CN110947977A - Production method of submicron AgSnTe alloy powder - Google Patents
Production method of submicron AgSnTe alloy powder Download PDFInfo
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- CN110947977A CN110947977A CN201911155348.7A CN201911155348A CN110947977A CN 110947977 A CN110947977 A CN 110947977A CN 201911155348 A CN201911155348 A CN 201911155348A CN 110947977 A CN110947977 A CN 110947977A
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 80
- 239000000956 alloy Substances 0.000 title claims abstract description 80
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000005507 spraying Methods 0.000 claims abstract description 39
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- 239000002245 particle Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 229910052709 silver Inorganic materials 0.000 claims abstract description 13
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 11
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- 238000002844 melting Methods 0.000 claims abstract description 4
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- 238000012546 transfer Methods 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
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- 230000000694 effects Effects 0.000 abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 3
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- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
Abstract
The invention discloses a production method of submicron AgSnTe alloy powder, which has the technical scheme that the method comprises the following steps of 1, weighing Ag, Sn and Te raw materials and mixing; step 2, adding the mixed raw materials into a high-temperature evaporator and vacuumizing the high-temperature evaporator; step 3, argon treatment; step 4, heating and melting the mixed raw materials; step 5, evaporating AgSnTe alloy liquid into a particle former; step 6, continuously adding the mixed raw materials, and enabling the AgSnTe alloy powder to enter a spraying tank; step 7, collecting AgSnTe alloy powder and liquid water by a water circulation powder collecting device; and 8, carrying out solid-liquid separation to obtain submicron AgSnTe alloy powder. The method has the advantages that the conductive silver paste is improved by adding the Te raw material, ohmic contact with the silicon bottom is formed, and simultaneously the conductive silver paste is combined with the aluminum plate to form a back field, the effects of high purity, high sphericity, high component uniformity, low oxygen content and large surface activity of the submicron AgSnTe alloy powder are effectively ensured, and the purpose of producing the submicron AgSnTe alloy powder in a large scale is realized.
Description
Technical Field
The invention relates to the technical field of generation and manufacture of an electric silver paste material, in particular to a production method of submicron AgSnTe alloy powder.
Background
Due to the development of economy and society of countries in the world, the consumption of energy is also increasing. The future stable energy supply has great influence on the economic development level of China and the stability of society. Currently, the main sources of energy are from oil, natural gas, coal, etc. These fuels are not only non-renewable energy sources, but also produce carbon dioxide and other greenhouse gases that contribute to global warming. In order to reduce the dependence on the traditional fossil fuel energy and reduce the emission of greenhouse gases, the development and utilization of solar energy resources become new power for economic development.
The conductive silver paste is a viscous paste of a mechanical mixture consisting of high-purity metal silver particles, a binder, a solvent and an auxiliary agent. Traditional conductive electrode materials, such as ITO, have excellent performance, but are relatively expensive to produce; the rare metal indium is limited in storage amount; the material is relatively brittle; the infrared transmittance is low and the application in flexible electrodes is limited. And the conductive silver paste is applied to the production and the manufacture of the monocrystalline silicon solar cell due to the good conductivity and the higher cost performance.
However, since the conductive silver paste is an important conductor in the cell after sintering, and needs to form an ohmic contact with the silicon substrate and combine with an aluminum plate to form a back surface field, the sintering performance of the current conductive silver paste is weak, which further affects the production and manufacture of the single crystal silicon solar cell, and needs to be improved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a production method of submicron AgSnTe alloy powder, and the production method of the submicron AgSnTe alloy powder has the effect of remarkably improving the sintering performance of conductive silver paste.
In order to achieve the purpose, the invention provides the following technical scheme:
a production method of submicron AgSnTe alloy powder comprises the following steps:
step 1, uniformly mixing 12-18 parts of Ag, 0.8-1.2 parts of Sn and 5-7 parts of Te according to parts by weight to obtain a mixed raw material;
step 2, adding the mixed raw materials into a crucible of a high-temperature evaporator, sealing the high-temperature evaporator and carrying out vacuum pumping treatment;
step 3, filling argon into the high-temperature evaporator from the bottom, and controlling the pressure of the high-temperature evaporator to be 110-120 kPa;
step 4, generating a plasma transfer arc by a plasma gun, heating the inside of the high-temperature evaporator from the top of the high-temperature evaporator by using the plasma transfer arc as a heating source, and heating and melting the mixed raw materials;
step 5, mixing the raw materials, mutually dissolving the raw materials into AgSnTe alloy liquid, evaporating the AgSnTe alloy liquid, and evaporating the AgSnTe alloy liquid into a particle former connected with a high-temperature evaporator along with argon flow;
and step 6, continuously feeding 12-18 parts of the following components in parts by weight into the high-temperature evaporator: 0.8-1.2 parts of: 5 to 7 portions of Ag, Sn and Te, and the flow of argon is controlled to be 23 to 27m3Forming AgSnTe alloy powder in a high-temperature evaporator, and moving the AgSnTe alloy powder into a spraying tank communicated with the particle former along with argon flow;
step 7, spraying water mist into the spraying tank by a spraying nozzle, mixing the water mist with the AgSnTe alloy powder, and then feeding the mixture into a water circulation powder collecting device;
and 8, starting a centrifugal machine in the water circulation powder collecting device to separate the AgSnTe alloy powder from liquid water, and obtaining submicron AgSnTe alloy powder with the purity of more than or equal to 99 percent, the particle size of 100-400nm and the spherical shape.
The invention is further configured to: in step 2, the crucible is a graphite crucible.
The invention is further configured to: in step 4, the working gas of the plasma transfer arc of the plasma gun is argon gas and ammonia gas, and the pressure is 3-4.5 MPa.
The invention is further configured to: in step 4, when the plasma gun is used as a heating source to generate a plasma transfer arc, the initial current is set to 350-400A, the voltage is set to 50-70V, the stable increase of the current and the voltage is controlled, the current is stably increased to 650-750A within 4 hours, and the voltage is increased to 70-90V.
The invention is further configured to: in the step 5, after the mixed raw materials are mutually dissolved into AgSnTe alloy liquid, the temperature is kept for 2 h.
The invention is further configured to: the particle former is a cold collecting pipe and is sequentially provided with a graphite pipe, a carbon felt layer, a stainless steel pipe and a stainless steel pipe from inside to outside, wherein a cold water circulating system is arranged between the two layers of stainless steel pipes.
The invention is further configured to: in the step 7, a plurality of spraying nozzles are arranged in the spraying tank and distributed in the same radian, and the plurality of spraying nozzles simultaneously spray water mist to the bottom of the spraying tank.
The invention is further configured to: the water circulation powder collecting device comprises a spraying tank, a large-volume solution storage, a centrifugal machine and a water pump which are connected, and liquid water is driven by the water pump to circulate in the water circulation powder collecting device.
The invention is further configured to: in step 8, the centrifuge is started up once per hour, and each start-up time is half an hour.
The invention is further configured to: in step 6, setting the feeding amount of the components in parts by weight to 12-18 parts per hour: 0.8-1.2 parts of: 5-7 parts of Ag, Sn and Te.
In conclusion, the invention has the following beneficial effects:
1. AgSnTe steam is cooled and nucleated by collision in a particle former and then grows into AgSnTe alloy powder, so that the AgSnTe steam is in a highly dispersed state in the whole reaction process, and the high purity, high sphericity, high component uniformity, low oxygen content and larger surface activity of the submicron-grade AgSnTe alloy powder are ensured under the protection of closed inert gas;
2. the circular processing production has high efficiency and low energy consumption, effectively improves the energy utilization rate, and is formed quickly and stably;
3. the plasma gun is used as a heating source to heat, melt and mutually dissolve Ag, Sn and Te raw materials, AgSnTe alloy liquid with uniform components is formed under the action of plasma arc spraying, and then AgSnTe alloy steam with uniform components is formed by increasing the power of the plasma gun;
4. submicron AgSnTe alloy powder with various particle sizes is produced by controlling the power of a plasma gun, the flow of system argon and the flow of cooling water of a cold water circulating system, the particle size of the alloy powder can be controlled at 100-500nm, and the yield of the submicron AgSnTe alloy powder is effectively controlled;
5. through the Te element added into the powder, the conductive silver paste is effectively improved, ohmic contact is formed between the conductive silver paste and the silicon bottom, and meanwhile, the conductive silver paste is combined with an aluminum plate to form a back surface field.
Drawings
Fig. 1 is an SEM image of the submicron-sized AgSnTe alloy powder of this example.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
As shown in FIG. 1, a submicron AgSnTe alloy powder has the effects of high purity, high sphericity, high compositional uniformity, low oxygen content, and large surface activity. The production and manufacturing of the submicron AgSnTe alloy powder are carried out by adopting a high-temperature evaporator, a particle former, a spray tank and a water circulation powder collecting device which are connected in sequence; the particle former is a cold collecting pipe, and is sequentially provided with a graphite pipe, a carbon felt layer, a stainless steel pipe and a stainless steel pipe from inside to outside, wherein a cold water circulating system is arranged between the two layers of stainless steel pipes; the water circulation powder collecting device comprises a spraying tank, a large-volume solution storage, a centrifugal machine and a water pump which are connected, and liquid water is driven by the water pump to circulate in the water circulation powder collecting device. A plurality of spraying nozzles distributed in the spraying tank in an equal radian mode are arranged in the spraying tank, and the plurality of spraying nozzles are used for spraying water mist to the bottom of the spraying tank at the same time.
Example one
The invention provides a production method of submicron AgSnTe alloy powder, which comprises the following steps:
step 1, uniformly mixing 12 parts of Ag, 0.8 part of Sn and 5 parts of Te according to parts by weight to obtain a mixed raw material;
step 2, adding the mixed raw materials into a graphite crucible of a high-temperature evaporator, sealing the high-temperature evaporator and performing vacuum-pumping treatment;
step 3, filling argon into the high-temperature evaporator from the bottom, and controlling the pressure of the high-temperature evaporator to be 110 kPa;
step 4, generating a plasma transfer arc by adopting a plasma gun with working gas of argon and ammonia, setting the pressure to be 3.2MPa, the initial current to be 350A and the initial voltage to be 50V, simultaneously controlling the stable increase of the current and the voltage, and stably increasing the current to be 650A and the voltage to be 70V by 4 hours, so that the plasma gun is used as a heating source to heat the high-temperature evaporator from the top of the high-temperature evaporator and heat and melt the mixed raw materials;
step 5, the mixed raw materials are mutually dissolved into AgSnTe alloy liquid and then are evaporated, and the temperature is kept for 2 hours, so that the AgSnTe alloy liquid is evaporated into a particle former connected with a high-temperature evaporator along with argon flow;
and step 6, continuously feeding 12 parts of the components in parts by weight: 0.8 part: 5 parts of Ag, Sn and Te, and controlling the flow of argon to be 23m3Forming AgSnTe alloy powder in a high-temperature evaporator, and moving the AgSnTe alloy powder into a spraying tank communicated with the particle former along with argon flow;
step 7, spraying water mist to the bottom of the spraying tank by the plurality of spraying nozzles simultaneously, mixing the water mist with the AgSnTe alloy powder, and then feeding the mixture into a water circulation powder collecting device;
step 8, starting the centrifugal machine in the water circulation powder collecting device once per hour, wherein the starting time of the centrifugal machine is half an hour each time, so that the AgSnTe alloy powder is separated from liquid water, and submicron AgSnTe alloy powder with the purity of more than or equal to 99%, the grain size of 100-400nm and the spherical shape is obtained;
and 9, when AgSnTe alloy powder starts to be stably produced, continuing the steps 6 to 8, and setting the quantitative components in parts by weight to 12 parts per hour: 0.8 part: 5 parts of Ag, Sn and Te.
Example two
The invention provides a production method of submicron AgSnTe alloy powder, which comprises the following steps:
step 1, uniformly mixing 15 parts of Ag, 1 part of Sn and 6 parts of Te according to parts by weight to obtain a mixed raw material;
step 2, adding the mixed raw materials into a graphite crucible of a high-temperature evaporator, sealing the high-temperature evaporator and performing vacuum-pumping treatment;
step 3, filling argon into the high-temperature evaporator from the bottom, and controlling the pressure of the high-temperature evaporator to be 115 kPa;
step 4, generating a plasma transfer arc by adopting a plasma gun with working gas of argon and ammonia, setting the pressure to be 3.8MPa, the initial current to be 375A and the initial voltage to be 60V, simultaneously controlling the stable increase of the current and the voltage, stably increasing the current to 700A and the voltage to 80V by 4 hours, and heating the plasma gun serving as a heating source from the top of the high-temperature evaporator to the high-temperature evaporator and heating and melting the mixed raw materials;
step 5, the mixed raw materials are mutually dissolved into AgSnTe alloy liquid and then are evaporated, and the temperature is kept for 2 hours, so that the AgSnTe alloy liquid is evaporated into a particle former connected with a high-temperature evaporator along with argon flow;
and step 6, continuously feeding 15 parts of the components in parts by weight into the high-temperature evaporator: 1 part of: 6 parts of Ag, Sn and Te, and controlling the flow of argon to be 25m3Forming AgSnTe alloy powder in a high-temperature evaporator, and moving the AgSnTe alloy powder into a spraying tank communicated with the particle former along with argon flow;
step 7, spraying water mist to the bottom of the spraying tank by the plurality of spraying nozzles simultaneously, mixing the water mist with the AgSnTe alloy powder, and then feeding the mixture into a water circulation powder collecting device;
step 8, starting the centrifugal machine in the water circulation powder collecting device once per hour, wherein the starting time of the centrifugal machine is half an hour each time, so that the AgSnTe alloy powder is separated from liquid water, and submicron AgSnTe alloy powder with the purity of more than or equal to 99%, the grain size of 100-400nm and the spherical shape is obtained;
and 9, when AgSnTe alloy powder starts to be stably produced, continuing the steps 6 to 8, and setting the quantitative components in parts by weight to 15 parts per hour: 1 part of: 6 parts of Ag, Sn and Te.
EXAMPLE III
The invention provides a production method of submicron AgSnTe alloy powder, which comprises the following steps:
step 1, uniformly mixing 18 parts of Ag, 1.2 parts of Sn and 7 parts of Te according to parts by weight to obtain a mixed raw material;
step 2, adding the mixed raw materials into a graphite crucible of a high-temperature evaporator, sealing the high-temperature evaporator and performing vacuum-pumping treatment;
step 3, filling argon into the high-temperature evaporator from the bottom, and controlling the pressure of the high-temperature evaporator to be 120 kPa;
step 4, generating a plasma transfer arc by adopting a plasma gun with working gas of argon and ammonia, setting the pressure to be 4.5MPa, the initial current to be 400A and the initial voltage to be 70V, simultaneously controlling the stable increase of the current and the voltage, stably increasing the current to 750A and the voltage to 90V by 4 hours, so that the plasma gun is used as a heating source to heat the high-temperature evaporator from the top of the high-temperature evaporator and heat and melt the mixed raw materials;
step 5, the mixed raw materials are mutually dissolved into AgSnTe alloy liquid and then are evaporated, and the temperature is kept for 2 hours, so that the AgSnTe alloy liquid is evaporated into a particle former connected with a high-temperature evaporator along with argon flow;
and step 6, continuously feeding 18 parts of the following components in parts by weight: 1.2 parts of: 7 parts of Ag, Sn and Te, and controlling the flow of argon gas to be 27m3Forming AgSnTe alloy powder in a high-temperature evaporator, and moving the AgSnTe alloy powder into a spraying tank communicated with the particle former along with argon flow;
step 7, spraying water mist to the bottom of the spraying tank by the plurality of spraying nozzles simultaneously, mixing the water mist with the AgSnTe alloy powder, and then feeding the mixture into a water circulation powder collecting device;
step 8, starting the centrifugal machine in the water circulation powder collecting device once per hour, wherein the starting time of the centrifugal machine is half an hour each time, so that the AgSnTe alloy powder is separated from liquid water, and submicron AgSnTe alloy powder with the purity of more than or equal to 99%, the grain size of 100-400nm and the spherical shape is obtained;
and 9, when AgSnTe alloy powder starts to be stably produced, continuing the steps 6 to 8, and setting the quantitative components in parts by weight to 18 parts per hour: 1.2 parts of: 7 parts of Ag, Sn and Te raw materials.
When a fixed amount of 5kg of the mixed raw materials was charged into the high-temperature evaporator per hour, submicron-sized AgSnTe alloy powder having a particle size of 457nm (see FIG. 1) was stably produced with a yield of 5 kg/h.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiment, but all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the present invention may occur to those skilled in the art without departing from the principle of the present invention, and such modifications and embellishments should also be considered as within the scope of the present invention.
Claims (10)
1. A production method of submicron AgSnTe alloy powder is characterized by comprising the following steps:
step 1, uniformly mixing 12-18 parts of Ag, 0.8-1.2 parts of Sn and 5-7 parts of Te according to parts by weight to obtain a mixed raw material;
step 2, adding the mixed raw materials into a crucible of a high-temperature evaporator, sealing the high-temperature evaporator and carrying out vacuum pumping treatment;
step 3, filling argon into the high-temperature evaporator from the bottom, and controlling the pressure of the high-temperature evaporator to be 110-120 kPa;
step 4, generating a plasma transfer arc by a plasma gun, heating the inside of the high-temperature evaporator from the top of the high-temperature evaporator by using the plasma transfer arc as a heating source, and heating and melting the mixed raw materials;
step 5, mixing the raw materials, mutually dissolving the raw materials into AgSnTe alloy liquid, evaporating the AgSnTe alloy liquid, and evaporating the AgSnTe alloy liquid into a particle former connected with a high-temperature evaporator along with argon flow;
and step 6, continuously feeding 12-18 parts of the following components in parts by weight into the high-temperature evaporator: 0.8-1.2 parts of: 5-7 parts of AgSn and Te, controlling the flow of argon gas to be 23-27m3Forming AgSnTe alloy powder in a high-temperature evaporator, and moving the AgSnTe alloy powder into a spraying tank communicated with the particle former along with argon flow;
step 7, spraying water mist into the spraying tank by a spraying nozzle, mixing the water mist with the AgSnTe alloy powder, and then feeding the mixture into a water circulation powder collecting device;
and 8, starting a centrifugal machine in the water circulation powder collecting device to separate the AgSnTe alloy powder from liquid water, and obtaining submicron AgSnTe alloy powder with the purity of more than or equal to 99 percent, the particle size of 100-400nm and the spherical shape.
2. The production method of a submicron-sized AgSnTe alloy powder according to claim 1, characterized in that: in step 2, the crucible is a graphite crucible.
3. The production method of a submicron-sized AgSnTe alloy powder according to claim 1, characterized in that: in step 4, the working gas of the plasma transfer arc of the plasma gun is argon gas and ammonia gas, and the pressure is 3-4.5 MPa.
4. The production method of a submicron-sized AgSnTe alloy powder according to claim 1, characterized in that: in step 4, when the plasma gun is used as a heating source to generate a plasma transfer arc, the initial current is set to 350-400A, the voltage is set to 50-70V, the stable increase of the current and the voltage is controlled, the current is stably increased to 650-750A within 4 hours, and the voltage is increased to 70-90V.
5. The production method of a submicron-sized AgSnTe alloy powder according to claim 4, characterized in that: in the step 5, after the mixed raw materials are mutually dissolved into AgSnTe alloy liquid, the temperature is kept for 2 h.
6. The production method of a submicron-sized AgSnTe alloy powder according to claim 1, characterized in that: the particle former is a cold collecting pipe and is sequentially provided with a graphite pipe, a carbon felt layer, a stainless steel pipe and a stainless steel pipe from inside to outside, wherein a cold water circulating system is arranged between the two layers of stainless steel pipes.
7. The production method of a submicron-sized AgSnTe alloy powder according to claim 1, characterized in that: in the step 7, a plurality of spraying nozzles are arranged in the spraying tank and distributed in the same radian, and the plurality of spraying nozzles simultaneously spray water mist to the bottom of the spraying tank.
8. The production method of a submicron-sized AgSnTe alloy powder according to claim 1, characterized in that: the water circulation powder collecting device comprises a spraying tank, a large-volume solution storage, a centrifugal machine and a water pump which are connected, and liquid water is driven by the water pump to circulate in the water circulation powder collecting device.
9. The production method of a submicron-sized AgSnTe alloy powder according to claim 8, characterized in that: in step 8, the centrifuge is started up once per hour, and each start-up time is half an hour.
10. The production method of a submicron-sized AgSnTe alloy powder according to claim 7, characterized in that: in step 6, when AgSnTe alloy powder starts to be stably produced, setting the quantitative components in parts by weight to 12-18 parts per hour: 0.8-1.2 parts of: 5-7 parts of Ag, Sn and Te.
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| CN112846205A (en) * | 2020-12-29 | 2021-05-28 | 宁波广新纳米材料有限公司 | Liquid phase collection method in superfine metal powder preparation process |
Citations (6)
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