CN115446323A - Method for preparing tungsten-molybdenum powder by using waste target scrap powder of tungsten and molybdenum - Google Patents
Method for preparing tungsten-molybdenum powder by using waste target scrap powder of tungsten and molybdenum Download PDFInfo
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- CN115446323A CN115446323A CN202211159877.6A CN202211159877A CN115446323A CN 115446323 A CN115446323 A CN 115446323A CN 202211159877 A CN202211159877 A CN 202211159877A CN 115446323 A CN115446323 A CN 115446323A
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- 239000000843 powder Substances 0.000 title claims abstract description 94
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 86
- 239000010937 tungsten Substances 0.000 title claims abstract description 86
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 84
- 239000011733 molybdenum Substances 0.000 title claims abstract description 84
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 84
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 239000002699 waste material Substances 0.000 title claims abstract description 58
- MGRWKWACZDFZJT-UHFFFAOYSA-N molybdenum tungsten Chemical compound [Mo].[W] MGRWKWACZDFZJT-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 25
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910001182 Mo alloy Inorganic materials 0.000 claims abstract description 27
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 23
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 18
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 18
- -1 tungsten-molybdenum ammonia Chemical compound 0.000 claims abstract description 16
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002386 leaching Methods 0.000 claims abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 8
- 238000005507 spraying Methods 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- AWOORJZBKBDNCP-UHFFFAOYSA-N molybdenum;oxotungsten Chemical compound [Mo].[W]=O AWOORJZBKBDNCP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000007935 neutral effect Effects 0.000 claims abstract description 5
- 238000000889 atomisation Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 3
- 238000005242 forging Methods 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 abstract description 4
- 238000006731 degradation reaction Methods 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000001694 spray drying Methods 0.000 abstract description 4
- 230000009467 reduction Effects 0.000 abstract description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract 2
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- 229910052573 porcelain Inorganic materials 0.000 description 7
- 230000008569 process Effects 0.000 description 4
- 238000005275 alloying Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
Images
Classifications
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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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for preparing tungsten-molybdenum powder by using waste target scrap powder of tungsten and molybdenum, which comprises the following steps: 1. placing waste target scrap powder of tungsten and molybdenum in an air atmosphere for high-temperature calcination to obtain an oxide A of tungsten and molybdenum; 2. putting the tungsten-molybdenum oxide A into a hot ammonia water solution for leaching to obtain a tungsten-molybdenum ammonia solution B; 3. filtering the ammonia solution B of tungsten and molybdenum, and adjusting the pH of the filtrate to be nearly neutral to obtain oxalic acid complex solution C of tungsten and molybdenum; 4. adjusting the concentration of tungsten and molybdenum ions in the oxalic acid complex solution C of tungsten and molybdenum, and spraying to obtain powder D; 5. and reducing the powder D in a hydrogen atmosphere to obtain tungsten-molybdenum alloy powder. According to the invention, the waste target scrap powder of tungsten and molybdenum is sequentially subjected to high-temperature calcination, hot ammonia leaching, spray drying and hydrogen reduction, so that the tungsten-molybdenum alloy powder is prepared by using the waste targets of tungsten and molybdenum, the resource recovery and utilization rate of tungsten and molybdenum waste is improved, the resource waste caused by degradation treatment of the waste target scrap powder of tungsten and molybdenum is avoided, and the method is simple and efficient and is suitable for industrialization.
Description
Technical Field
The invention belongs to the technical field of metallurgical engineering, and particularly relates to a method for preparing tungsten-molybdenum powder by using waste target scrap powder of tungsten and molybdenum.
Background
Tungsten and molybdenum targets are basic materials in the industrial fields of electronics, semiconductors and the like, a large amount of waste materials are generated in the using process, the high-end recycling can be realized for targets with low loss through in-situ repair, and the high-loss and high-pollution blocky waste materials can be degraded and utilized after being cleaned or prepared into metal powder by a certain method to realize resource recycling. The scrap-shaped or powdery waste materials generated in the processes of processing, using, transporting and storing are mostly used as waste materials for degradation treatment, so that certain resource waste is caused; on the other hand, the spherical tungsten-molybdenum alloy powder has the characteristics of high sphericity, high fluidity and the like, so that the spherical tungsten-molybdenum alloy powder has a wide application range, and if the tungsten-molybdenum alloy powder is prepared by taking the degraded and utilized waste as a raw material, not only can the resource be recovered, but also the high-end reutilization of the tungsten-molybdenum alloy powder can be realized, and the assistance is provided for the high-quality development strategy.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for preparing tungsten-molybdenum powder by using waste target scrap powder of tungsten and molybdenum, aiming at the defects of the prior art. According to the method, the tungsten-molybdenum alloy powder is prepared by sequentially carrying out high-temperature calcination, hot ammonia water leaching, spray drying and hydrogen reduction on the waste target scrap powder of tungsten and molybdenum, so that the tungsten-molybdenum alloy powder is prepared by utilizing the waste targets of tungsten and molybdenum, the resource recovery and utilization rate of tungsten and molybdenum waste is improved, and the resource waste caused by degradation treatment of the waste target scrap powder of tungsten and molybdenum is avoided.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a method for preparing tungsten-molybdenum powder by using waste target scrap powder of tungsten and molybdenum is characterized by comprising the following steps:
placing waste target scrap powder of tungsten and molybdenum in an air atmosphere for high-temperature calcination to obtain an oxide A of tungsten and molybdenum;
step two, placing the tungsten-molybdenum oxide A obtained in the step one into a hot ammonia water solution for leaching to obtain a tungsten-molybdenum ammonia solution B;
step three, filtering the ammonia solution B of the tungsten and the molybdenum obtained in the step two, and adding oxalic acid into the filtrate to adjust the pH value to be nearly neutral to obtain oxalic acid complex solution C of the tungsten and the molybdenum;
step four, adjusting the concentration of tungsten and molybdenum ions in the oxalic acid complex liquid C of tungsten and molybdenum obtained in the step three, and then spraying through airflow type atomization to obtain powder D;
and step five, reducing the powder D obtained in the step four in a hydrogen atmosphere to obtain the tungsten-molybdenum alloy powder.
According to the invention, tungsten waste target scrap powder and molybdenum waste target scrap powder are subjected to high-temperature calcination in the air atmosphere to obtain oxides of tungsten and molybdenum, then metal elements of tungsten and molybdenum are leached out in a hot ammonia water solution, the obtained ammonia solution of tungsten and molybdenum is filtered and added with oxalic acid to adjust the pH value to be near neutral, so that the ammonium solution of tungsten and molybdenum is prevented from being decomposed into smaller irregular particles in the subsequent spray atomization process and is difficult to collect, the yield of tungsten-molybdenum alloy powder is improved, the sphericity of tungsten-molybdenum alloy powder is improved, the quality of tungsten-molybdenum alloy powder is improved, meanwhile, the tungsten and molybdenum are stably mixed at the atomic level through complexation, the alloying degree of the tungsten-molybdenum alloy powder is favorably improved, the application of the tungsten-molybdenum alloy powder is expanded, and the near neutral solution has no pungent smell of the ammonia solution, so that a good preparation environment is ensured; and then adjusting the concentration of tungsten and molybdenum ions to ensure that the granularity of the tungsten-molybdenum alloy powder is proper and avoid influencing the yield due to over-small granularity, preparing tungsten-molybdenum precursor powder by a spray drying method, and reducing at high temperature in a hydrogen atmosphere to obtain the tungsten-molybdenum alloy powder.
The method for preparing the tungsten-molybdenum powder by using the waste target scrap powder of tungsten and molybdenum is characterized in that in the step one, the waste target scrap powder of tungsten and molybdenum is scrap-shaped or powder, the high-temperature forging temperature is 650-800 ℃, and the mass content of the waste target scrap powder of tungsten in the waste target scrap powder of tungsten and molybdenum is 5-95%. According to the invention, the temperature of high-temperature calcination is controlled, so that the molybdenum loss caused by molybdenum volatilization due to high temperature is avoided while tungsten and molybdenum are oxidized.
The method for preparing the tungsten-molybdenum powder by using the waste target scrap powder of tungsten and molybdenum is characterized in that the concentration of the hot ammonia water solution in the step two is 1-4 mol/L, and the leaching temperature is 30-70 ℃. By controlling the concentration of the hot ammonia water solution and the leaching temperature, the dissolution and leaching of tungsten and molybdenum elements are realized, and the waste of resources and energy is avoided.
The method for preparing the tungsten-molybdenum powder by using the waste target scrap powder of tungsten and molybdenum is characterized in that the pH value is 6-8 in the step three.
The method for preparing the tungsten-molybdenum powder by using the waste target scrap powder of tungsten and molybdenum is characterized in that the total concentration of tungsten and molybdenum ions in the adjusted oxalic acid complex liquid C of tungsten and molybdenum is 1 g/L-20 g/L. The particle size of the tungsten-molybdenum alloy powder is controlled to be moderate through the total concentration of tungsten ions and molybdenum ions, and the yield of the tungsten-molybdenum alloy powder is improved.
Compared with the prior art, the invention has the following advantages:
1. compared with the traditional recovery of waste tungsten and molybdenum targets, the method is based on the characteristics of tungsten and molybdenum waste materials and tungsten-molybdenum alloy powder, the waste target scrap powder of tungsten and molybdenum is sequentially subjected to high-temperature calcination, hot ammonia water leaching, spray drying and hydrogen reduction to prepare the tungsten-molybdenum alloy powder, the tungsten-molybdenum powder is prepared by utilizing the waste targets of tungsten and molybdenum, the resource recovery utilization rate of the tungsten and molybdenum waste materials is improved, and the resource waste caused by degradation treatment of the waste target scrap powder of tungsten and molybdenum is avoided.
2. According to the invention, oxalic acid is adopted to adjust PH for complexing, and a subsequent spraying process is combined, so that the alloying degree of the tungsten-molybdenum alloy powder is improved, the yield of the tungsten-molybdenum alloy powder is improved, the sphericity of the tungsten-molybdenum alloy powder is improved, and the application of the tungsten-molybdenum alloy powder is expanded.
3. The method for preparing the tungsten-molybdenum powder by using the waste target scrap powder of tungsten and molybdenum is simple and efficient, and is suitable for industrial operation.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a flow chart of the process for preparing tungsten-molybdenum powder from waste target scrap powder of tungsten and molybdenum.
Detailed Description
Example 1
As shown in fig. 1, the present embodiment includes the following steps:
placing waste target scraps of tungsten and molybdenum in a porcelain boat, covering the porcelain boat, placing the porcelain boat in a muffle furnace, and calcining at high temperature of 650 ℃ in an air atmosphere to obtain an oxide A of tungsten and molybdenum; the mass content of the tungsten waste target scraps in the tungsten and molybdenum waste target scraps is 5%;
step two, leaching the tungsten-molybdenum oxide A obtained in the step one in a 1mol/L hot ammonia water solution at the temperature of 30 ℃ to obtain a tungsten-molybdenum ammonia solution B;
step three, filtering the ammonia solution B of tungsten and molybdenum obtained in the step two, and adding oxalic acid into the filtrate to adjust the pH value to 8 to obtain oxalic acid complex solution C of tungsten and molybdenum;
step four, adjusting the total concentration of tungsten and molybdenum ions in the oxalic acid complex solution C of tungsten and molybdenum obtained in the step three to be 20g/L, and then spraying by airflow atomization, wherein the atomization temperature is 180 ℃, and the addition amount of the solution is 200mL/h, so as to obtain powder D;
and step five, reducing the powder D obtained in the step four in a hydrogen atmosphere at the temperature of 700 ℃ for 2 hours to obtain the tungsten-molybdenum alloy powder.
Example 2
As shown in fig. 1, the present embodiment includes the following steps:
placing waste target powder of tungsten and molybdenum in a porcelain boat, covering the porcelain boat, placing the porcelain boat in a muffle furnace, and calcining the porcelain boat at 800 ℃ in an air atmosphere to obtain an oxide A of tungsten and molybdenum; the mass content of the tungsten waste target powder in the tungsten and molybdenum waste target powder is 95%;
step two, placing the tungsten-molybdenum oxide A obtained in the step one into a 4mol/L hot ammonia water solution for leaching, wherein the leaching temperature is 70 ℃, and obtaining a tungsten-molybdenum ammonia solution B;
step three, filtering the ammonia solution B of the tungsten and the molybdenum obtained in the step two, and adding oxalic acid into the filtrate to adjust the pH value to 6 to obtain oxalic acid complex solution C of the tungsten and the molybdenum;
step four, adjusting the total concentration of tungsten ions and molybdenum ions in the oxalic acid complex solution C of tungsten and molybdenum obtained in the step three to be 1g/L, and then spraying through airflow atomization, wherein the atomization temperature is 180 ℃, and the addition amount of the solution is 200mL/h, so as to obtain powder D;
and step five, reducing the powder D obtained in the step four in a hydrogen atmosphere at the temperature of 700 ℃ for 2 hours to obtain the tungsten-molybdenum alloy powder.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modifications, alterations and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (5)
1. A method for preparing tungsten-molybdenum powder by using waste target scrap powder of tungsten and molybdenum is characterized by comprising the following steps:
placing waste target scrap powder of tungsten and molybdenum in an air atmosphere for high-temperature calcination to obtain an oxide A of tungsten and molybdenum;
step two, placing the tungsten-molybdenum oxide A obtained in the step one into a hot ammonia water solution for leaching to obtain a tungsten-molybdenum ammonia solution B;
step three, filtering the ammonia solution B of tungsten and molybdenum obtained in the step two, and adding oxalic acid into the filtrate to adjust the pH value to be nearly neutral to obtain oxalic acid complex solution C of tungsten and molybdenum;
step four, adjusting the concentration of tungsten and molybdenum ions in the oxalic acid complex liquid C of tungsten and molybdenum obtained in the step three, and then spraying through airflow atomization to obtain powder D;
and step five, reducing the powder D obtained in the step four in a hydrogen atmosphere to obtain the tungsten-molybdenum alloy powder.
2. The method for preparing tungsten-molybdenum powder from the waste target scrap powder of tungsten and molybdenum according to claim 1, wherein the waste target scrap powder of tungsten and molybdenum in the step one is scrap-shaped or powder-shaped, the high-temperature forging temperature is 650 ℃ to 800 ℃, and the mass content of the waste target scrap powder of tungsten in the waste target scrap powder of tungsten and molybdenum is 5% to 95%.
3. The method for preparing tungsten-molybdenum powder from waste target swarf of tungsten and molybdenum as claimed in claim 1, wherein the concentration of the hot ammonia solution in the second step is 1-4 mol/L, and the leaching temperature is 30-70 ℃.
4. The method for preparing tungsten-molybdenum powder from waste target scrap powder of tungsten and molybdenum as claimed in claim 1, wherein the pH is 6-8 in step three.
5. The method for preparing tungsten-molybdenum powder from waste target scrap powder of tungsten and molybdenum according to claim 1, wherein the total concentration of tungsten and molybdenum ions in the adjusted oxalic acid complex solution C of tungsten and molybdenum is 1g/L to 20g/L in the fourth step.
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