CN111151762A - Preparation method of low-cost fine-grained low-oxygen titanium and titanium alloy powder - Google Patents
Preparation method of low-cost fine-grained low-oxygen titanium and titanium alloy powder Download PDFInfo
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- CN111151762A CN111151762A CN202010044238.XA CN202010044238A CN111151762A CN 111151762 A CN111151762 A CN 111151762A CN 202010044238 A CN202010044238 A CN 202010044238A CN 111151762 A CN111151762 A CN 111151762A
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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Abstract
The invention discloses a preparation method of low-cost fine-grained low-oxygen titanium and titanium alloy powder, belonging to the technical field of powder metallurgy powder preparation. The method takes titanium sponge and alloy powder as raw materials, and obtains a final product through the processes of hydrogenation, crushing, dehydrogenation, pre-alloying, passivation and the like. The method adopts the hydrogenation dehydrogenation method to prepare the titanium and the titanium alloy powder, so that the cost is low; after crushing, dehydrogenation and pre-alloying treatment, the titanium alloy powder without segregation and with uniform components can be obtained; the surface oxidation layer state and the oxygen content of the powder particles are controlled by passivation treatment, so that the oxygen content of less than or equal to 0.2wt percent and the particle size (D) can be prepared50) 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 low-cost fine-grained low-oxygen titanium and titanium alloy powder.
Background
Titanium and titanium alloy have the advantages of low density, high strength, good biocompatibility and the like, and have wide application in the fields of aerospace, biomedicine, machinery and the like. Because titanium and titanium alloy have high melting points and are difficult to process, the traditional ingot metallurgy process has high manufacturing cost, and the application and the industrial development of the ingot metallurgy process are limited. The powder metallurgy process can solve the problem of smelting high-melting-point metals, has the advantages of near-net-shape forming, high material utilization rate, fine and uniform structure, excellent performance and the like, and provides an effective way for preparing titanium products with low cost and high performance.
In the titanium and titanium alloy powder metallurgy process, a high-quality titanium powder raw material is a key primary factor for obtaining a high-performance product. At present, the hydrogenation dehydrogenation method (HDH) for preparing titanium and titanium alloy powder has the advantages of low cost, controllable powder granularity and the like, but because the titanium and titanium alloy powder has high activity and is easy to oxidize, the powder is difficult to avoid being exposed in air in the subsequent use process, the oxygen content of powder impurities is increased, and the material performance is influenced. Therefore, how to control the oxygen content of hydrogenated titanium hydride and titanium alloy powder and improve the oxidation resistance of the powder is a problem to be solved.
Disclosure of Invention
The invention aims to provide a preparation method of titanium and titanium alloy powder with low cost, fine granularity and low oxygen content. Titanium sponge is used as a raw material, titanium and titanium alloy powder is prepared by a hydrogenation dehydrogenation method (HDH), and the titanium and titanium alloy powder is treated by a passivation technology, so that the oxygen content of the powder is controlled, and the oxidation resistance of the powder is improved.
The invention comprises the following specific steps:
(1) carrying out hydrogenation treatment on titanium sponge serving as a raw material;
(2) crushing the titanium hydride obtained in the step (1) to obtain powder with required granularity; aiming at the preparation of titanium alloy powder, the titanium hydride obtained in the step (1) is mixed with other prealloy or element powder according to the components of the prepared titanium alloy, and then crushing and mixing are carried out;
(3) carrying out dehydrogenation treatment on the powder obtained in the step (2); aiming at the preparation of titanium alloy powder, carrying out dehydrogenation treatment on the powder obtained in the step (2) and pre-alloying simultaneously;
(4) passivating the powder obtained in the step (3) in a certain atmosphere to obtain a final powder product;
(5) and testing the granularity and the oxygen content of the powder, and standing the powder in the air for a period of time to evaluate the oxidation resistance of the powder.
Further, the hydrogenation temperature in the step (1) is 500-800 ℃, and the hydrogenation treatment time is 2-7 h.
Further, the crushing and screening in the step (2) are carried out under a protective atmosphere of argon to prevent the oxidation of the powder.
Further, the dehydrogenation treatment temperature in the step (3) is 650-800 ℃, and the time is 2-6 h.
Further, the passivation treatment atmosphere in the step (4) 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) titanium sponge is used as a raw material, and a hydrogenation dehydrogenation method is adopted to prepare titanium and titanium alloy powder, so that the powder granularity is controllable, and the cost is low.
(2) Through crushing, dehydrogenation and alloying, the alloy powder without segregation and with uniform components can be obtained, and the energy consumption is low.
(3) The passivation technology is adopted for treatment, so that the oxide phase and the thickness of an oxide layer on the surface of titanium powder particles can be controlled, and the titanium and titanium alloy powder with low oxygen content and excellent oxidation resistance can be obtained.
(4) 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 titanium and titanium alloy powder with the particle size less than 50 mu m is stable and unchanged after the powder is placed in the air at room temperature for one week.
Drawings
FIG. 1 scanning electron micrograph of pure titanium powder subjected to hydrogenation dehydrogenation and passivation treatment prepared in example 1,
FIG. 2 scanning electron micrograph of hydrogenated dehydrogenated passivated titanium alloy powder prepared in example 5.
Detailed Description
Example 1
Weighing 5kg of sponge titanium powder, loading into a hydrogenation furnace, and vacuumizing to 1 x 10-3Pa, filling high-purity hydrogen to carry out three-time furnace washing, then heating to 700 ℃ at the speed of 15 ℃/min under the hydrogen atmosphere, and preserving heat for 5 hours to complete hydrogenation reaction to obtain titanium hydride powder; 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 deg.C at a speed of 10 deg.C/min in Pa vacuum furnace for dehydrogenation, and pumping out hydrogen generated by dehydrogenation reaction to maintain vacuum degree at 1 × 10-3Pa, after dehydrogenation reaction for 3 hours, cooling to room temperature, introducing a mixed gas of argon with the oxygen content of 1% and oxygen at the flow rate of 0.8L/min for passivation treatment for 3 hours, 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 15 microns and the oxygen content of 0.15 wt.%, and taking 50g of powder, placing the powder in the air for 168 hours and keeping the oxygen content of 0.15 wt.%.
Example 2
Weighing 10kg of sponge titanium powder, loading into a hydrogenation furnace, and vacuumizing to 1 x 10-3Pa, filling high-purity hydrogen to carry out three-time furnace washing, then heating to 710 ℃ at the speed of 10 ℃/min under the hydrogen atmosphere, and preserving heat for 5 hours to complete hydrogenation reaction to obtain titanium hydride powder; 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 760 deg.C at a rate of 15 deg.C/min in a Pa vacuum furnace for dehydrogenation to obtainTo maintain the degree of vacuum at 1X 10-3Pa, carrying out dehydrogenation reaction for 5 hours, cooling to room temperature, introducing a mixed gas of argon with the oxygen content of 5% and oxygen at the flow rate of 1L/min for passivation for 3 hours, taking powder from a vacuum glove box, detecting the oxygen content, carrying out vacuum packaging and storing to obtain powder with the particle size of 50 microns and the oxygen content of 0.06 wt.%, and taking 50g of powder, and placing the powder in the air for 240 hours to obtain the powder with the oxygen content of 0.07 wt.%.
Example 3
Weighing 20kg of sponge titanium powder, loading into a hydrogenation furnace, and vacuumizing to 1 x 10-3Pa, filling high-purity hydrogen to carry out three-time furnace washing, then heating to 680 ℃ at the speed of 10 ℃/min under the hydrogen atmosphere, preserving heat for 5.5h, and finishing hydrogenation reaction to obtain titanium hydride powder; 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 deg.C at a speed of 15 deg.C/min in Pa vacuum furnace for dehydrogenation, and pumping out hydrogen generated by dehydrogenation reaction to maintain vacuum degree of 1 × 10-3Pa, carrying out dehydrogenation reaction for 5 hours, cooling to room temperature, introducing a mixed gas of argon with the oxygen content of 3% and oxygen at the flow rate of 1L/min for passivation for 4 hours, 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 powder, placing in the air for 240 hours and the oxygen content of 0.11 wt.%.
Example 4
Weighing 10kg of sponge titanium powder, loading into a hydrogenation furnace, and vacuumizing to 1 x 10-3Pa, filling high-purity hydrogen to carry out three-time furnace washing, then heating to 680 ℃ at the speed of 10 ℃/min under the hydrogen atmosphere, preserving heat for 5.5h, and finishing hydrogenation reaction to obtain titanium hydride powder; 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 deg.C at a speed of 15 deg.C/min in Pa vacuum furnace for dehydrogenation, and pumping out hydrogen generated by dehydrogenation reaction to maintain vacuum degree of 1 × 10-3Pa, dehydrogenation reaction for 5h, cooling to room temperature, and introducing argon with oxygen content of 7% at flow rate of 1.5L/minPassivating the gas mixture of gas and oxygen for 3.5h, taking powder in a vacuum glove box, detecting the oxygen content, vacuum packaging and storing to obtain powder with the particle size of 10 μm and the oxygen content of 0.16 wt.%, and taking 50g of powder and placing in the air for 240h to obtain the powder with the oxygen content of 0.17 wt.%.
Example 5
Weighing 5kg of titanium sponge powder, loading the titanium sponge powder into a hydrogenation furnace, vacuumizing, washing the hydrogenation furnace by using high-purity hydrogen, heating to 700 ℃ at the speed of 15 ℃/min, and preserving heat for 5 hours to perform hydrogenation reaction to obtain titanium hydride powder; cooling to room temperature, adding AlV master alloy powder for mixing, crushing, placing the treated powder into a vacuum furnace, heating to 750 ℃ at the speed of 10 ℃/min for dehydrogenation, pumping out hydrogen generated by dehydrogenation reaction to maintain the vacuum degree, cooling to room temperature after dehydrogenation reaction for 3h, introducing a mixed gas of argon with the oxygen content of 6% and oxygen at the flow rate of 0.8L/min for passivation for 5h, taking powder, detecting the oxygen content, carrying out vacuum packaging and storing, wherein the particle size of the powder is 30 mu m, the oxygen content is 0.10 wt%, taking 50g of the powder, placing in the air for 168h, and then detecting the oxygen content to be 0.11 wt%.
Example 6
Weighing 10kg of titanium sponge powder, loading into a hydrogenation furnace, vacuumizing, washing the furnace by using high-purity hydrogen, heating to 720 ℃ at the speed of 15 ℃/min, and preserving heat for 5 hours to perform hydrogenation reaction to obtain titanium hydride powder; cooling to room temperature, adding Al powder to mix, crushing, placing the treated powder into a vacuum furnace, heating to 760 ℃ at the speed of 10 ℃/min for dehydrogenation, pumping out hydrogen generated by dehydrogenation reaction to maintain the vacuum degree, cooling to room temperature after 3h of dehydrogenation reaction, introducing mixed gas of argon with the oxygen content of 4% and oxygen at the flow rate of 1L/min for passivation for 3h, taking powder, detecting the oxygen content, carrying out vacuum packaging and storing, wherein the particle size of the powder is 50 mu m, the oxygen content is 0.07 wt%, taking 50g of the powder, placing in the air for 240h, and then detecting the oxygen content, and finally obtaining the oxygen content of 0.07 wt%.
Example 7
Weighing 15kg of titanium sponge powder, loading into a hydrogenation furnace, vacuumizing, washing the hydrogenation furnace by using high-purity hydrogen, heating to 710 ℃ at a heating rate of 10 ℃/min, and preserving heat for 5 hours to perform hydrogenation reaction to obtain titanium hydride powder; cooling to room temperature, adding AlMn master alloy powder for mixing, crushing, placing the treated powder into a vacuum furnace, heating to 760 ℃ at the speed of 10 ℃/min for dehydrogenation, pumping out hydrogen generated by dehydrogenation reaction to keep the vacuum degree, cooling to room temperature after dehydrogenation reaction for 3.5h, introducing a mixed gas of argon and oxygen with the oxygen content of 3% at the flow rate of 1L/min for passivation for 3h, taking powder, detecting the oxygen content, carrying out vacuum packaging and storing, wherein the particle size of the powder is 15 mu m, the oxygen content is 0.15 wt%, taking 50g of the powder, placing in the air for 240h, and then detecting the oxygen content, and the detected oxygen content is 0.16 wt%.
Example 8
Weighing 5kg of titanium sponge powder, loading into a hydrogenation furnace, vacuumizing, washing the hydrogenation furnace by using high-purity hydrogen, heating to 690 ℃ at a heating rate of 10 ℃/min, and preserving heat for 5 hours to perform hydrogenation reaction to obtain titanium hydride powder; cooling to room temperature, adding AlNb master alloy powder for mixing, crushing, placing the treated powder into a vacuum furnace, heating to 730 ℃ at a speed of 10 ℃/min for dehydrogenation, pumping hydrogen generated by dehydrogenation reaction to maintain vacuum degree, cooling to room temperature after dehydrogenation reaction for 3h, introducing mixed gas of argon and oxygen with the oxygen content of 4% at a flow rate of 1.5L/min for passivation for 3.5h, taking powder, detecting the oxygen content, carrying out vacuum packaging and storing, wherein the particle size of the powder is 35 mu m, the oxygen content is 0.11 wt%, taking 50g of the powder, placing in the air for 168h, and then detecting the oxygen content, and the detected oxygen content is 0.12 wt%.
Claims (5)
1. A method for preparing low-cost fine-grained low-oxygen titanium and titanium alloy powder is characterized by comprising the following preparation steps
(1) Carrying out hydrogenation treatment on titanium sponge serving as a raw material;
(2) crushing the titanium hydride obtained in the step (1) to obtain powder with required granularity; aiming at the preparation of titanium alloy powder, the titanium hydride obtained in the step (1) is mixed with other prealloy or element powder according to the components of the prepared titanium alloy, and then crushing and mixing are carried out;
(3) carrying out dehydrogenation treatment on the powder obtained in the step (2); aiming at the preparation of titanium alloy powder, carrying out dehydrogenation treatment on the powder obtained in the step (2) and pre-alloying simultaneously;
(4) passivating the powder obtained in the step (3) in a certain atmosphere to obtain a final powder product;
(5) and testing the granularity and the oxygen content of the powder, and standing the powder in the air for a period of time to evaluate the oxidation resistance of the powder.
2. The method for preparing low-cost fine-grained titanium suboxide and titanium alloy powder as claimed in claim 1, wherein the hydrogenation temperature in step (1) is 500-.
3. The method of claim 1 wherein the step (2) of crushing and sieving is performed under a protective atmosphere of argon to prevent oxidation of the powder.
4. The method for preparing low-cost fine-grained titanium suboxide and titanium alloy powder as claimed in claim 1, wherein the dehydrogenation treatment temperature in step (3) is 650-.
5. The method for preparing low-cost fine-grained low-oxygen titanium and titanium alloy powder according to claim 1, wherein the passivation treatment atmosphere in the step (4) 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 more than 5 h.
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| WO2022021488A1 (en) * | 2020-07-29 | 2022-02-03 | 北京科技大学 | High-strength and high-plasticity titanium-based composite material and preparation method therefor |
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