CN102950293A - Method for producing nano-aluminum powder - Google Patents
Method for producing nano-aluminum powder Download PDFInfo
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- CN102950293A CN102950293A CN2012103923349A CN201210392334A CN102950293A CN 102950293 A CN102950293 A CN 102950293A CN 2012103923349 A CN2012103923349 A CN 2012103923349A CN 201210392334 A CN201210392334 A CN 201210392334A CN 102950293 A CN102950293 A CN 102950293A
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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, at aerospace field important application is arranged.Change the aluminium powder in the solid propellant propulsion agent prescription into nanometer aluminium powder, can change its combustibility and quick-fried calorific value.The nanometer aluminium powder activity is high, with at once oxidation of contact with air.The mode of production of aluminium powder mainly is the nitrogen atomization method at present, specifically aluminium ingot is fused into aluminium liquid, then uses high pressure nitrogen high speed impact aluminium fluid column, makes aluminium liquid be atomized into fine droplet and is frozen into aluminium powder.The aluminium powder that the method is produced, its particle diameter is thicker, does not specifically wait at the 1-100um ratio respectively, and wherein accounts for the less than 10% of total amount less than 2 microns aluminium powder.Its key depends mainly on the atomization technique of producer, such as the employing high-pressure atomization that has, and the employing high pressure supersonic atomization that has, although latter's particle diameter is thin, average grain diameter is also up to arriving 15um.Except particle diameter slightly, oxidation is also more serious, causes the content of activated aluminum low.In addition, the production method of nanometer aluminium powder mainly is the ion sputtering method, but this method yields poorly the cost height.
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, the content of 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 is put into the crucible of high-temperature metal evaporimeter, after the air-tightness of inspection machine is qualified, whole system is vacuumized, then use the inert gas rinse-system, until be inert atmosphere in the system; As heating source, aluminium is fused into liquid by the plasma transferred arc that between crucible and plasma arcs torch, produces; The power of plasma transferred arc is 50 ~ 150KW;
(2) beginning continuous feed in the 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) be cooled gas cooled and be transported to particle controller of the aluminum vapor that is evaporated, the steam of aluminium is continued cooling in particle controller, become solid-stately, forms nanometer aluminium powder, and 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 behind the gas-solid separator below 100 ℃, depositing in the gas-solid separator and is collected in the nanometer aluminium powder collector, obtains the nano aluminum powder, and gas then recycles after supercooling or is emptying.
The described aluminum feedstock of step of the present invention (1) is granular, fritter shape etc.
The gas of the described generation plasma of 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 the 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 pressure in the crucible, because whole air-flow communicates.
High-temperature metal evaporimeter of the present invention is the high-temperature metal evaporimeter in the patent 201110119245.2, and this evaporation structure is as follows: comprise crucible, plasma transferred arc torch, plasma transferred arc, graphite, power supply and wire be used to the metal liquid after holding metal derby and melting; Be provided with the air inlet pipe that supplied gas enters in the described plasma transferred arc torch; The plasma transferred arc lower end that described plasma transferred arc torch produces and the metal bath surface in the crucible join; Described graphite is located at the bottom of crucible; Consist of electric loop between described plasma transferred arc torch, plasma transferred arc, crucible, graphite, power supply and the wire, the top of described plasma transferred arc is provided with the feed pipe that adds for raw metal.
The production method of nanometer aluminium powder of the present invention, the technological process of this production method specifically describes: the crucible of the rafifinal raw material being put into the high-temperature metal evaporimeter, install plasma producing apparatus, and the air-tightness that checks whole system qualified rear (air tight), system is vacuumized, be filled with inert gas (such as nitrogen, argon gas etc.) system is washed, making in the system is inert environments; Start plasma producing apparatus, the electric current of plasma transferred arc is 100 ~ 1000A, and voltage is 60 ~ 200V, aluminum feedstock is fused into aluminium liquid after, beginning continuous feed in the evaporimeter crucible, and the liquid level stabilizing in the maintenance crucible, aluminum vapor is continual to be evaporated, and the gas that is cooled is taken the high-temperature metal evaporimeter out of, enter particle controller, in particle controller, because the rapid cooling of refrigerating gas is got off the aluminum vapor condensation, form nanometer aluminium powder; Nanometer aluminium powder and gas are through behind the 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 the condenser cooling, and emptying or recycle; In process of production, inlet amount is 0.3 ~ 5.0Kg/h; Reinforced and stable current/voltage by given pace carries out production continually and steadily; The amount of regulating evaporation capacity and adjustments of gas by regulating current/voltage is controlled size and the output of particle diameter.
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 fully, and particle diameter is thin, can satisfy the instructions for use of efficient rocket fuel catalyst fully.
2. nanometer aluminium powder of the present invention is difficult for oxidation, so that the content of its activated aluminum is high, has effectively guaranteed 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.
Description of drawings
Nanometer aluminium powder preparation technology flow chart of the present invention.
The specific embodiment
Describe the present invention in detail below by embodiment, but the present invention not only is confined to following examples.
Embodiment 1,
3Kg fine aluminium piece is put into the crucible of high-temperature metal evaporimeter, install plasma generator, and inspection air-tightness, taken out vacuum, pour inert gas (argon gas) so that whole system is under the inert gas atmosphere, control crucible internal pressure is 0.12MPa, start plasma generator, the power of plasma transferred arc is elevated to 70KW, it is metal liquid that aluminium block melts, observe the metal bath surface height, the adjusting inlet amount is 1.5Kg/h, and heating raw materials is aluminum vapor under the effect of plasma transferred arc, and the aluminum vapor that the is evaporated gas (argon gas) that is cooled cools off and is transported to particle controller, aluminium steam is through the cooling of refrigerating gas, steam-condensation becomes nanometer aluminium powder, and nanometer aluminium powder and gas are through behind the gas-solid separator, and nanometer aluminium powder is deposited on the inwall of gas-solid separator, gas is extracted out separator by air blast, then recycles after the condenser cooling.The aluminium powder average grain diameter of producing is 58nm, and output is 1.2Kg/h.
Embodiment 2,
3Kg fine aluminium piece is put into high-temperature metal evaporimeter crucible, install plasma generator, and inspection air-tightness, taken out vacuum, pour inert gas (argon gas) so that whole system is under the inert gas atmosphere, control crucible internal pressure is 0.15MPa, start plasma generator, the power of plasma transferred arc is elevated to 90KW, it is metal liquid that aluminium block melts, observe the height of metal bath surface, the adjusting inlet amount is 3.0Kg/h, and heating raw materials is aluminum vapor under the effect of plasma transferred arc, be cooled gas cooled and be transported to particle controller aluminium steam through the cooling of refrigerating gas of the aluminum vapor that is evaporated, aluminium steam is through the cooling of refrigerating gas, be condensed into nanometer aluminium powder, nanometer aluminium powder and gas are through behind the gas-solid separator, and nanometer aluminium powder is deposited on the inwall of separator, gas is extracted out separator by air blast, then recycles after the condenser cooling.The aluminium powder particle diameter of producing is 101nm, and output is 2.6Kg/h.
Claims (6)
1. the production method of a nanometer aluminium powder, it is characterized in that: preparation process comprises:
(1) raw material of aluminium is put into the crucible of high-temperature metal evaporimeter, after the air-tightness of inspection machine is qualified, whole system is vacuumized, then use the inert gas rinse-system, until be inert atmosphere in the system; As heating source, aluminium is fused into liquid by the plasma transferred arc that between crucible and plasma arcs torch, produces; The heating power of plasma transferred arc is 50 ~ 150KW;
(2) beginning continuous feed in the crucible of high-temperature metal evaporimeter, feed rate is: 0.3 ~ 5.0Kg/h;
(3) be cooled gas cooled and be transported to particle controller of the aluminum vapor that is evaporated, the steam of aluminium is continued cooling in particle controller, become solid-stately, forms nanometer aluminium powder, and particle diameter is between 10 ~ 1000 nanometers;
(4) nanometer aluminium powder is under the carrying of gas, by being cooled to behind the gas-solid separator below 100 ℃, depositing in the gas-solid separator and is collected in the nanometer aluminium powder collector, obtains the nano aluminum powder, and gas then recycles after supercooling or is emptying.
2. the production method of nanometer aluminium powder according to claim 1, it is characterized in that: the described aluminum feedstock of step (1) is granular or little bulk.
3. the production method of nanometer aluminium powder according to claim 1 is characterized in that: the gas of the described generation plasma of step (1) is one or more mist of argon gas, hydrogen, helium.
4. the production method of nanometer aluminium powder according to claim 3, it is characterized in that: the gas of the described generation plasma of step (1) is the mist of argon gas and hydrogen.
5. the production method of nanometer aluminium powder according to claim 1 is characterized in that: the pressure in the high-temperature metal evaporimeter crucible is 0.04～0.17MPa.
6. the production method of nanometer aluminium powder according to claim 7 is characterized in that: the pressure in the high-temperature metal evaporimeter crucible is 0.1～0.15MPa.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103537703A (en) * | 2013-09-12 | 2014-01-29 | 江苏博迁新材料有限公司 | 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 |
| 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 |
| 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 |
| 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 |
| TWI820578B (en) * | 2021-01-25 | 2023-11-01 | 鐘筆 | Ultrafine powder particle aggregation cooling tube structure and method for forming ulterfine powder particle |
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| US20040065170A1 (en) * | 2002-10-07 | 2004-04-08 | L. W. Wu | Method for producing nano-structured materials |
| 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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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103537703A (en) * | 2013-09-12 | 2014-01-29 | 江苏博迁新材料有限公司 | 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 |
| TWI820578B (en) * | 2021-01-25 | 2023-11-01 | 鐘筆 | Ultrafine powder particle aggregation cooling tube structure and method for forming ulterfine powder particle |
| 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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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. |