CN111185592A - Method for preparing high-performance powder metallurgy titanium and titanium alloy products by solid-phase deoxidization - Google Patents
Method for preparing high-performance powder metallurgy titanium and titanium alloy products by solid-phase deoxidization Download PDFInfo
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- CN111185592A CN111185592A CN202010112994.1A CN202010112994A CN111185592A CN 111185592 A CN111185592 A CN 111185592A CN 202010112994 A CN202010112994 A CN 202010112994A CN 111185592 A CN111185592 A CN 111185592A
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- titanium
- powder
- titanium alloy
- ticl
- sintering
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000010936 titanium Substances 0.000 title claims abstract description 41
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 40
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000004663 powder metallurgy Methods 0.000 title claims abstract description 20
- 239000007790 solid phase Substances 0.000 title claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 28
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000001301 oxygen Substances 0.000 claims abstract description 21
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 21
- 229910010068 TiCl2 Inorganic materials 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 238000009694 cold isostatic pressing Methods 0.000 claims description 10
- 239000011812 mixed powder Substances 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229920001971 elastomer Polymers 0.000 claims description 3
- 239000005060 rubber Substances 0.000 claims description 3
- 239000000741 silica gel Substances 0.000 claims description 3
- 229910002027 silica gel Inorganic materials 0.000 claims description 3
- 238000005056 compaction Methods 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- 229940123973 Oxygen scavenger Drugs 0.000 abstract description 4
- 239000012071 phase Substances 0.000 abstract description 4
- 230000001737 promoting effect Effects 0.000 abstract description 4
- 238000000280 densification Methods 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 238000006479 redox reaction Methods 0.000 abstract description 2
- 238000007493 shaping process Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 14
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
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- B22F1/0003—
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Powder Metallurgy (AREA)
Abstract
A method for preparing high-performance powder metallurgy titanium and titanium alloy by solid-phase deoxidization belongs to the field of powder metallurgy titanium. The invention provides a method for preparing TiCl2As titanium powder oxygen scavenger, TiCl is used2Mixing with titanium powder, shaping and sintering to obtain high-performance titanium product. In the sintering process, TiCl2Oxidation-reduction reaction is carried out on the titanium powder and the oxide film on the surface to generate TiClxOyThe titanium matrix is removed in a gaseous form without producing solid phase impurity particles, without introducing a second phase to hinder sintering, and TiClxOyThe method is favorable for breaking oxide films on the surfaces of the titanium powder, thereby improving the sintering activity of the titanium powder and promoting densification sintering, so that the titanium product with low oxygen and high density is obtained, and the titanium product has excellent comprehensive mechanical properties. The method provides a new idea for deoxidizing the powder metallurgy titanium and the titanium alloy, and is beneficial to promoting the industrial development of the low-cost powder metallurgy titanium and the titanium alloy.
Description
Technical Field
The invention belongs to the field of powder metallurgy titanium, and provides a method for preparing high-performance powder metallurgy titanium and titanium alloy by solid-phase deoxidization.
Background
Because titanium and titanium alloy have poor processability and low material utilization rate, the processing cost is high, and the near-net forming technology has attracted extensive research interest and application emphasis. The powder metallurgy technology can directly prepare the titanium alloy product with the final shape, avoids the links of hot processing, deep processing and the like of titanium, and greatly reduces the preparation and processing cost of the titanium alloy product. However, high oxygen content is one of the challenges currently faced by powder metallurgy titanium products, with a maximum critical oxygen content of 3200ppm in the titanium product. The oxygen in the titanium product is mainly derived from the oxide film on the surface of the powder and the oxygen increment in the forming and sintering process. The oxygen content of the prior commercially available hydrogenated and dehydrogenated titanium powder is about 2500-5000ppm, and the price is 70-200 yuan/Kg, but the price of the high-purity titanium powder with the oxygen content within 1000-2000ppm is more than 300 yuan/Kg. Therefore, how to realize oxygen removal of titanium powder is one of the major research directions in powder metallurgy of titanium and titanium alloy.
At present, rare earth elements are generally used as oxygen scavengers to improve the influence of over-high oxygen content on the mechanical properties of materials, and generally form second-phase particles with oxygen impurity atoms to purify the surfaces of the particles. However, since the solid solubility of the rare earth element in the titanium alloy is low, and intermetallic compounds do not exist generally, the sintering compactness, strength and elongation are greatly reduced after the content of the rare earth element is too high, so that the amount of the added rare earth is generally less than 1 wt.%, the oxygen removal effect is limited, the price of the rare earth element is expensive, and the cost of the purifying agent is high.
In order to realize surface purification and deoxidization of titanium powder, the invention provides a method for preparing high-performance powder metallurgy titanium and titanium alloy by solid-phase deoxidizationThe method of (1). With TiCl2As oxygen scavenger, TiCl2Mixing with titanium powder, and sintering while TiCl2Carrying out oxidation-reduction reaction with titanium powder and an oxide film on the surface of the powder to generate gaseous TiClxOyCompound of TiClxOyThe matrix is removed in a gaseous state, so that the purpose of reducing the oxygen content is achieved, no impurities are generated in the sintered titanium matrix, and a second phase cannot be introduced to hinder sintering. Thus, TiCl2The content can be properly increased to remove the oxide film and the adsorbed oxygen atoms on the surface of the titanium powder to the maximum extent, and the functions of purifying the surface of the powder particles and promoting sintering densification are achieved.
Disclosure of Invention
The invention aims to provide a method for preparing high-performance powder metallurgy titanium and titanium alloy by solid-phase deoxidization, which adopts TiCl2As oxygen scavenger, TiCl2Mixing with titanium powder, shaping and sintering to obtain high-performance titanium product. TiCl in the sintering process2Reacting with titanium powder and surface oxide film to generate gaseous TiCl4And TiClxOy. On one hand, the method is beneficial to breaking an oxide film on the surface of titanium powder and improving the sintering activity of the powder, thereby being beneficial to sintering densification; on the other hand, the product is removed in a gaseous form, so that the oxygen content in the sintered titanium and the titanium alloy is reduced, no impurity is generated, and the mechanical property of the titanium product is finally ensured.
In order to obtain the method for preparing the high-performance powder metallurgy titanium and titanium alloy product by solid-phase deoxidization, the method is characterized by comprising the following steps of: TiCl (titanium dioxide)2And the titanium or titanium alloy product comprises the following components in percentage by weight: 1 to 10 wt.% TiCl2And the balance of titanium or titanium alloy powder, and the specific preparation steps are as follows:
(1) TiCl meeting the requirements of the formula2And titanium powder are put into a mixing tank in a glove box protected by argon gas, and then are mixed for 1 to 24 hours on a mixer to obtain uniform mixed powder;
(2) putting the mixed powder into a cold isostatic pressing sheath in a glove box protected by argon gas for compaction, vacuumizing and sealing, and then performing cold isostatic pressing at the pressing pressure of 100-600MPa for 1-4min to obtain a pressed compact sample;
(3) and placing the pressed compact sample into a sintering furnace for argon or vacuum sintering, firstly preserving the heat for 60-120min at 850 ℃ with 500 plus materials, and then preserving the heat for 1-4h at 1350 ℃ with 1150 plus materials to finally obtain the high-performance titanium product part.
Further, the titanium powder in the step (1) is various commercially available pure titanium powder or titanium alloy powder.
Further, the cold isostatic pressing sheath in the step (2) is an elastic sheath made of polyurethane, rubber, silica gel and the like.
Further, the vacuum sintering is carried out in the step (3) with the vacuum degree of 10-3-10-2Pa。
The invention has the advantages that:
1. with TiCl2The solid-phase deoxidant can break an oxide film on the surface of titanium powder, reduce the oxygen content in a sintered titanium product, is favorable for increasing the sintering driving force on the surface of the titanium powder, improves the sintering activity, is easy to obtain the titanium product with low oxygen and high density, and has excellent comprehensive mechanical properties.
2、TiCl2The reaction product generated with the titanium powder is removed in a gas form, no impurity is generated, a second phase is not introduced to hinder sintering, and adverse effects on sintering performance are reduced.
3. By TiCl2Purifying the surface of titanium powder, and improving TiCl because the reaction product has no negative effect2The content of the deoxidant can play the purifying effect of the deoxidant to the maximum extent.
4、TiCl2The deoxidant has low price and simple preparation process, is beneficial to expanding the application range of the titanium powder with high oxygen content and low cost, and further reduces the preparation cost of the titanium alloy.
5. Provides a new idea for deoxidizing powder metallurgy titanium and titanium alloy, and is beneficial to promoting the industrial development of low-cost powder metallurgy titanium and titanium alloy.
Detailed Description
Example 1:
the adhesive is prepared from the following components in percentage by mass: 4 wt.% TiCl2The balance being hydrogenationDehydrogenated pure titanium powder (HDH-Ti), wherein the particle size D of the HDH-Ti5015 μm, oxygen content 3500 ppm. The preparation method comprises the following specific steps:
(1) TiCl meeting the requirements of the formula2Mixing the powder and HDH-Ti under the protection of argon atmosphere in a glove box, and mixing for 15 hours on a mixer to obtain uniform mixed powder;
(2) putting the mixed powder into a cold isostatic pressing silica gel sheath in an argon-protected glove box, compacting, vacuumizing, sealing, and performing cold isostatic pressing at a pressing pressure of 300MPa for 2min to obtain a pressed compact sample;
(3) putting the pressed compact sample into a sintering furnace for vacuum sintering, wherein the vacuum degree is 10-3And Pa, firstly preserving the heat at 600 ℃ for 60min, and then preserving the heat at 1170 ℃ for 1h to finally obtain the high-performance pure titanium part.
Example 2:
the adhesive is prepared from the following components in percentage by mass: 3 wt.% TiCl2The balance being HDH-TC4 titanium alloy powder, wherein the particle diameter D of HDH-TC45030 μm and an oxygen content of 2500 ppm. The preparation method comprises the following specific steps:
(1) TiCl meeting the requirements of the formula2Mixing with HDH-TC4 under the protection of argon atmosphere in a glove box, and mixing for 10h on a mixer to obtain uniform mixed powder;
(2) putting the mixed powder into a cold isostatic pressing rubber sheath in an argon-protected glove box, compacting, vacuumizing, sealing, and performing cold isostatic pressing at a pressing pressure of 400MPa for 1min to obtain a pressed compact sample;
(3) and (3) placing the pressed compact sample into a sintering furnace for argon sintering, preserving heat at 750 ℃ for 90min, and preserving heat at 1250 ℃ for 1.5h to finally obtain the high-performance TC4 titanium alloy part.
Claims (4)
1. A method for preparing high-performance powder metallurgy titanium and titanium alloy products by solid-phase deoxidization is characterized in that: the titanium product component is prepared from the following components in percentage by weight: 1 to 10 wt.% TiCl2The balance being titanium or titanium alloy powder; the preparation method comprises the following specific steps:
(1) ti meeting the formula requirementsCl2And titanium or titanium alloy powder are put into a mixing tank in an argon-protected glove box, and then are mixed for 1 to 24 hours on a mixer to obtain uniform mixed powder;
(2) putting the mixed powder into a cold isostatic pressing sheath in a glove box protected by argon gas for compaction, vacuumizing and sealing, and then performing cold isostatic pressing at the pressing pressure of 100-600MPa for 1-4min to obtain a pressed compact sample;
(3) and placing the pressed compact sample into a sintering furnace for argon or vacuum sintering, firstly preserving the heat for 60-120min at 850 ℃ with 500 plus materials, and then preserving the heat for 1-4h at 1350 ℃ with 1150 plus materials to finally obtain the high-performance titanium product part.
2. The method for preparing high-performance powder metallurgy titanium and titanium alloy products by solid-phase oxygen removal according to claim 1, characterized in that: the titanium powder in the step (1) is various commercially available pure titanium powder or titanium alloy powder.
3. The method for preparing high-performance powder metallurgy titanium and titanium alloy by solid-phase oxygen removal according to claim 1, characterized in that: the cold isostatic pressing sheath in the step (2) is a polyurethane, rubber or silica gel elastic sheath.
4. The method for preparing high-performance powder metallurgy titanium and titanium alloy by solid-phase oxygen removal according to claim 1, characterized in that: vacuum sintering is carried out in the step (3), the vacuum degree is 10-3-10-2Pa。
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| CN202010112994.1A CN111185592B (en) | 2020-02-24 | 2020-02-24 | Method for preparing high-performance powder metallurgy titanium and titanium alloy products by solid-phase deoxidization |
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| CN202010112994.1A CN111185592B (en) | 2020-02-24 | 2020-02-24 | Method for preparing high-performance powder metallurgy titanium and titanium alloy products by solid-phase deoxidization |
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| CN111185592A true CN111185592A (en) | 2020-05-22 |
| CN111185592B CN111185592B (en) | 2021-04-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111957972A (en) * | 2020-07-31 | 2020-11-20 | 石家庄金钛净化设备有限公司 | Preparation method of titanium filter element anti-corrosion film |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023250363A1 (en) * | 2022-06-21 | 2023-12-28 | Nutech Ventures | Titanium alloy powder reconditioning for 3d additive manufacturing |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59146918A (en) * | 1983-02-10 | 1984-08-23 | Toyo Soda Mfg Co Ltd | Production of double carbide |
| CN1852997A (en) * | 2003-09-19 | 2006-10-25 | 思研（Sri）国际顾问与咨询公司 | Methods and apparatuses for producing metallic compositions via reduction of metal halides |
| CN106507829B (en) * | 2003-09-30 | 2012-01-18 | 西北有色金属研究院 | A kind of powder metallurgy process of titanium alloy |
| CN104736273A (en) * | 2012-06-06 | 2015-06-24 | Csir公司 | Process for the production of crystalline titanium powder |
| US10245642B2 (en) * | 2015-02-23 | 2019-04-02 | Nanoscale Powders LLC | Methods for producing metal powders |
| CN109988940A (en) * | 2019-04-16 | 2019-07-09 | 上海材料研究所 | A kind of rare earth modified 3D printing hyperoxia titanium valve and preparation method |
-
2020
- 2020-02-24 CN CN202010112994.1A patent/CN111185592B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59146918A (en) * | 1983-02-10 | 1984-08-23 | Toyo Soda Mfg Co Ltd | Production of double carbide |
| CN1852997A (en) * | 2003-09-19 | 2006-10-25 | 思研（Sri）国际顾问与咨询公司 | Methods and apparatuses for producing metallic compositions via reduction of metal halides |
| CN106507829B (en) * | 2003-09-30 | 2012-01-18 | 西北有色金属研究院 | A kind of powder metallurgy process of titanium alloy |
| CN104736273A (en) * | 2012-06-06 | 2015-06-24 | Csir公司 | Process for the production of crystalline titanium powder |
| US10245642B2 (en) * | 2015-02-23 | 2019-04-02 | Nanoscale Powders LLC | Methods for producing metal powders |
| CN109988940A (en) * | 2019-04-16 | 2019-07-09 | 上海材料研究所 | A kind of rare earth modified 3D printing hyperoxia titanium valve and preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111957972A (en) * | 2020-07-31 | 2020-11-20 | 石家庄金钛净化设备有限公司 | Preparation method of titanium filter element anti-corrosion film |
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