CN111112628A - Method for preparing fine-grained low-oxygen titanium and titanium alloy powder by using cutting waste - Google Patents
Method for preparing fine-grained low-oxygen titanium and titanium alloy powder by using cutting waste Download PDFInfo
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- CN111112628A CN111112628A CN202010044236.0A CN202010044236A CN111112628A CN 111112628 A CN111112628 A CN 111112628A CN 202010044236 A CN202010044236 A CN 202010044236A CN 111112628 A CN111112628 A CN 111112628A
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- titanium
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- titanium alloy
- oxygen
- cutting waste
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- 239000000843 powder Substances 0.000 title claims abstract description 58
- 239000001301 oxygen Substances 0.000 title claims abstract description 43
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 43
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000002699 waste material Substances 0.000 title claims abstract description 29
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 28
- 239000010936 titanium Substances 0.000 title claims abstract description 28
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 27
- 238000005520 cutting process Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000006356 dehydrogenation reaction Methods 0.000 claims abstract description 16
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 15
- 238000002161 passivation Methods 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 229910052786 argon Inorganic materials 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 238000004663 powder metallurgy Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000012467 final product Substances 0.000 abstract 1
- 238000010301 surface-oxidation reaction Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 16
- 238000001816 cooling Methods 0.000 description 8
- -1 titanium hydride Chemical compound 0.000 description 8
- 229910000048 titanium hydride Inorganic materials 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 238000009461 vacuum packaging Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000010814 metallic waste Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
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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
- B22F9/023—Hydrogen absorption
-
- 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
-
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a method for preparing low-cost fine-grained low-oxygen titanium and titanium alloy powder by using cutting waste, belonging to the technical field of powder metallurgy powder preparation. The method takes titanium and titanium alloy cutting waste as raw materials, and obtains the final product through the processes of hydrogenation, crushing, dehydrogenation, passivation and the like. The method has low cost by recycling the titanium and titanium alloy waste materials, and effectively solves the problems of waste of cutting waste materials, environmental pollution and the like; preparing the waste material into titanium and titanium alloy powder by adopting a hydrogenation dehydrogenation method, and controlling the surface oxidation layer state and the oxygen content of powder particles by passivation treatment to prepare the titanium and titanium alloy powder with the oxygen content of less than or equal to 0.2 wt.% and the granularity (D)50) The titanium and titanium alloy powder with the particle size less than 50 mu m has excellent powder oxidation resistance, and the oxygen content of the powder is basically stable and unchanged after the powder is placed in the air at room temperature for one week.
Description
Technical Field
The invention belongs to the field of powder metallurgy, and relates to a method for preparing powder from titanium and titanium alloy cutting waste.
Background
Titanium and titanium alloy have excellent performance and are widely applied in the fields of aerospace, biomedicine, machinery and the like. In the process of processing titanium materials, a large amount of scraps are generated due to the factors of difficult processing, complex process, low material utilization rate and the like, so that the great waste of titanium resources and environmental pollution are caused. At present, the metal waste is recycled mainly by adopting a smelting method, and because titanium and titanium alloy have the characteristic of high melting point, the high energy consumption in the smelting process causes the sharp increase of the production cost, and the application and the development of recycling are severely restricted. Compared with the traditional smelting casting and forging process, the powder metallurgy technology has the advantages of near net shape and high material utilization rate, and effectively reduces the production cost. The method recycles the raw materials at the temperature lower than the melting point of the metal and produces the raw materials suitable for powder metallurgy, thereby being an effective method for preparing products with high performance and low cost and reducing energy consumption. The titanium and titanium alloy powder is prepared by carrying out hydrogenation dehydrogenation (namely hydrogenation, crushing and dehydrogenation) on the cutting waste, so that the cutting waste can be effectively recycled; because titanium and titanium alloy powder have high activity and are easy to oxidize, the key point for producing high-quality powder is the powder passivation treatment process, controlling the oxygen content and the powder oxidation resistance in the preparation process.
Disclosure of Invention
The invention aims to develop a method for preparing low-cost fine-grained low-oxygen titanium and titanium alloy powder by using cutting waste.
The invention comprises the following specific steps:
(1) cleaning the surface of the waste material by using titanium and titanium alloy cutting waste material as raw materials;
(2) carrying out hydrogenation, crushing and dehydrogenation treatment on the clean waste obtained in the step (1);
(3) passivating the powder obtained in the step (2) in a certain atmosphere to obtain a final powder product;
(4) the powder particle size and oxygen content were tested and left in air for a period of time to compare the change in oxygen content.
Further, the cleaning solvent in step (1) is an organic solvent or a weak acid, such as acetone or dilute hydrochloric acid.
Further, the hydrogenation treatment temperature in the step (2) is 500-; the dehydrogenation treatment temperature is 500-800 ℃, and the time is 2-5 h.
Further, the passivation treatment atmosphere in the step (3) is a mixed atmosphere of argon and oxygen with the oxygen content not more than 10%, the passivation temperature is not higher than 300 ℃, and the passivation time is not more than 5 hours.
The technique of the invention has the following advantages:
(1) the titanium and titanium alloy powder is prepared by taking the cutting waste as the raw material, so that the waste is effectively utilized, the resource utilization rate is improved, and the production cost is reduced.
(2) Through passivation treatment, the type and thickness of an oxide film phase on the surface of powder particles are controlled, a compact oxide film is formed, further oxidation of the powder is effectively prevented, and the powder with low oxygen content and excellent oxidation resistance is obtained.
(3) Can prepare the product with oxygen content less than or equal to 0.2 wt.% and particle size (D)50) The oxygen content of the powder with the particle size less than 50 mu m is basically stable and unchanged after the powder is placed in air at room temperature for one week.
Drawings
FIG. 1 scanning electron micrograph of hydrogenated dehydrogenated low cost titanium powder prepared in example 1.
Detailed Description
Example 1
The titanium cutting waste is cut into filaments with the length of 8-10mm, and the filaments are placed into acetone for ultrasonic cleaning for 10 min. Weighing 5kg of titanium filament, loading into a hydrogenation furnace, and heating to 7 ℃ at a heating rate of 15 ℃/min in a hydrogen atmosphere by high-purity hydrogenKeeping the temperature at 00 ℃ for 5h, and then completing the hydrogenation reaction to obtain titanium hydride filaments; cooling to room temperature, taking out titanium hydride powder in a vacuum glove box, crushing under protective atmosphere argon, sieving, grading, and then putting the treated powder into a container of 1 × 10-3Heating to 750 ℃ in a Pa vacuum furnace at a heating rate of 10 ℃/min for dehydrogenation, cooling to room temperature after dehydrogenation reaction for 3h, introducing argon with the oxygen content of 5% at a flow rate of 0.8L/min into a mixed atmosphere of the argon and the oxygen for pre-oxidation or passivation for 5h, taking powder in a vacuum glove box, detecting the oxygen content, carrying out vacuum packaging and storing to obtain powder with the particle size of 50 mu m and the oxygen content of 0.06 wt%, and taking 50g of the powder and placing the powder in the air for 168h with the oxygen content of 0.07 wt%.
Example 2
The titanium cutting waste is cut into filaments with the length of 3-5mm, and the filaments are placed into acetone for ultrasonic cleaning for 10 min. Weighing 10kg of titanium filaments, loading the titanium filaments into a hydrogenation furnace, heating to 680 ℃ at a heating rate of 15 ℃/min in a hydrogen atmosphere through high-purity hydrogen, and preserving heat for 5h to complete hydrogenation reaction to obtain titanium hydride filaments; cooling to room temperature, taking out titanium hydride powder in a vacuum glove box, crushing under protective atmosphere argon, sieving, grading, and then putting the treated powder into a container of 1 × 10-3Heating to 730 ℃ at a heating rate of 10 ℃/min in a Pa vacuum furnace for dehydrogenation, cooling to room temperature after dehydrogenation reaction for 3h, introducing argon with the oxygen content of 3% at a flow rate of 0.8L/min into a mixed atmosphere of the argon and the oxygen for pre-oxidation or passivation for 5h, taking powder in a vacuum glove box, detecting the oxygen content, carrying out vacuum packaging and storing to obtain powder with the particle size of 30 mu m and the oxygen content of 0.10 wt%, and taking 50g of the powder and placing the powder in the air for 168h with the oxygen content of 0.11 wt%.
Example 3
Cutting the titanium alloy cutting waste into filaments with the length of 3-5mm, and putting the filaments into acetone for ultrasonic cleaning for 10 min. Weighing 10kg of titanium alloy filaments, loading the titanium alloy filaments into a hydrogenation furnace, heating to 680 ℃ at a heating rate of 15 ℃/min in a hydrogen atmosphere through high-purity hydrogen, and preserving heat for 3h to complete hydrogenation reaction to obtain titanium hydride alloy filaments; cooling to room temperature, taking out titanium hydride alloy powder in a vacuum glove box, crushing under protective atmosphere argon, sieving and grading, and then putting the treated powder into a production line 110-3Heating to 730 ℃ at a heating rate of 10 ℃/min in a Pa vacuum furnace for dehydrogenation, cooling to room temperature after dehydrogenation reaction for 3h, introducing argon with the oxygen content of 5% at a flow rate of 1L/min into a mixed atmosphere of the argon and the oxygen for preoxidation or passivation treatment for 3.5h, taking powder in a vacuum glove box, detecting the oxygen content, carrying out vacuum packaging and storing to obtain the powder with the particle size of 35 mu m and the oxygen content of 0.10 wt%, and taking 50g of the powder, placing the powder in the air for 168h with the oxygen content of 0.11 wt%.
Example 4
Cutting the titanium alloy cutting waste into filaments with the length of 3-5mm, and putting the filaments into acetone for ultrasonic cleaning for 10 min. Weighing 10kg of titanium alloy filaments, loading the titanium alloy filaments into a hydrogenation furnace, heating to 680 ℃ at a heating rate of 10 ℃/min in a hydrogen atmosphere through high-purity hydrogen, and preserving heat for 3h to complete hydrogenation reaction to obtain titanium hydride alloy filaments; cooling to room temperature, taking out titanium hydride alloy powder in a vacuum glove box, crushing under protective atmosphere argon, sieving, grading, and then putting the treated powder into a vacuum glove box with the volume of 1 multiplied by 10-3Heating to 730 ℃ in a Pa vacuum furnace at the heating rate of 12 ℃/min for dehydrogenation, cooling to room temperature after dehydrogenation reaction for 3.5h, introducing argon with the oxygen content of 8% at the flow rate of 1L/min into the atmosphere of the mixture of the argon and the oxygen for preoxidation or passivation for 2.5h, taking powder in a vacuum glove box, detecting the oxygen content, carrying out vacuum packaging and storing to obtain the powder with the particle size of 40 mu m and the oxygen content of 0.09 wt%, and taking 50g of the powder and placing the powder in the air for 168h with the oxygen content of 0.09 wt%.
Claims (4)
1. A method for preparing fine-grained low-oxygen titanium and titanium alloy powder by using cutting waste is characterized by comprising the following preparation steps:
(1) cleaning the surface of the waste material by using titanium and titanium alloy cutting waste material as raw materials;
(2) carrying out hydrogenation, crushing and dehydrogenation treatment on the clean waste obtained in the step (1);
(3) passivating the powder obtained in the step (2) in a certain atmosphere to obtain a final powder product;
(4) the powder particle size and oxygen content were tested and left in air for a period of time to compare the change in oxygen content.
2. The method for preparing fine-grained low-oxygen powder from titanium and titanium alloy cutting waste according to claim 1, wherein the cleaning solvent in step (1) is an organic solvent or a weak acid, in particular acetone or dilute hydrochloric acid.
3. The method for preparing fine-grained low-oxygen powder from titanium and titanium alloy cutting waste material as claimed in claim 1, wherein the hydrotreating temperature in step (2) is 500-750 ℃ and the time is 2-6 h; the dehydrogenation treatment temperature is 500-800 ℃, and the time is 2-5 h.
4. The method for preparing fine-grained low-oxygen powder from titanium and titanium alloy cutting waste according to claim 1, wherein the passivation treatment atmosphere in the step (3) is a mixed atmosphere of argon and oxygen with an oxygen content of not more than 10%, the passivation temperature is not higher than 300 ℃, and the passivation time is not longer than 5 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010044236.0A CN111112628A (en) | 2020-01-15 | 2020-01-15 | Method for preparing fine-grained low-oxygen titanium and titanium alloy powder by using cutting waste |
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| CN202010044236.0A CN111112628A (en) | 2020-01-15 | 2020-01-15 | Method for preparing fine-grained low-oxygen titanium and titanium alloy powder by using cutting waste |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111644610A (en) * | 2020-05-13 | 2020-09-11 | 西南科技大学 | Method for reducing oxygen content in titanium powder |
| CN112941365A (en) * | 2021-01-25 | 2021-06-11 | 北京科技大学 | Method for preparing high-performance powder metallurgy titanium and titanium alloy by recycling residual titanium |
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| CN101164723A (en) * | 2007-10-11 | 2008-04-23 | 宝鸡富士特钛业有限公司 | Method for preparing high-purification ultrafine titanium powder for aviation |
| CN101568398A (en) * | 2006-12-22 | 2009-10-28 | 国际钛粉有限责任公司 | Direct passivation of metal powder |
| US20130315773A1 (en) * | 2012-05-24 | 2013-11-28 | Advance Materials Products, Inc. (Adma Products, Inc.) | Method of Manufacturing Pure Titanium Hydride Powder and Alloyed Titanium Hydride Powders By Combined Hydrogen-Magnesium Reduction of Metal Halides |
| KR20140040476A (en) * | 2012-09-26 | 2014-04-03 | 한국기계연구원 | The fabrication method of spherical titanium powder and the spherical titanium powder thereby |
| CN104325147A (en) * | 2014-11-25 | 2015-02-04 | 北京康普锡威科技有限公司 | In-situ passivation method for preparing spherical brazing powder through atomization |
| CN106955996A (en) * | 2017-05-18 | 2017-07-18 | 江门富祥电子材料有限公司 | The method and apparatus that a kind of tantalum powder is passivated completely |
-
2020
- 2020-01-15 CN CN202010044236.0A patent/CN111112628A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101568398A (en) * | 2006-12-22 | 2009-10-28 | 国际钛粉有限责任公司 | Direct passivation of metal powder |
| CN101164723A (en) * | 2007-10-11 | 2008-04-23 | 宝鸡富士特钛业有限公司 | Method for preparing high-purification ultrafine titanium powder for aviation |
| US20130315773A1 (en) * | 2012-05-24 | 2013-11-28 | Advance Materials Products, Inc. (Adma Products, Inc.) | Method of Manufacturing Pure Titanium Hydride Powder and Alloyed Titanium Hydride Powders By Combined Hydrogen-Magnesium Reduction of Metal Halides |
| KR20140040476A (en) * | 2012-09-26 | 2014-04-03 | 한국기계연구원 | The fabrication method of spherical titanium powder and the spherical titanium powder thereby |
| CN104325147A (en) * | 2014-11-25 | 2015-02-04 | 北京康普锡威科技有限公司 | In-situ passivation method for preparing spherical brazing powder through atomization |
| CN106955996A (en) * | 2017-05-18 | 2017-07-18 | 江门富祥电子材料有限公司 | The method and apparatus that a kind of tantalum powder is passivated completely |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111644610A (en) * | 2020-05-13 | 2020-09-11 | 西南科技大学 | Method for reducing oxygen content in titanium powder |
| CN112941365A (en) * | 2021-01-25 | 2021-06-11 | 北京科技大学 | Method for preparing high-performance powder metallurgy titanium and titanium alloy by recycling residual titanium |
| CN112941365B (en) * | 2021-01-25 | 2022-03-04 | 北京科技大学 | Method for preparing high-performance powder metallurgy titanium and titanium alloy by recycling residual titanium |
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Application publication date: 20200508 |