CN112809012B - Preparation method of nanoscale aluminum powder - Google Patents
Preparation method of nanoscale aluminum powder Download PDFInfo
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- CN112809012B CN112809012B CN202011622891.6A CN202011622891A CN112809012B CN 112809012 B CN112809012 B CN 112809012B CN 202011622891 A CN202011622891 A CN 202011622891A CN 112809012 B CN112809012 B CN 112809012B
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000004880 explosion Methods 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 23
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 17
- 239000003990 capacitor Substances 0.000 claims abstract description 11
- 238000007599 discharging Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005086 pumping Methods 0.000 claims abstract description 10
- 238000007789 sealing Methods 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 36
- 229910052786 argon Inorganic materials 0.000 claims description 18
- 230000001105 regulatory effect Effects 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 abstract description 7
- 238000001816 cooling Methods 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention provides a preparation method of nanoscale aluminum powder, which comprises the following steps: (1) Fixing aluminum wires on upper and lower electrodes of the electric explosion cavity, and sealing the electric explosion cavity; (2) Pumping the electric explosion cavity to a negative pressure vacuum state, and filling inert gas to ensure that the pressure in the cavity is more than or equal to 0.1Mpa; (3) Repeating the treatment method in the step (2) for 2-3 times to ensure that the pressure in the cavity is more than or equal to 0.2Mpa; (4) Starting a power supply to charge a capacitor, adjusting the charging voltage to 20-30 KV, continuously feeding wires by a wire feeding device, and starting discharging; (5) When the voltage is 0KV, inert gas in the electric explosion cavity is discharged, and nano-scale aluminum powder is obtained; (6) Dispersing the obtained nano-scale aluminum powder in absolute ethyl alcohol, and vacuum drying at the temperature of minus 50 ℃ to minus 55 ℃ for 24-48 hours. Obtaining the product. The preparation method has higher cooling efficiency, so that aluminum vapor clusters and clusters generated by electric explosion are rapidly condensed, and the growth time of crystal grains is greatly shortened, thereby forming the nano aluminum powder with smaller and more uniform granularity.
Description
Technical Field
The invention relates to the field of nano metals, in particular to a preparation method of nanoscale aluminum powder.
Background
To date, most of nano aluminum particles produced at home and abroad have an average diameter of 30-300 nm. In recent years, there are two widely used methods for producing nano-aluminum particles. One is a plasma chemical synthesis method established by evaporating microparticles in a high temperature plasma chamber; the other is an electric explosion method of the conductor. In the 1970 s, the high-voltage electric college of the Tomsk institute of technology was researching the electric explosion method and was applied to siberian chemical companies and some foreign institutions.
The electric explosion method is a new method for producing nano powder material based on high-frequency pulse transformation technologyThe method. When the pulse current density on the wire reaches 10 6 ～10 9 A/cm 2 The phenomenon of electric explosion occurs, in which the wire is heated by the thermal effect of the pulsed current, decomposed in a burst-like manner, the metal vapor diffuses in an inert atmosphere, and finally sublimates to form nanoparticles of the corresponding metal. The main advantages of the electric explosion method are as follows: (1) High-efficiency energy conversion, wherein in the electric explosion process, most pulse energy acts on the metal wire, and only a small amount of energy is dissipated in a thermal form; (2) The process parameters can be flexibly regulated and controlled, and the controllable synthesis of the nano powder material is realized; (3) The method can be widely applied to the synthesis of various metal powders, and has certain requirements on the particle size of raw material wires, but not on other characteristics of the wires; (4) the particle size distribution range of the product is relatively narrow; (5) The nano metal powder produced by the electric explosion method has good stability during storage and higher activity during chemical application. But the quenching rate of the gas medium is relatively low, and the average particle size of the nano aluminum particles prepared under the same conditions is large and the particle size is uneven.
At present, a preparation method of nanoscale aluminum powder capable of solving the technical problems is lacking.
Disclosure of Invention
The invention aims to provide a preparation method of nanoscale aluminum powder.
In order to achieve the above object, the present invention provides a method for preparing nano-sized aluminum powder, comprising the steps of:
(1) Fixing aluminum wires on upper and lower electrodes of the electric explosion cavity, and sealing the electric explosion cavity;
(2) Pumping the electric explosion cavity to a negative pressure vacuum state, and filling inert gas to ensure that the pressure in the cavity is more than or equal to 0.1Mpa;
(3) Repeating the treatment method in the step (2) for 2-3 times to ensure that the pressure in the cavity is more than or equal to 0.2Mpa;
(4) Starting a power supply to charge a capacitor, adjusting the charging voltage to 20-30 KV, continuously feeding wires by a wire feeding device, and starting discharging;
(5) When the voltage is 0KV, inert gas in the electric explosion cavity is discharged, and nano-scale aluminum powder is obtained;
(6) Dispersing the obtained nano-scale aluminum powder in absolute ethyl alcohol, and vacuum drying at the temperature of minus 50 ℃ to minus 55 ℃ for 24-48 hours. Obtaining the product.
Preferably, the purity of the aluminum wire is more than or equal to 99.99%.
Preferably, the diameter of the aluminum wire is 0.5-0.8 mm.
Preferably, the inert gas comprises one or more of nitrogen, argon, helium and carbon dioxide.
Preferably, the purity of the inert gas is greater than or equal to 99.99%.
Preferably, the inert gas is argon.
Preferably, in the step (4), the refrigerator cycle is turned on before discharging to make the temperature in the chamber 20 to 25 ℃.
Preferably, the capacitance value of the capacitor is 3 to 4 μF.
In one embodiment, the preparation method comprises the steps of:
(1) Fixing aluminum wires with the purity of more than or equal to 99.99% and the diameter of 0.5mm on the upper electrode and the lower electrode of the electric explosion cavity, and sealing the electric explosion cavity;
(2) Pumping the electric explosion cavity to a negative pressure vacuum state, and filling argon with the purity more than or equal to 99.99% so that the pressure in the cavity is more than or equal to 0.1Mpa;
(3) Repeating the treatment method in the step (2) for 2 times to ensure that the pressure in the cavity is more than or equal to 0.2Mpa;
(4) Starting a power supply to charge a capacitor, regulating the charging voltage to 20KV, continuously feeding wires by a wire feeding device, opening a refrigerator circulation to enable the temperature in a cavity to be 20 ℃, and starting discharge;
(5) When the voltage is 0KV, discharging argon in the electric explosion cavity to obtain nano-scale aluminum powder;
(6) Dispersing the obtained nano-scale aluminum powder in absolute ethyl alcohol, and vacuum drying at-50 ℃ for 24 hours. Obtaining the product.
In one embodiment, the preparation method comprises the steps of:
(1) Fixing aluminum wires with the purity of more than or equal to 99.99% and the diameter of 0.8mm on the upper electrode and the lower electrode of the electric explosion cavity, and sealing the electric explosion cavity;
(2) Pumping the electric explosion cavity to a negative pressure vacuum state, and filling argon with the purity more than or equal to 99.99% so that the pressure in the cavity is more than or equal to 0.1Mpa;
(3) Repeating the treatment method in the step (2) for 3 times to ensure that the pressure in the cavity is more than or equal to 0.2Mpa;
(4) Starting a power supply to charge a capacitor, regulating the charging voltage to 30KV, continuously feeding wires by a wire feeding device, opening a refrigerator circulation to enable the temperature in a cavity to be 25 ℃, and starting discharge;
(5) When the voltage is 0KV, discharging argon in the electric explosion cavity to obtain nano-scale aluminum powder;
(6) Dispersing the obtained nano-scale aluminum powder in absolute ethyl alcohol, and vacuum drying at the temperature of-55 ℃ for 48 hours. Obtaining the product.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method has higher cooling efficiency, so that aluminum vapor clusters and clusters generated by electric explosion are rapidly condensed, and the growth time of crystal grains is greatly shortened, thereby forming the nano aluminum powder with smaller and more uniform granularity.
2. The average granularity of the currently known nano aluminum powder is more than 30nm, and the average granularity of the nano aluminum powder prepared by the method is about 25 nm.
3. The powder Cheng Qiuxing of the invention shows that the oxide film with the thickness of 2-10 nm is inert, and can prolong the storage time of aluminum powder.
Drawings
FIG. 1 is a schematic diagram of the nano-aluminum powder prepared in example 1.
Detailed Description
Example 1
(1) Fixing aluminum wires with the purity of more than or equal to 99.99% and the diameter of 0.5mm on the upper electrode and the lower electrode of the electric explosion cavity, and sealing the electric explosion cavity;
(2) Pumping the electric explosion cavity to a negative pressure vacuum state, and filling argon with the purity more than or equal to 99.99% so that the pressure in the cavity is more than or equal to 0.1Mpa;
(3) Repeating the treatment method in the step (2) for 2 times to ensure that the pressure in the cavity is more than or equal to 0.2Mpa;
(4) Starting a power supply to charge a capacitor, regulating the charging voltage to 20KV, continuously feeding wires by a wire feeding device, opening a refrigerator circulation to enable the temperature in a cavity to be 20 ℃, and starting discharge;
(5) When the voltage is 0KV, discharging argon in the electric explosion cavity to obtain nano-scale aluminum powder;
(6) Dispersing the obtained nano-scale aluminum powder in absolute ethyl alcohol, and vacuum drying at-50 ℃ for 24 hours. Obtaining the product.
Example 2
(1) Fixing aluminum wires with the purity of more than or equal to 99.99% and the diameter of 0.8mm on the upper electrode and the lower electrode of the electric explosion cavity, and sealing the electric explosion cavity;
(2) Pumping the electric explosion cavity to a negative pressure vacuum state, and filling argon with the purity more than or equal to 99.99% so that the pressure in the cavity is more than or equal to 0.1Mpa;
(3) Repeating the treatment method in the step (2) for 3 times to ensure that the pressure in the cavity is more than or equal to 0.2Mpa;
(4) Starting a power supply to charge a capacitor, regulating the charging voltage to 30KV, continuously feeding wires by a wire feeding device, opening a refrigerator circulation to enable the temperature in a cavity to be 25 ℃, and starting discharge;
(5) When the voltage is 0KV, discharging argon in the electric explosion cavity to obtain nano-scale aluminum powder;
(6) Dispersing the obtained nano-scale aluminum powder in absolute ethyl alcohol, and vacuum drying at the temperature of-55 ℃ for 48 hours. Obtaining the product.
Example 3
(1) Fixing aluminum wires with the purity of more than or equal to 99.99% and the diameter of 0.8mm on the upper electrode and the lower electrode of the electric explosion cavity, and sealing the electric explosion cavity;
(2) Pumping the electric explosion cavity to a negative pressure vacuum state, and filling argon with the purity more than or equal to 99.99% so that the pressure in the cavity is more than or equal to 0.2Mpa;
(3) Repeating the treatment method in the step (2) for 3 times to ensure that the pressure in the cavity is more than or equal to 0.4Mpa;
(4) Starting a power supply to charge a capacitor, regulating the charging voltage to 30KV, continuously feeding wires by a wire feeding device, opening a refrigerator circulation to enable the temperature in a cavity to be 20 ℃, and starting discharge;
(5) When the voltage is 0KV, discharging argon in the electric explosion cavity to obtain nano-scale aluminum powder;
(6) Dispersing the obtained nano-scale aluminum powder in absolute ethyl alcohol, and vacuum drying at the temperature of-55 ℃ for 48 hours. Obtaining the product.
Example 4
(1) Fixing aluminum wires with the purity of more than or equal to 99.99% and the diameter of 0.6mm on the upper electrode and the lower electrode of the electric explosion cavity, and sealing the electric explosion cavity;
(2) Pumping the electric explosion cavity to a negative pressure vacuum state, and filling argon with the purity more than or equal to 99.99% so that the pressure in the cavity is more than or equal to 0.2Mpa;
(3) Repeating the treatment method in the step (2) for 2 times to ensure that the pressure in the cavity is more than or equal to 0.4Mpa;
(4) Starting a power supply to charge a capacitor, regulating the charging voltage to 25KV, continuously feeding wires by a wire feeding device, opening a refrigerator circulation to enable the temperature in a cavity to be 20 ℃, and starting discharge;
(5) When the voltage is 0KV, discharging argon in the electric explosion cavity to obtain nano-scale aluminum powder;
(6) Dispersing the obtained nano-scale aluminum powder in absolute ethyl alcohol, and vacuum drying at the temperature of-55 ℃ for 48 hours. Obtaining the product.
Example 5
(1) Fixing aluminum wires with the purity of more than or equal to 99.99% and the diameter of 0.6mm on the upper electrode and the lower electrode of the electric explosion cavity, and sealing the electric explosion cavity;
(2) Pumping the electric explosion cavity to a negative pressure vacuum state, and filling argon with the purity more than or equal to 99.99% so that the pressure in the cavity is more than or equal to 0.2Mpa;
(3) Repeating the treatment method in the step (2) for 2 times to ensure that the pressure in the cavity is more than or equal to 0.4Mpa;
(4) Starting a power supply to charge a capacitor, regulating the charging voltage to 23KV, continuously feeding wires by a wire feeding device, opening a refrigerator circulation to enable the temperature in a cavity to be 20 ℃, and starting discharge;
(5) When the voltage is 0KV, discharging argon in the electric explosion cavity to obtain nano-scale aluminum powder;
(6) Dispersing the obtained nano-scale aluminum powder in absolute ethyl alcohol, and vacuum drying at-50 ℃ for 48 hours. Obtaining the product.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (1)
1. The preparation method of the nano-scale aluminum powder is characterized by comprising the following steps of:
(1) Fixing aluminum wires with the purity of more than or equal to 99.99% and the diameter of 0.5mm on the upper electrode and the lower electrode of the electric explosion cavity, and sealing the electric explosion cavity;
(2) Pumping the electric explosion cavity to a negative pressure vacuum state, and filling argon with the purity more than or equal to 99.99% so that the pressure in the cavity is more than or equal to 0.1Mpa;
(3) Repeating the treatment method in the step (2) for 2 times to ensure that the pressure in the cavity is more than or equal to 0.2Mpa;
(4) Starting a power supply to charge a capacitor, regulating the charging voltage to 20KV, continuously feeding wires by a wire feeding device, opening a refrigerator circulation to enable the temperature in a cavity to be 20 ℃, and starting discharge;
(5) When the voltage is 0KV, discharging argon in the electric explosion cavity to obtain nano-scale aluminum powder;
(6) Dispersing the obtained nano-scale aluminum powder in absolute ethyl alcohol, and vacuum drying at-50 ℃ for 24 hours to obtain the nano-scale aluminum powder.
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2020
- 2020-12-30 CN CN202011622891.6A patent/CN112809012B/en active Active
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