CN218855618U - Equipment for preparing amorphous powder - Google Patents
Equipment for preparing amorphous powder Download PDFInfo
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- CN218855618U CN218855618U CN202221721368.3U CN202221721368U CN218855618U CN 218855618 U CN218855618 U CN 218855618U CN 202221721368 U CN202221721368 U CN 202221721368U CN 218855618 U CN218855618 U CN 218855618U
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Abstract
The utility model discloses an equipment of preparation amorphous powder, include: the device comprises a feeding system, a material crucible, a steam drainage channel, a condensing roller, a powder collecting system and an electron beam heating evaporation system which are sequentially connected; the material crucible, the steam drainage channel and the condensing roller are all arranged in the vacuum chamber, and the electron beam heating evaporation system is positioned above the material crucible. The amorphous powder is formed by heating the material by electron beam evaporation under vacuum conditions and guiding the material vapor to condense on a cooling roller. The utility model discloses an equipment has the higher melting point scope that is suitable for the material, obtains the powder to the quick cooling of vapour under the high vacuum condition simultaneously, overcomes current equipment and method and is suitable for the material and receive the melting point restriction, and the problem that oxygen content is difficult to control.
Description
Technical Field
The utility model relates to a technical field of amorphous metal powder, concretely relates to equipment of preparation amorphous powder.
Background
The amorphous material has the characteristics of high yield strength, high hardness, high specific strength, superelasticity, high wear resistance, high magnetic permeability, high resistivity, radiation resistance, high corrosion resistance, high catalytic activity and the like, and has a very wide application prospect in the fields of electronics, electric power, chemical industry and the like. For example, the amorphous soft magnetic alloy has high saturation magnetic induction, extremely low high-frequency loss and good thermal stability, and is the best choice of soft magnetic materials for high-power switching power supplies; the cobalt-based amorphous narrow band is used for a harmonic anti-theft label; amorphous silicon is commonly used in solar cells and photoconductive devices. Common methods for preparing amorphous materials include melt cooling powder metallurgy, vapor deposition, liquid deposition, sol-gel, and the like, wherein the melt cooling method is a relatively common method for preparing amorphous ingots, ribbons, and powders with low oxygen content.
The melt cooling method is that molten metal is quenched at a speed of more than 105 ℃/s to obtain amorphous metal materials, and the methods of rapid quenching, strip throwing, gas atomization powder making and the like all belong to the preparation methods of the amorphous materials, and the more active metal mainly depends on the methods. CN 2200710065359.7 discloses a method for preparing Fe-based amorphous nanocrystalline powder by gas atomization with argon as a medium, which effectively reduces the oxygen content introduced when inactive metals such as Fe are prepared into powder by gas atomization by adopting high-purity argon, and finally can obtain amorphous Fe-based alloy with the oxygen content not higher than 300ppm (namely, the oxygen content is 0.03wt percent), on one hand, the oxygen content in the high-purity argon is only 1.5ppm, and the argon purity is further improved to reduce the oxygen content of the amorphous material, which means that for active elements such as Ti, zr, B and the like, the amorphous material with low oxygen content is difficult to obtain by adopting the method, and on the other hand, the cost is increased sharply by further improving the argon purity; CN 202111307143.3 discloses a refractory high-entropy amorphous alloy material and a preparation method thereof, which realizes the preparation of an alloy containing refractory metal elements, adopts an arc melting mode under argon atmosphere to prepare an alloy mother ingot, then the mother ingot is crushed, argon is introduced and vacuumized to-0.09 MPaG (namely, the absolute pressure is 0.01 MPa), and liquid alloy is sprayed onto a cooling copper roller under the condition of differential pressure. The method reduces the argon partial pressure when the alloy is in a liquid state, so that the oxygen content of the amorphous material is reduced, but argon still needs to be introduced, and meanwhile, the crushed mother ingot needs to be melted by induction heating, so that the temperature of the material prepared by the method is limited.
For the material with higher melting point and stronger affinity with oxygen, the amorphous powder prepared by the equipment obviously has the defects that the oxygen content is difficult to control and the equipment is difficult to be suitable for the material with high melting point.
Disclosure of Invention
To the deficiencies of the prior art, the utility model provides a device for preparing amorphous powder.
The utility model discloses a realize through following technical scheme.
An apparatus for preparing amorphous powder, comprising: the device comprises a feeding system, a material crucible, a steam drainage channel, a condensing roller, a powder collecting system and an electron beam heating evaporation system which are sequentially connected; the material crucible, the steam drainage channel and the condensing roller are all arranged in the vacuum chamber, and the electron beam heating evaporation system is positioned above the material crucible in an inclined mode.
Further, the feeding system comprises a feeding bin port, a first-stage feeding bin, a vacuum valve, a second-stage feeding bin and a discharging port which are sequentially connected from top to bottom, the first-stage feeding bin is connected with the first vacuum system, the discharging port is provided with a control valve, and the discharging port is connected with a feeding port of the material crucible.
Furthermore, the powder collecting system comprises a material receiving bin, a discharge valve and a discharge pipe which are sequentially connected from top to bottom, the upper end of the material receiving bin is connected with the discharge end of the condensing roller, the bottom end of the discharge pipe is connected with a detachable material receiving barrel, and the discharge pipe is connected with a second vacuum system.
Further, the receiving barrel is connected with the bottom end of the discharging pipe through a flange.
Furthermore, the steam drainage channel is of a horizontal tubular structure, one end of the steam drainage channel is connected with the material crucible, and the other end of the steam drainage channel is connected with the feeding end of the condensing roller.
Furthermore, the condensing roller is a water-cooling condensing roller made of molybdenum or copper.
Furthermore, the material crucible is a water-cooled copper crucible or a quartz crucible, and the horizontal section of the material crucible is square or circular.
Further, the vacuum chamber comprises a hollow rectangular chamber, and the hollow rectangular chamber is connected with a third vacuum system.
The utility model has the advantages of the technical effect, the utility model discloses an equipment has the higher melting point scope that is suitable for the material, cools off fast to steam and obtains the powder simultaneously under high vacuum condition, overcomes current equipment and method and is suitable for the material and receives the melting point restriction, and oxygen content uncontrollable's problem. The utility model adopts the electron beam heating evaporation system as the heat source, which can provide high energy, directly evaporate the raw material for preparing amorphous powder, avoid the pollution caused by excessive contact with the crucible, and is suitable for non-conductive materials compared with the modes of electric arc, induction melting and the like; under the vacuum environment, the oxygen content of the amorphous powder material is effectively reduced; the utility model can realize reasonable air flow distribution and improve the vapor collection efficiency; the condensing roller is used as a condensing and collecting device of material vapor, and highly amorphized nano powder can be obtained.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
FIG. 2 is a schematic diagram of the feed system.
FIG. 3 is a schematic view of the construction of the fluff collection system.
Fig. 4 is a schematic structural diagram of an electron beam heating evaporation system according to the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
The utility model is used for the amorphous powder of preparation can be metal material or non-metallic material, is particularly suitable for having materials such as titanium, zirconium, vanadium, boron or cobalt of higher melting point.
As shown in fig. 1, an apparatus for preparing amorphous powder includes: the device comprises a feeding system 1, a material crucible 2, a steam drainage channel 3, a condensing roller 4, a powder collecting system 5 and an electron beam heating evaporation system 6 which are connected in sequence; the material crucible 2, the steam drainage channel 3 and the condensing roller 4 are all arranged in the vacuum chamber 7, and the electron beam heating evaporation system 6 is positioned above the material crucible 2.
The electron beam heating evaporation system 6 is used for providing a heat source (known equipment), the electron beam heating evaporation system 6 is connected with a heat source inlet arranged at the top of the vacuum chamber 7, and the heat source inlet is positioned obliquely above the material crucible. For example, an electron beam heating evaporation system as shown in fig. 4 is adopted, which includes an electron beam generating electrical control system, a high voltage power supply, an electron beam generating system, an electron beam deflection scanning system, and a scanning deflection electrical control system. The electron beam generation electric control system is connected with the high-voltage power supply and used for controlling the starting and the closing of the high-voltage power supply. The electron beam generating system comprises a filament, a cathode, a focusing electrode, an anode and the like, and is used for emitting electron beams. The electron beam deflection scanning system mainly comprises coils required for deflection scanning, and is used for controlling the deflection direction and the scanning path of the electron beam. The high-voltage power supply is used for providing high voltage required by links such as filament heating, electron beam acceleration and the like. The scanning deflection electric control system provides a deflection parameter signal and a scanning path signal of the electron beam. After the filament is electrified and heated, electrons are released to bombard the cathode to form an electron beam, the electron beam is accelerated to flow through the focusing electrode to be focused under high voltage, then passes through the anode, is deflected by the scanning deflection coil, and is driven into the material in the crucible from the oblique upper part of the material crucible, and the scanning deflection coil determines the scanning pattern to melt and evaporate the material.
The feeding system 1 is shown in fig. 2 and used for adding raw materials into a material crucible 2 and realizing continuous feeding, and the specific structure comprises a feeding bin port 8, a primary feeding bin 9, a vacuum valve 10, a secondary feeding bin 11 and a discharge port 12 which are sequentially connected from top to bottom, wherein the primary feeding bin 9 is connected with a first vacuum system 13, the discharge port 12 is provided with a control valve 14, and the discharge port 12 extends into a vacuum chamber 7 through a connecting hole formed in the wall of the vacuum chamber 7 and is connected with a feeding port of the material crucible 2.
The powder collecting system 5 is shown in fig. 3 and is used for collecting prepared amorphous powder, and the specific structure comprises a material receiving bin 15, a discharge valve 16 and a discharge pipe 17 which are sequentially connected from top to bottom, wherein the upper end of the material receiving bin 15 is connected with the discharge end of the condensing roller 4 through a connecting hole formed in the bottom of the vacuum chamber 7, the bottom end of the discharge pipe 17 is connected with a material receiving barrel 18 through a flange 20, the material receiving barrel 18 can be detached, and the discharge pipe 17 is connected with a second vacuum system 19.
The steam drainage channel 3 is a horizontal hollow tubular structure, one end of the steam drainage channel 3 is connected with the material crucible 2, the other end of the steam drainage channel is connected with the feeding end of the condensing roller 4, and steam evaporated from the crucible is drained to the condensing roller 4 through gas flowing between the vacuum system and the crucible, so that the powder obtaining rate of the steam is improved.
The condensing roller 4 is a commercially available product, and may be a water-cooled condensing roller, which includes a hollow rotatable metal roller, a driving device, and a circulating cooling system, and is usually made of molybdenum or copper.
The material crucible 2 is used for forming a material molten pool to obtain steam, and can be a water-cooled copper crucible or a quartz crucible, and the horizontal section of the material crucible 2 is square or round.
The vacuum chamber 7 structurally comprises a hollow rectangular chamber which is connected with a third vacuum system 21, and the ultimate vacuum degree in the vacuum chamber 7 is not lower than 10 -2 Pa。
The first, second and third vacuum systems are all known devices for obtaining and maintaining vacuum, the main structures of the first and second vacuum systems include components such as a molecular pump, a mechanical pump or a rotary vane pump, and the main structure of the third vacuum system 21 includes a diffusion pump and a slide valve pump.
Example 1
The utility model discloses an equipment for preparing amorphous powder, vacuum chamber 7's ultimate vacuum reaches 5X 10 -3 Pa, the material crucible 2 is made of square water-cooled copperThe crucible adopts an electron beam heating evaporation system as a heat source, the third vacuum system 21 comprises two stages of a diffusion pump and a slide valve pump, the model of the diffusion pump is KT800, the two 2H-150 slide valve pumps are adopted as backing pumps, and a dust collector is arranged at the mouth of the diffusion pump to prevent residual powder from entering the vacuum system. The first vacuum system 13 is used to maintain vacuum in the feed system 1 and the second vacuum system 19 is used to maintain vacuum in the frit collection system.
The preparation process comprises the following steps: raw materials are continuously fed into a material crucible 2 through a feeding system 1, and specifically, the raw materials enter the material crucible 2 through a feeding bin port 8, a first-level feeding bin 9, a vacuum valve 10, a second-level feeding bin 11 and a discharge port 12, an electron beam generating system of an electron beam heating evaporation system, namely an electron gun is connected with a heat source inlet arranged at the top of a vacuum chamber 7, the heat source inlet is positioned above the material crucible 2 in an inclined mode, electron beams are obtained through a high-voltage power supply, and the electron beams are injected into the material crucible 2 through a scanning deflection electric control system, so that the raw materials in the crucible are melted and evaporated, wherein the power of the high-voltage power supply of the electron beams is 400kW. The evaporated steam enters the condensing roller 4 through the steam drainage channel 3, is solidified into amorphous powder, then enters the powder collecting system 5 for collection, and particularly enters the material collecting barrel 18 through the material receiving bin 15, the discharge valve 16 and the discharge pipe 17 to realize collection of the amorphous powder.
Example 2
Titanium powder was prepared using the apparatus described in example 1, with electrolytic titanium crystals as the starting material and a chamber vacuum of 1X 10 -2 Pa, electron beam power 400kW. And carrying out X-ray diffraction and oxygen content analysis on the obtained titanium powder, wherein the X-ray diffraction result shows that the titanium powder is in an amorphous state, and the oxygen content is 500ppm by adopting an inert gas pulse infrared method.
Example 3
The boron powder was prepared using the apparatus described in example 1 with bulk boron as the raw material, 5wt.% oxygen content, 1 × 10 chamber vacuum -2 Pa, electron beam power 450kW. And (3) carrying out X-ray diffraction and oxygen content analysis on the obtained boron powder, wherein the X-ray diffraction result shows that the boron powder is in an amorphous state, and the oxygen content is 1.8 wt% by adopting an inert gas pulse infrared method.
Example 4
The vanadium powder prepared by the equipment in the example 1 is prepared by using lump vanadium as the raw material, the purity is 99.5 percent, and the vacuum degree of a chamber is 1 multiplied by 10 -2 Pa, the power of the electron beam is 450kW. And carrying out X-ray diffraction and oxygen content analysis on the obtained vanadium powder, wherein the X-ray diffraction result shows that the vanadium powder is in an amorphous state, and the oxygen content is 450ppm by adopting an inert gas pulse infrared method.
Example 5
The apparatus described in example 1 was used to prepare cobalt powder from electrolytic cobalt as the starting material with a chamber vacuum of 1X 10 -2 Pa, electron beam power 400kW. And (3) carrying out X-ray diffraction and oxygen content analysis on the obtained cobalt powder, wherein the X-ray diffraction result shows that the cobalt powder is in an amorphous state, and the oxygen content is 0.3wt% by adopting an inert gas pulse infrared method.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other modifications and equivalents may be made by those skilled in the art in light of the teachings of the present disclosure to achieve the same purpose, and should be construed as within the scope of the present disclosure.
Claims (8)
1. An apparatus for preparing amorphous powder, comprising: the device comprises a feeding system, a material crucible, a steam drainage channel, a condensing roller, a powder collecting system and an electron beam heating evaporation system which are sequentially connected; the material crucible, the steam drainage channel and the condensing roller are all arranged in the vacuum chamber, and the electron beam heating evaporation system is positioned above the material crucible in an inclined mode.
2. The apparatus of claim 1, wherein the feeding system comprises a feeding bin port, a primary feeding bin, a vacuum valve, a secondary feeding bin, and a discharge port, which are sequentially connected from top to bottom, the primary feeding bin is connected with the first vacuum system, the discharge port is provided with a control valve, and the discharge port is connected with the feeding port of the material crucible.
3. The apparatus according to claim 1 or 2, wherein the powder collection system comprises a material receiving bin, a discharge valve and a material discharge pipe which are sequentially connected from top to bottom, the upper end of the material receiving bin is connected with the discharge end of the condensing roller, the bottom end of the material discharge pipe is connected with a detachable material receiving barrel, and the material discharge pipe is connected with the second vacuum system.
4. The apparatus of claim 3, wherein the receiving barrel is connected to a bottom end of the discharging pipe through a flange.
5. An apparatus for preparing amorphous powder according to claim 1 or 2, wherein the vapor diversion channel has a horizontal tubular structure, one end of the vapor diversion channel is connected with the material crucible, and the other end is connected with the feeding end of the condensing roller.
6. The apparatus of claim 1 or 2, wherein the condensing roller is a water-cooled condensing roller made of molybdenum or copper.
7. An apparatus for preparing amorphous powder according to claim 1 or 2, wherein the material crucible is a water-cooled copper crucible or a quartz crucible, and the horizontal cross-sectional shape of the material crucible is square or circular.
8. The apparatus of claim 1 or 2, wherein the vacuum chamber comprises a hollow rectangular chamber, and the hollow rectangular chamber is connected with a third vacuum system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221721368.3U CN218855618U (en) | 2022-07-04 | 2022-07-04 | Equipment for preparing amorphous powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221721368.3U CN218855618U (en) | 2022-07-04 | 2022-07-04 | Equipment for preparing amorphous powder |
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| Publication Number | Publication Date |
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| CN218855618U true CN218855618U (en) | 2023-04-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202221721368.3U Active CN218855618U (en) | 2022-07-04 | 2022-07-04 | Equipment for preparing amorphous powder |
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| CN (1) | CN218855618U (en) |
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