation method of the present invention, carbon source is not only as the primitive reaction thing, and it can also absorb microwave and the energy transformation of microwave is become heat, as the main thermal source supplier of this technology.Carbon black and refinery coke have the specific inductivity height, characteristics such as microwave absorbing property is good in the temperature section of normal temperature～2000K, it can provide the required heat of formation reaction of norbide in microwave field, simultaneously because microwave heating and traditional heating mode (thermal conduction that the present invention adopts, convection current, radiation) mechanism is different fully, micro-wave energy makes the carbon source self-heating, and equipment and air do not absorb microwave energy, reaction mass can reach Heating temperature at short notice and react (existing technology synthesis temperature is much lower) like this, with traditional electrically heated, far-infrared heating is compared energy-conservation several times, save the energy to a great extent, improved working efficiency.Therefore, norbide preparation method proposed by the invention has advantages such as temperature of reaction is low, energy-efficient, with low cost.
In the reaction process, carbon source can absorb energy rapidly and heat up in microwave field, and its temperature that raises is rapidly decomposed the boron source or fusing, forms the liquid phase boron trioxide.Along with the increase of microwave heating time, carbon source is constantly drawn microwave energy and has been gathered certain heat, and material temperature is heated to 1650 ℃～1800 ℃, and following reaction takes place:
7C+2B2O3＝6CO↑+B4C
The CO (carbon monoxide converter) gas that generates is volatilized away, obtains the solid reaction product norbide at last.More than reaction is thermo-negative reaction, and the heat of its absorption is by carbon source microwave energy to be converted, and carbon source disappeared after reaction was finished, and system no longer includes a large amount of heat supplies, does not promptly have heat to make product norbide crystal grain further grow up.In addition, constantly the volatilization of the CO (carbon monoxide converter) gas that produces makes product structure become loose relatively, has also stoped product norbide crystal grain further to be grown up.Therefore, the norbide crystal grain of the present invention preparation has advantages such as prevented from caking, particle diameter are tiny.
Preparation method of the present invention further specifies: boron source and carbon source are mixed by a certain percentage; pack in the corundum crucible; under argon gas or protection of nitrogen gas atmosphere; adopt microwave heating equipment that this reaction mass is heated to 1650 ℃～1800 ℃; be incubated and adopt recirculated water cooling burner hearth after 10～30 minutes, obtain nano boron carbide powder to room temperature.
The microwave heating equipment of indication is the commercially available prod among the present invention; plant capacity is made as 4～20KW during use; the frequency of microwave is 2.45GHz; the microwave heating equipment of being mentioned in the specific embodiment reaches scientific and technological Industrial Co., Ltd by the Luoyang essence and makes; temp measuring system is an infrared measurement of temperature, and furnace chamber can be realized atmosphere protection.The performance characterization of prepared boron carbide powder comprises: X-ray diffraction (XRD) is measured the thing phase composite; Adopt the grain size of transmission electron microscope (TEM) observation analysis boron carbide powder; Adopt spectroscopic analysis to measure the content of norbide in the product.
Embodiment
Provide embodiments of the invention, but do not constitute any limitation of the invention.
Embodiment 1
Take by weighing 3 gram carbon blacks and 9 gram industrial boric acids, and they are mixed the back in mortar, ground 5 minutes, mixed powder is poured in the corundum crucible, place microwave heating equipment burner hearth center, be incubated with refractory brick around the crucible.Begin under the argon shield to heat up, plant capacity is made as 4KW, heats 15 minutes, and the sample surfaces temperature reaches 1800 ℃, is incubated and cuts off device power supply (DPS) after 10 minutes, and water-cooled is taken out sample to room temperature.Through the XRD check and analysis, the gained result is a norbide, and tem observation is 15-20nm to the grain size of boron carbide powder, and the content that is obtained norbide by the spectroscopic analysis result is not less than 92wt%.
Embodiment 2
Take by weighing 140 gram refinery cokes and 260 gram boron trioxides, and, mixed powder is poured in the corundum crucible, place microwave heating equipment burner hearth center, be incubated with refractory brick around the crucible its ball milling 20 minutes.Begin under the argon shield to heat up, plant capacity is made as 20KW, heats 25 minutes, and the sample surfaces temperature reaches 1750 ℃, is incubated and cuts off device power supply (DPS) after 15 minutes, and water-cooled is taken out sample to room temperature.Through the XRD check and analysis, the gained result is a norbide.Tem observation is 15-20nm to the grain size of boron carbide powder.The content that is obtained norbide by the spectroscopic analysis result is not less than 90wt%.
Embodiment 3
Take by weighing 100 gram carbon blacks and 300 gram industrial boric acids, and, mixed powder is poured in the corundum crucible, place microwave heating equipment burner hearth center, be incubated with refractory brick around the crucible its ball milling 20 minutes.Begin under the nitrogen protection to heat up, plant capacity is made as 10KW, heats 30 minutes, and the sample surfaces temperature reaches 1680 ℃, is incubated and cuts off device power supply (DPS) after 30 minutes, and water-cooled is taken out sample to room temperature.Through the XRD check and analysis, the gained result is a norbide.Tem observation is about 15-20nm to the grain size of boron carbide powder.The content that is obtained norbide by the spectroscopic analysis result is not less than 91wt%.
Embodiment 4
Take by weighing 25 gram carbon blacks and 100g refinery coke as carbon source, take by weighing 75g boric acid and 200g boron trioxide as the boron source, it is mixed and ball milling 20 minutes, mixed powder is poured in the corundum crucible, place microwave heating equipment burner hearth center, be incubated with refractory brick around the crucible.Begin under the nitrogen protection to heat up, plant capacity is made as 15KW, heats 30 minutes, and the sample surfaces temperature reaches 1650 ℃, is incubated and cuts off device power supply (DPS) after 20 minutes, and water-cooled is taken out sample to room temperature.Through the XRD check and analysis, the gained result is a norbide.Tem observation is about 15-20nm to the grain size of boron carbide powder.The content that is obtained norbide by the spectroscopic analysis result is not less than 90wt%.
Claims (4)
1. the preparation method of a nano boron carbide powder; it is characterized in that utilizing carbon source to the absorption of microwave energy and convert the characteristic of heat to; carbon source and boron source are mixed by a certain percentage as the initial reaction material; under argon gas or protection of nitrogen gas; adopt microwave heating method that reaction mass is heated to 1650 ℃～1800 ℃; be incubated and cool off after 10～30 minutes; obtain nano boron carbide powder; described carbon source absorbs microwave and the energy transformation of microwave is become heat in microwave field, carbon source provides the required heat of formation reaction of norbide in whole technological process.
2. the preparation method of a kind of nano boron carbide powder according to claim 1 is characterized in that described carbon source is one or both the combination in carbon black, the refinery coke, its granularity＜300 orders, purity＞99%; Described boron source is one or both the combination in boric acid, the boron oxide, its granularity＜50 orders, purity＞98%.
3. the preparation method of a kind of nano boron carbide powder according to claim 1 and 2, the adding weight percent that it is characterized in that described carbon source is 25%～35%, the adding weight percent in boron source is 65%～75%.
4. the preparation method of a kind of nano boron carbide powder according to claim 1, power is made as 4～20KW when it is characterized in that described microwave heating equipment uses, and the frequency of microwave is 2.45GHz.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102731110A (en) * | 2012-07-03 | 2012-10-17 | 武汉理工大学 | Method for fast preparing boron carbide ceramic powder |
| CN103754875A (en) * | 2013-11-06 | 2014-04-30 | 溧阳市江大技术转移中心有限公司 | Manufacturing method of boron carbide sandblast nozzle |
| CN103803551A (en) * | 2013-11-06 | 2014-05-21 | 溧阳市江大技术转移中心有限公司 | Method for manufacturing abrasive material |
| CN105502400A (en) * | 2015-12-03 | 2016-04-20 | 郑州大学 | Preparation method of B4C whiskers |
| CN106006644A (en) * | 2016-05-19 | 2016-10-12 | 深圳市鑫成炭素科技有限公司 | Preparation method of nano boron carbide powder |
| CN106082228A (en) * | 2016-06-12 | 2016-11-09 | 郑州航空工业管理学院 | A kind of B4the preparation method of C nano sheet and B4c nano sheet |
| CN106882807A (en) * | 2017-01-18 | 2017-06-23 | 沈阳工业大学 | A kind of preparation method of boron carbide powder |
| CN107337210A (en) * | 2017-07-24 | 2017-11-10 | 润鸣新素材(通辽)有限公司 | A kind of boron carbide preparation method |
| CN107758670A (en) * | 2017-12-08 | 2018-03-06 | 中国科学院青海盐湖研究所 | A kind of preparation method of boron carbide superfine powder |
| CN107954718A (en) * | 2017-12-08 | 2018-04-24 | 中国科学院青海盐湖研究所 | A kind of preparation method of boron carbide smelting device and boron carbide |
| CN108675301A (en) * | 2018-08-16 | 2018-10-19 | 景德镇陶瓷大学 | A method of preparing boron carbide using gas-solid method |
| CN113860313A (en) * | 2021-09-29 | 2021-12-31 | 西安交通大学 | Amorphous boron carbide and preparation method and application thereof |
| CN115676834A (en) * | 2022-10-02 | 2023-02-03 | 郑州大学 | Method for preparing boron carbide powder with assistance of microwave molten salt |
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| US11465905B2 (en) * | 2019-10-21 | 2022-10-11 | National Chung-Shan Institute Of Science And Technology | Chemical synthesis method for fabricating boron carbide powders |
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2008
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731110A (en) * | 2012-07-03 | 2012-10-17 | 武汉理工大学 | Method for fast preparing boron carbide ceramic powder |
| CN103754875A (en) * | 2013-11-06 | 2014-04-30 | 溧阳市江大技术转移中心有限公司 | Manufacturing method of boron carbide sandblast nozzle |
| CN103803551A (en) * | 2013-11-06 | 2014-05-21 | 溧阳市江大技术转移中心有限公司 | Method for manufacturing abrasive material |
| CN105502400A (en) * | 2015-12-03 | 2016-04-20 | 郑州大学 | Preparation method of B4C whiskers |
| CN105502400B (en) * | 2015-12-03 | 2017-08-22 | 郑州大学 | A kind of B4The preparation method of C whiskers |
| CN106006644A (en) * | 2016-05-19 | 2016-10-12 | 深圳市鑫成炭素科技有限公司 | Preparation method of nano boron carbide powder |
| CN106082228B (en) * | 2016-06-12 | 2018-03-23 | 郑州航空工业管理学院 | A kind of B4The preparation method and B of C nano piece4C nano piece |
| CN106082228A (en) * | 2016-06-12 | 2016-11-09 | 郑州航空工业管理学院 | A kind of B4the preparation method of C nano sheet and B4c nano sheet |
| CN106882807A (en) * | 2017-01-18 | 2017-06-23 | 沈阳工业大学 | A kind of preparation method of boron carbide powder |
| CN106882807B (en) * | 2017-01-18 | 2019-07-16 | 沈阳工业大学 | A kind of preparation method of boron carbide powder |
| CN107337210A (en) * | 2017-07-24 | 2017-11-10 | 润鸣新素材(通辽)有限公司 | A kind of boron carbide preparation method |
| CN107954718A (en) * | 2017-12-08 | 2018-04-24 | 中国科学院青海盐湖研究所 | A kind of preparation method of boron carbide smelting device and boron carbide |
| CN107758670A (en) * | 2017-12-08 | 2018-03-06 | 中国科学院青海盐湖研究所 | A kind of preparation method of boron carbide superfine powder |
| CN107758670B (en) * | 2017-12-08 | 2020-07-21 | 中国科学院青海盐湖研究所 | Preparation method of boron carbide superfine powder |
| CN107954718B (en) * | 2017-12-08 | 2021-09-14 | 中国科学院青海盐湖研究所 | Boron carbide smelting device and preparation method of boron carbide |
| CN108675301A (en) * | 2018-08-16 | 2018-10-19 | 景德镇陶瓷大学 | A method of preparing boron carbide using gas-solid method |
| CN113860313A (en) * | 2021-09-29 | 2021-12-31 | 西安交通大学 | Amorphous boron carbide and preparation method and application thereof |
| CN113860313B (en) * | 2021-09-29 | 2024-02-06 | 西安交通大学 | Amorphous boron carbide and preparation method and application thereof |
| CN115676834A (en) * | 2022-10-02 | 2023-02-03 | 郑州大学 | Method for preparing boron carbide powder with assistance of microwave molten salt |
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| CN100540469C (en) | 2009-09-16 |
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