CN112941366A - Method for preparing high-performance powder metallurgy titanium and titanium alloy from superfine titanium powder - Google Patents
Method for preparing high-performance powder metallurgy titanium and titanium alloy from superfine titanium powder Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C14/00—Alloys based on titanium
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- 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]
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- 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
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- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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Abstract
A method for preparing high-performance powder metallurgy titanium and titanium alloy from superfine titanium powder belongs to the field of powder metallurgy titanium. The invention takes titanium sponge and zirconium hafnium sponge (oxygen fixing agent) as raw materials, the superfine hydrogenated dehydrogenation powder is obtained by hydrogenation, crushing and dehydrogenation processes after the raw materials are uniformly mixed, and the high-performance powder metallurgy titanium product can be obtained after forming and sintering. In the invention, the ultrafine powder is used for realizing the sintering full-compactness of the powder metallurgy titanium alloy, the grains are fine, in order to reduce the adverse effect of the high oxygen content in the ultrafine powder on the titanium matrix, zirconium and hafnium are used as oxygen fixing agents, and a Ti-Zr (Hf) -O ordered phase is formed with titanium and oxygen elements in the sintering process, so that the oxygen content in the titanium matrix is greatly reduced, the strengthening effect is simultaneously realized, and the mechanical property of the material is improved. The preparation method has the advantages of simple preparation process, capability of solving the problem of overhigh oxygen content of the superfine titanium powder without additional equipment, guarantee of the mechanical property of the final titanium product, suitability for large-scale industrial production and contribution to promoting the industrial development of powder metallurgy titanium.
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 from superfine titanium powder.
Background
Titanium and titanium alloy have low density, high strength, good corrosion resistance and heat resistance, can maintain the mechanical properties at relatively high service temperature, have excellent biocompatibility, are applied to the fields of aerospace, military oceans, medical chemical industry and the like, and gradually expand into the industries of energy sources, automobiles and the like. Titanium is abundant on earth, the abundance of earth crust is 0.61%, compared with metallic copper, the total resource amount is nearly 61 times of that of copper, but the yield is only 1/80 of copper. This is because titanium is highly reactive and chemically reactive with many elements and even refractories in conventional smelting processes, and therefore must be carried out under vacuum or inert atmosphere protection, and it is difficult to find a suitable condenser. The powder metallurgy technology with the near-net-shape forming advantage can avoid solid-liquid phase change during vacuum melting and reduce energy consumption, so that the method is an effective method for preparing low-cost high-performance titanium and titanium alloy in a short process.
However, titanium has high affinity to interstitial elements, the maximum critical content of oxygen in a titanium product is 3200ppm, the ductility of the material is rapidly reduced until the material is subjected to brittle fracture after the critical oxygen content is exceeded, the specific surface area of the powder is large, oxygen in the environment is easily adsorbed, and the oxygen content of the final product is too high to well meet the application performance requirement. In addition, how to densify is another problem which needs to be solved in the practical application of the powder metallurgy product, and the existence of the pores can cause the material to cause stress concentration in the practical application, become a crack source and finally cause the failure and fracture of the material. The sintering density can be improved by increasing the sintering temperature, but crystal grains can grow violently, and the final performance of the material is difficult to ensure. At present, the full densification of powder metallurgy titanium is mainly realized by adopting pressure sintering, such as hot isostatic pressing, hot-pressing sintering and the like, the sintering temperature can be reduced, the sintering time is shortened, and a titanium product with fine grains, high density and better mechanical property is obtained. But the method has high requirements on equipment, high processing cost, low production efficiency and small production scale, and is not easy to produce powder metallurgy titanium products with complex shapes.
The driving force for sintering the powder mainly comes from the specific surface energy of the powder, generally, the smaller the particle size of the powder, the more irregular the morphology, the larger the specific surface area, the higher the specific surface energy, the better the sinterability, but the higher the oxygen content, the oxygen adsorbed on the surface can not be removed in the subsequent process, and the mechanical properties of the final product are seriously affected. Therefore, how to solve the problem of overhigh oxygen in the superfine powder is the key for preparing the fully-compact high-performance powder metallurgy titanium product.
Disclosure of Invention
The invention aims to provide a method for preparing high-performance powder metallurgy titanium and titanium alloy from superfine titanium powder. The method takes titanium sponge and zirconium hafnium sponge (oxygen fixing agent) as raw materials, the superfine hydrogenated dehydrogenation powder is obtained by hydrogenation, crushing and dehydrogenation processes after the raw materials are uniformly mixed, and the high-performance powder metallurgy titanium product is obtained after forming and sintering. Firstly, Zr, Hf and Ti belong to the same group of elements, have similar chemical properties, are infinitely mutually soluble in a Ti matrix, and cannot hinder sintering and influence the compactness of a product. Meanwhile, in the sintering process, three elements of Ti, Zr (Hf) and O form an ordered phase, so that the oxygen content in the titanium matrix is reduced and the strengthening effect is achieved. In this case, even if the oxygen content in the powder metallurgy titanium product is higher than 3200ppm, the oxygen element in the titanium matrix is deprived by Zr and Hf elements to form a Ti-Zr (Hf) -O ordered phase, so that the oxygen content in the titanium matrix is greatly reduced and the material still shows excellent plasticity. In addition, by using the superfine titanium powder as a raw material, the full compactness of a sintered product can be realized by low-temperature sintering, and fine grains are ensured, so that the function of fine grain strengthening is achieved, and the strength of the material is further improved. In addition, the Zr content and the Hf content in the system can be regulated and controlled according to application requirements, oxygen in the superfine titanium powder is fixed to the maximum extent, the adverse effect of solid dissolved oxygen on the ductility of a titanium matrix is reduced, and high-performance powder metallurgy titanium and titanium alloy are obtained. The method has simple process, can solve the problem of overhigh oxygen content of the superfine titanium powder without additional equipment, ensures the mechanical property of the final titanium product, provides a new idea for oxygen fixation of powder metallurgy titanium and titanium alloy, and is favorable for promoting the industrialized development of the powder metallurgy titanium.
In order to obtain the method for preparing the high-performance powder metallurgy titanium and the titanium alloy by the superfine titanium powder, the method is characterized by comprising the following specific preparation steps of:
(1) weighing titanium sponge and zirconium hafnium sponge according to a mass ratio of 99.5:0.5-95:5, putting the weighed titanium sponge and zirconium hafnium sponge into a mixing tank, mixing for 0.5-2h, putting the mixture into a hydrogen furnace for hydrogenation treatment at a hydrogenation temperature of 350-;
(2) weighing the hydrogenated material and various alloy powders in the step (1) in proportion, then carrying out high-energy ball milling for 12-48h at a ball-to-material ratio of 4:1-10:1, and crushing to obtain superfine hydrogenated material powder;
(3) placing the superfine hydrogenated material powder in the step (2) into a vacuum sintering furnace for dehydrogenation treatment, wherein the vacuum degree is less than 1Pa, the dehydrogenation temperature is 800 ℃ and the temperature is kept for 4-10h, so as to obtain superfine hydrogenated and dehydrogenated titanium material powder;
(4) placing the superfine hydrogenated and dehydrogenated titanium material powder in the step (3) into a cold isostatic pressing sheath in a glove box protected by high-purity argon gas, compacting, sealing, and then carrying out cold isostatic pressing forming, wherein the pressing pressure is 200-600MPa, and the pressure maintaining time is 30-300s, so as to obtain a pressed compact sample;
(5) putting the pressed compact sample in the step (4) into a sintering furnace for argon or vacuum (the vacuum degree is 10)-3-10- 2Pa) sintering at the temperature of 1000-1150 ℃ and keeping the temperature for 2-5h to finally obtain the high-performance powder metallurgy titanium product.
Further, the hafnium zirconium sponge in the step (1) is one or a mixture of commercially available zirconium sponge and hafnium sponge.
Further, the various alloy powders in the step (2) are alloy powders required by various commercially available titanium alloy grades, the particle size of the powders is 50-500 μm, and the powders are proportioned according to the titanium alloy grades.
Furthermore, the grain size of the superfine hydrogenated material powder in the step (2) is less than or equal to 5 mu m.
Furthermore, the grain size of the superfine hydrogenated and dehydrogenated titanium powder in the step (3) is less than or equal to 5 mu m.
Further, the sheath in the step (4) is a polyurethane, rubber or silica gel elastic sheath.
Further, the high-performance powder metallurgy titanium product in the step (5) is not limited to various titanium alloy products, and also includes a pure titanium product.
The key points of the technology of the invention are as follows: (1) through a large number of experiments and by combining the oxygen content of the superfine titanium powder and the comprehensive performance of a final product, the mass percent of the sponge zirconium hafnium is determined to be 0.5-5 wt.%. (2) The superfine titanium powder is used as a raw material, and sintering can be carried out at low temperature to realize full compactness and achieve the fine grain strengthening effect. (3) In order to reduce the adverse effect of high oxygen content in the ultrafine powder on a titanium matrix, zirconium and hafnium are used as an oxygen fixing agent, and the characteristics that zirconium, hafnium and titanium have similar properties and can be dissolved in each other infinitely are utilized to fix oxygen in the titanium matrix to generate a Ti-Zr (Hf) -O ordered phase, so that the oxygen content in the matrix is reduced, the plasticity of the high-oxygen titanium alloy is ensured, the effect of strengthening the matrix is realized, and the Zr content and the Hf content in the system can be flexibly regulated and controlled to ensure that the oxygen content in the matrix is fixed to the maximum extent. (4) The high-performance titanium alloy product is prepared by a powder metallurgy process, the problem that the oxygen content of the superfine titanium powder is too high is effectively solved, full compactness can be realized by low-temperature sintering, fine crystal grains are ensured, the energy consumption is reduced, a new idea is provided for oxygen fixation of powder metallurgy titanium and titanium alloy, and the low-cost development of the titanium industry is facilitated.
The invention has the advantages that:
1. the invention solves the problem of overhigh oxygen content of the superfine titanium powder, provides a new idea for oxygen fixation of powder metallurgy titanium and titanium alloy, and is beneficial to promoting the industrialized development of the powder metallurgy titanium.
2. The properties of zirconium and hafnium are similar to those of titanium, and the zirconium and hafnium are infinitely mutually soluble in a Ti matrix, so that sintering is not hindered, and the compactness of a product is not influenced.
3. Zirconium hafnium is used as an oxygen fixing agent, and can form a Ti-Zr (Hf) -O ordered phase with titanium and oxygen elements in the sintering process, so that even if the oxygen content in the superfine titanium powder is higher, the zirconium hafnium element in the superfine titanium powder can greatly reduce the oxygen content in a titanium matrix, and simultaneously plays a role in strengthening and improving the mechanical property of the material.
4. The superfine titanium powder is used for realizing low-temperature sintering, so that the grains of the final product are fine, the grains are prevented from growing violently, the effect of fine grain strengthening can be achieved, and the strength of the material is further improved.
5. According to application requirements, the Zr content and the Hf content in the system can be flexibly regulated and controlled, oxygen in the superfine titanium powder is fixed to the maximum extent, adverse effects of dissolved oxygen on ductility of a titanium matrix are reduced, and high-performance powder metallurgy titanium and titanium alloy products are obtained.
6. The method has the advantages of simple preparation process, no need of additional equipment and process steps, strong applicability and suitability for large-scale industrial production.
Detailed Description
Example 1:
a method for preparing high-performance powder metallurgy titanium and titanium alloy from superfine titanium powder comprises the following specific preparation steps:
(1) weighing titanium sponge and zirconium sponge according to a mass ratio of 98:2, loading into a mixing tank, mixing for 1h, placing into a hydrogen furnace for hydrogenation treatment at a hydrogenation temperature of 600 ℃, and preserving heat for 5h to obtain a hydrogenated material;
(2) mixing the hydrogenated material in the step (1) with 6 wt.% of aluminum powder (200 mu m) and 4 wt.% of vanadium powder (100 mu m), performing high-energy ball milling for 24 hours at a ball-to-material ratio of 5:1, and crushing to obtain superfine hydrogenated material powder with the particle size of 4 mu m;
(3) placing the superfine hydrogenated material powder in the step (2) into a vacuum sintering furnace for dehydrogenation treatment, wherein the vacuum degree is less than 1Pa, the dehydrogenation temperature is 700 ℃, and the temperature is kept for 6 hours to obtain superfine hydrogenated and dehydrogenated material powder with the particle size of 4 mu m;
(4) putting the superfine hydrogenated and dehydrogenated material powder in the step (3) into a polyurethane cold isostatic pressing sheath in a glove box protected by high-purity argon gas, compacting, sealing, and then carrying out cold isostatic pressing forming, wherein the pressing pressure is 300MPa, and the pressure maintaining time is 180s, so as to obtain a pressed compact sample;
(5) putting the pressed compact sample in the step (4) into a sintering furnace for vacuum (the vacuum degree is 10)-3Pa), sintering at 1080 ℃, and keeping the temperature for 2h to finally obtain the high-performance powder metallurgy TC4 titanium alloy product.
Example 2:
a method for preparing high-performance powder metallurgy titanium and titanium alloy from superfine titanium powder comprises the following specific preparation steps:
(1) weighing titanium sponge and zirconium sponge according to a mass ratio of 96.5:3.5, putting the titanium sponge and the zirconium sponge into a mixing tank, mixing for 0.5h, putting the mixture into a hydrogen furnace for hydrogenation treatment at a hydrogenation temperature of 650 ℃, and keeping the temperature for 4h to obtain a hydrogenated material;
(2) carrying out high-energy ball milling on the hydrogenated material in the step (1), wherein the ball-material ratio is 8:1, the ball milling time is 18h, and crushing to obtain superfine hydrogenated material powder with the particle size of 2 mu m;
(3) placing the superfine hydrogenated material powder in the step (2) into a vacuum sintering furnace for dehydrogenation treatment, wherein the vacuum degree is less than 1Pa, the dehydrogenation temperature is 680 ℃, and the temperature is kept for 4 hours to obtain superfine hydrogenated and dehydrogenated material powder with the particle size of 2 mu m;
(4) putting the superfine hydrogenated and dehydrogenated material powder in the step (3) into a silica gel cold isostatic pressing sheath in a glove box protected by high-purity argon gas, compacting, sealing, and carrying out cold isostatic pressing forming, wherein the pressing pressure is 400MPa, and the pressure maintaining time is 90s, so as to obtain a pressed blank sample;
(5) and (4) placing the pressed compact sample in the step (4) into a sintering furnace for argon sintering, wherein the sintering temperature is 1020 ℃, and keeping the temperature for 2 hours to finally obtain the high-performance powder metallurgy titanium product.
Example 3:
a method for preparing high-performance powder metallurgy titanium and titanium alloy from superfine titanium powder comprises the following specific preparation steps:
(1) weighing titanium sponge, zirconium sponge and hafnium sponge according to a mass ratio of 98:2, wherein the ratio of zirconium sponge to hafnium sponge is 1:1, putting the materials into a mixing tank, mixing for 1.5h, putting the mixture into a hydrogen furnace for hydrogenation treatment at a hydrogenation temperature of 750 ℃, and preserving heat for 5h to obtain a hydrogenated material;
(2) mixing the hydrogenated material obtained in the step (1) with 8 wt.% of aluminum powder (100 mu m), 1 wt.% of molybdenum powder (200 mu m) and 1 wt.% of vanadium powder (300 mu m), carrying out high-energy ball milling, wherein the ball-to-material ratio is 7:1, the ball milling time is 36h, and crushing to obtain superfine hydrogenated material powder with the particle size of 3 mu m;
(3) placing the superfine hydrogenated material powder in the step (2) into a vacuum sintering furnace for dehydrogenation treatment, wherein the vacuum degree is less than 1Pa, the dehydrogenation temperature is 780 ℃, and the temperature is kept for 7 hours to obtain superfine hydrogenated and dehydrogenated material powder with the granularity of 3 mu m;
(4) putting the superfine hydrogenated and dehydrogenated material powder in the step (3) into a silica gel cold isostatic pressing sheath in a glove box protected by high-purity argon gas, compacting, sealing, and carrying out cold isostatic pressing for forming, wherein the pressing pressure is 200MPa, and the pressure maintaining time is 200s, so as to obtain a pressed blank sample;
(5) and (4) placing the pressed compact sample in the step (4) into a sintering furnace for argon sintering, wherein the sintering temperature is 1000 ℃, and preserving heat for 5 hours to finally obtain the high-performance powder metallurgy TA11 titanium alloy product.
Claims (7)
1. A method for preparing high-performance powder metallurgy titanium and titanium alloy from superfine titanium powder is characterized by comprising the following specific preparation steps:
(1) weighing titanium sponge and zirconium hafnium sponge according to a mass ratio of 99.5:0.5-95:5, putting the weighed titanium sponge and zirconium hafnium sponge into a mixing tank, mixing for 0.5-2h, putting the mixture into a hydrogen furnace for hydrogenation treatment at a hydrogenation temperature of 350-;
(2) weighing the hydrogenated material and various alloy powders in the step (1) in proportion, then carrying out high-energy ball milling for 12-48h at a ball-to-material ratio of 4:1-10:1, and crushing to obtain superfine hydrogenated material powder;
(3) placing the superfine hydrogenated material powder in the step (2) into a vacuum sintering furnace for dehydrogenation treatment, wherein the vacuum degree is less than 1Pa, the dehydrogenation temperature is 800 ℃ and the temperature is kept for 4-10h, so as to obtain superfine hydrogenated and dehydrogenated titanium material powder;
(4) placing the superfine hydrogenated and dehydrogenated titanium material powder in the step (3) into a cold isostatic pressing sheath in a glove box protected by high-purity argon gas, compacting, sealing, and then carrying out cold isostatic pressing forming, wherein the pressing pressure is 200-600MPa, and the pressure maintaining time is 30-300s, so as to obtain a pressed compact sample;
(5) putting the pressed compact sample in the step (4) into a sintering furnace for argon or vacuum (the vacuum degree is 10)-3-10-2Pa) sintering at the temperature of 1000-1150 ℃ and keeping the temperature for 2-5h to finally obtain the high-performance powder metallurgy titanium product.
2. The method for preparing high-performance powder metallurgy titanium and titanium alloy from ultrafine titanium powder according to claim 1, wherein the method comprises the following steps: the zirconium sponge hafnium in the step (1) is one or a mixture of commercially available zirconium sponge and hafnium sponge.
3. The method for preparing high-performance powder metallurgy titanium and titanium alloy from ultrafine titanium powder according to claim 1, wherein the method comprises the following steps: the various alloy powders in the step (2) are alloy powders required by various commercially available titanium alloy grades, the particle size of the powder is 50-500 mu m, and the weighing proportion is matched according to the titanium alloy grades.
4. The method for preparing high-performance powder metallurgy titanium and titanium alloy from ultrafine titanium powder according to claim 1, wherein the method comprises the following steps: the granularity of the superfine hydride powder in the step (2) is less than or equal to 5 mu m.
5. The method for preparing high-performance powder metallurgy titanium and titanium alloy from ultrafine titanium powder according to claim 1, wherein the method comprises the following steps: the granularity of the superfine hydrogenated and dehydrogenated titanium material powder in the step (3) is less than or equal to 5 mu m.
6. The method for preparing high-performance powder metallurgy titanium and titanium alloy from ultrafine titanium powder according to claim 1, wherein the method comprises the following steps: the sheath in the step (4) is a polyurethane, rubber or silica gel elastic sheath.
7. The method for preparing high-performance powder metallurgy titanium and titanium alloy from ultrafine titanium powder according to claim 1, wherein the method comprises the following steps: the high-performance powder metallurgy titanium product in the step (5) is not limited to various titanium alloy products, and also comprises a pure titanium product.
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Cited By (2)
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| CN114250398A (en) * | 2021-12-06 | 2022-03-29 | 北京科技大学 | Preparation method of titanium/zirconium-based hydrogen storage alloy powder |
| CN114293047A (en) * | 2021-12-06 | 2022-04-08 | 北京科技大学 | Preparation method of ultrahigh-strength powder metallurgy titanium alloy |
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| WO2013022531A1 (en) * | 2011-08-08 | 2013-02-14 | Advance Material Products, Inc. | Manufacture of near-net shape titanium alloy articles from metal powders by sintering with presence of atomic hydrogen |
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| CN113481408A (en) * | 2021-07-08 | 2021-10-08 | 中南大学 | Powder metallurgy Ti-Zr alloy for dentistry and preparation method thereof |
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| US20120058002A1 (en) * | 2007-06-11 | 2012-03-08 | Advance Material Products, Inc.,(ADMA Products, Inc.) | Manufacture of near-net shape titanium alloy articles from metal powders by sintering with presence of atomic hydrogen |
| WO2013022531A1 (en) * | 2011-08-08 | 2013-02-14 | Advance Material Products, Inc. | Manufacture of near-net shape titanium alloy articles from metal powders by sintering with presence of atomic hydrogen |
| CN112030024A (en) * | 2020-07-29 | 2020-12-04 | 北京科技大学 | High-strength high-plasticity titanium-based composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114250398A (en) * | 2021-12-06 | 2022-03-29 | 北京科技大学 | Preparation method of titanium/zirconium-based hydrogen storage alloy powder |
| CN114293047A (en) * | 2021-12-06 | 2022-04-08 | 北京科技大学 | Preparation method of ultrahigh-strength powder metallurgy titanium alloy |
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