CN102950293B - Method for producing nano-aluminum powder - Google Patents
Method for producing nano-aluminum powder Download PDFInfo
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- CN102950293B CN102950293B CN201210392334.9A CN201210392334A CN102950293B CN 102950293 B CN102950293 B CN 102950293B CN 201210392334 A CN201210392334 A CN 201210392334A CN 102950293 B CN102950293 B CN 102950293B
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Abstract
The invention discloses a method for producing nano-aluminum powder, and the method comprises the following steps of: putting aluminum in a crucible of a high-temperature metal evaporator, and melting the aluminum into liquid by taking a plasma transferred arc as a heating source, wherein the heating power of the plasma transferred arc is 50-150KW; starting to continuously feed into the crucible of the high-temperature metal evaporator, wherein the feed rate is 0.3-5.0Kg/h; cooling the evaporated aluminum vapor by using cooling gas, outputting the cooled aluminum vapor to a particle controller, continuing cooling the aluminum vapor in the particle controller, turning the vapor into a solid state and forming the nano-aluminum powder with the particle diameter of 10-1000 nanometers; and cooling the nano-aluminum powder to below 100 DEG C via a gas-solid separator under the carry of gas, depositing cooled nano-aluminum powder in the gas-solid separator and collecting the nano-aluminum powder into a nano-aluminum powder collector so as to obtain the nano-aluminum powder, wherein the gas is recycled or vent after being cooled. The method disclosed by the invention has the advantages of fine particle diameter, slight oxidation, high content of active aluminum and high yield.
Description
Technical field
The present invention relates to technical field of nano material, be specifically related to a kind of production method of nanometer aluminium powder.
Background technology
Nanometer aluminium powder is a kind of Efficient rocket fuel catalyst, has important application at aerospace field.Change the aluminium powder in solid propellant propulsion agent prescription into nanometer aluminium powder, its combustibility and quick-fried calorific value can be changed.Nanometer aluminium powder activity is high, contacts at once be oxidized with air.The mode of production mainly nitrogen atomization method of current aluminium powder, is specifically fused into aluminium liquid by aluminium ingot, then uses high pressure nitrogen high speed impact aluminium fluid column, makes aluminium liquid be atomized into fine droplet and be frozen into aluminium powder.The aluminium powder that the method is produced, its particle diameter is comparatively thick, specifically respectively between 1-100um ratio not etc., and the aluminium powder being wherein less than 2 microns account for total amount less than 10%.Its key depends mainly on the atomization technique of producer, than if any employing high-pressure atomization, some employing high pressure supersonic atomizations, although the latter's particle diameter is thin, average grain diameter is also up to 15um.Except particle diameter slightly except, oxidation is also comparatively serious, causes the content of activated aluminum low.In addition, the production method mainly ion sputtering process of nanometer aluminium powder, but this method yields poorly, and cost is high.
Summary of the invention
The present invention is directed to the above-mentioned deficiency of prior art, provide that a kind of particle diameter is thin, oxidation is light, content that is activated aluminum is high, and the production method of the high nanometer aluminium powder of output.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of production method of nanometer aluminium powder.Preparation process comprises:
(1) raw material of aluminium are put into the crucible of high-temperature metal evaporimeter, after the air-tightness of inspection machine is qualified, whole system is vacuumized, then uses inert gas rinse-system, until be inert atmosphere in system; By the plasma transferred arc that produces between crucible and plasma arcs torch as heating source, aluminium is fused into liquid; The power of plasma transferred arc is 50 ~ 150KW;
(2) start to continuous feed in high-temperature metal evaporimeter crucible, feed rate is: 0.3 ~ 5.0Kg/h; Under the effect of plasma transferred arc, aluminium liquid becomes aluminium steam;
(3) aluminum vapor the be evaporated gas that is cooled cools and is transported to particle controller, and the steam of aluminium is by continuation cooling in particle controller, and become solid-state, form nanometer aluminium powder, particle diameter is between 10 ~ 1000 nanometers (0.01 ~ 1 micron);
(4) nanometer aluminium powder is under the carrying of gas, by being cooled to less than 100 DEG C after gas-solid separator, depositing in gas-solid separator and being collected in nanometer aluminium powder collector, obtaining nano aluminum powder, and gas is then through the use or emptying of supercooling Posterior circle.
Aluminum feedstock described in step of the present invention (1) is granular, little bulk etc.
The gas of the generation plasma described in step of the present invention (1) is one or more mist of argon gas, hydrogen, helium, is preferably: the mist of argon gas and hydrogen.
Pressure in high-temperature metal evaporimeter crucible of the present invention is 0.04 ~ 0.17MPa, is preferably 0.1 ~ 0.15MPa.
The pressure of the whole preparation system of the present invention is the same with the pressure in crucible, because whole air-flow communicates.
High-temperature metal evaporimeter of the present invention is the high-temperature metal evaporimeter in patent 201110119245.2, and this evaporation structure is as follows: comprise the crucible for holding metal derby and the metal liquid after melting, plasma transferred arc torch, plasma transferred arc, graphite, power supply and wire; The air inlet pipe that supplied gas enters is provided with in described plasma transferred arc torch; The plasma transferred arc lower end that described plasma transferred arc torch produces connects with the metal bath surface in crucible; Described graphite is located at the bottom of crucible; Described plasma transferred arc torch, plasma transferred arc, crucible, graphite, form electric loop between power supply and wire, the top of described plasma transferred arc is provided with the feed pipe added for raw metal.
The production method of nanometer aluminium powder of the present invention, the technological process of this production method specifically describes and is: crucible rafifinal raw material being put into high-temperature metal evaporimeter, install plasma producing apparatus, and check the air-tightness of whole system qualified rear (air tight), system is vacuumized, be filled with inert gas (as nitrogen, argon gas etc.) to rinse system, make to be inert environments in system; Start plasma producing apparatus, the electric current of plasma transferred arc is 100 ~ 1000A, and voltage is 60 ~ 200V, after aluminum feedstock being fused into aluminium liquid, start to continuous feed in evaporimeter crucible, and keeping the liquid level stabilizing in crucible, aluminum vapor is continual to be evaporated, and cooled gas takes high-temperature metal evaporimeter out of, enter particle controller, due to the quick refrigeration of refrigerating gas in particle controller, aluminum vapor condensation is got off, form nanometer aluminium powder; Nanometer aluminium powder and gas are after gas-solid separator, and nanometer aluminium powder is deposited on the inwall of separator, and gas is extracted out separator by air blast, then after condenser cooling, and emptying or recycle; In process of production, inlet amount is 0.3 ~ 5.0Kg/h; By the reinforced and stable Current Voltage of given pace, production is carried out continually and steadily; The amount of evaporation capacity and adjustments of gas is regulated to control size and the output of particle diameter by regulating Current Voltage.
Advantage of the present invention and beneficial effect:
1. nanometer aluminium powder of the present invention, its average grain diameter is distributed in 0.01 ~ 1 micron completely, and particle diameter is thin, can meet the instructions for use of Efficient rocket fuel catalyst completely.
2. nanometer aluminium powder of the present invention, not oxidizable, make the content of its activated aluminum high, effectively ensure that the result of use of nanometer aluminium powder.
3. the preparation method of nanometer aluminium powder of the present invention is simple, and technique is easy to control, and output is high, and cost is low.
Accompanying drawing explanation
Nanometer aluminium powder preparation technology flow chart of the present invention.
Detailed description of the invention
Describe the present invention in detail below by embodiment, but the present invention is not only confined to following examples.
Embodiment 1,
3Kg fine aluminium block is put into the crucible of high-temperature metal evaporimeter, install plasma generator, and check air-tightness, take out vacuum, pour under inert gas (argon gas) makes whole system be in inert gas atmosphere, controlling pressure in crucible is 0.12MPa, start plasma generator, the power of plasma transferred arc is elevated to 70KW, aluminium block melts as metal liquid, observe metal bath surface height, adjustment inlet amount is 1.5Kg/h, under the effect of plasma transferred arc, heating raw materials is aluminum vapor, the aluminum vapor the be evaporated gas (argon gas) that is cooled cools and is transported to particle controller, aluminium steam is through the cooling of refrigerating gas, steam-condensation becomes nanometer aluminium powder, nanometer aluminium powder and gas are after gas-solid separator, nanometer aluminium powder is deposited on the inwall of gas-solid separator, gas is extracted out separator by air blast, then use through condenser cooling Posterior circle.The aluminium powder average grain diameter of producing is 58nm, and output is 1.2Kg/h.
Embodiment 2,
3Kg fine aluminium block is put into high-temperature metal evaporimeter crucible, install plasma generator, and check air-tightness, take out vacuum, pour under inert gas (argon gas) makes whole system be in inert gas atmosphere, controlling pressure in crucible is 0.15MPa, start plasma generator, the power of plasma transferred arc is elevated to 90KW, aluminium block melts as metal liquid, observe the height of metal bath surface, adjustment inlet amount is 3.0Kg/h, under the effect of plasma transferred arc, heating raw materials is aluminum vapor, the aluminum vapor the be evaporated gas that is cooled cools and is transported to the cooling of particle controller aluminium steam through refrigerating gas, aluminium steam is through the cooling of refrigerating gas, be condensed into nanometer aluminium powder, nanometer aluminium powder and gas are after gas-solid separator, nanometer aluminium powder is deposited on the inwall of separator, gas is extracted out separator by air blast, then use through condenser cooling Posterior circle.The aluminium powder particle diameter produced is 101nm, and output is 2.6Kg/h.
Claims (1)
1. a production method for nanometer aluminium powder, is characterized in that: preparation process comprises:
(1) raw material of aluminium are put into the crucible of high-temperature metal evaporimeter, after the air-tightness of inspection machine is qualified, whole system is vacuumized, then uses inert gas rinse-system, until be inert atmosphere in system; By the plasma transferred arc that produces between crucible and plasma arcs torch as heating source, aluminium is fused into liquid; The heating power of plasma transferred arc is 50 ~ 150KW;
(2) start to continuous feed in the crucible of high-temperature metal evaporimeter, feed rate is: 0.3 ~ 5.0Kg/h;
(3) aluminum vapor the be evaporated gas that is cooled cools and is transported to particle controller, and the steam of aluminium is by continuation cooling in particle controller, and become solid-state, form nanometer aluminium powder, particle diameter is between 10 ~ 1000 nanometers;
(4) nanometer aluminium powder is under the carrying of gas, by being cooled to less than 100 DEG C after gas-solid separator, depositing in gas-solid separator and being collected in nanometer aluminium powder collector, obtaining nano aluminum powder, and gas is then through the use or emptying of supercooling Posterior circle;
Aluminum feedstock described in step (1) is granular or little bulk; The gas of the generation plasma described in step (1) is the mist of argon gas and hydrogen;
Pressure in high-temperature metal evaporimeter crucible is 0.1 ~ 0.15MPa.
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| CN103537703B (en) * | 2013-09-12 | 2017-04-12 | 江苏博迁新材料股份有限公司 | Method for internal-reverse-flow type rubbish removal |
| CN104368821A (en) * | 2014-12-11 | 2015-02-25 | 成都明日星辰科技有限公司 | Silver palladium alloy composite powder preparation method |
| WO2020034090A1 (en) * | 2018-08-14 | 2020-02-20 | 深圳市百柔新材料技术有限公司 | Apparatus and method for preparing nanomaterial |
| CN109365828A (en) * | 2018-12-25 | 2019-02-22 | 江苏科创金属新材料有限公司 | A kind of ultra-fine powder producing method of flake zinc aluminium alloy |
| WO2022156217A1 (en) * | 2021-01-25 | 2022-07-28 | 钟笔 | Ultrafine powder particle aggregation cooling tube type structure and ultrafine powder particle forming method |
| CN113201251A (en) * | 2021-05-12 | 2021-08-03 | 深圳市凌普鑫科技有限公司 | Water-based photo-curing type nano aluminum powder ink and processing method thereof |
| CN114260458A (en) * | 2021-12-28 | 2022-04-01 | 西安交通大学 | Device and method for preparing superfine high-purity spherical magnesium powder |
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| US6379419B1 (en) * | 1998-08-18 | 2002-04-30 | Noranda Inc. | Method and transferred arc plasma system for production of fine and ultrafine powders |
| CN1422195A (en) * | 2000-02-10 | 2003-06-04 | 特乔尼科斯有限公司 | Plasma arc reactor for the production of fine powders |
| CN102211197A (en) * | 2011-05-06 | 2011-10-12 | 宁波广博纳米新材料股份有限公司 | Metal evaporating device and method for preparing ultrafine metal powder by using same |
| CN102615289A (en) * | 2011-01-28 | 2012-08-01 | 杭州华纳塔器科技有限公司 | Evaporation-condensation method for preparing superfine metal powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20040065170A1 (en) * | 2002-10-07 | 2004-04-08 | L. W. Wu | Method for producing nano-structured materials |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6379419B1 (en) * | 1998-08-18 | 2002-04-30 | Noranda Inc. | Method and transferred arc plasma system for production of fine and ultrafine powders |
| CN1422195A (en) * | 2000-02-10 | 2003-06-04 | 特乔尼科斯有限公司 | Plasma arc reactor for the production of fine powders |
| CN102615289A (en) * | 2011-01-28 | 2012-08-01 | 杭州华纳塔器科技有限公司 | Evaporation-condensation method for preparing superfine metal powder |
| CN102211197A (en) * | 2011-05-06 | 2011-10-12 | 宁波广博纳米新材料股份有限公司 | Metal evaporating device and method for preparing ultrafine metal powder by using same |
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Effective date of registration: 20161028 Address after: 223801 Suqian province high tech Development Zone, Jiangshan Road, No. 23, No. Patentee after: Jiangsu Bo move new materials Limited by Share Ltd Address before: Yinzhou District Shiqi car 315153 Zhejiang city in Ningbo province where extensive science and Technology Park Patentee before: Ningbo Guangbo New Nanomaterials Stock Co.,Ltd. |