CN116875836A - Ultra-fine grain titanium alloy material and in-situ synthesis method thereof - Google Patents
Ultra-fine grain titanium alloy material and in-situ synthesis method thereof Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 94
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 66
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 23
- 238000001308 synthesis method Methods 0.000 title claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 57
- 239000002184 metal Substances 0.000 claims abstract description 57
- 239000000843 powder Substances 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000002243 precursor Substances 0.000 claims abstract description 30
- 238000002844 melting Methods 0.000 claims abstract description 16
- 230000008018 melting Effects 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract 2
- 229910045601 alloy Inorganic materials 0.000 claims description 24
- 238000000498 ball milling Methods 0.000 claims description 20
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 4
- 238000004093 laser heating Methods 0.000 claims description 3
- 230000006911 nucleation Effects 0.000 abstract description 18
- 238000010899 nucleation Methods 0.000 abstract description 18
- 230000008569 process Effects 0.000 abstract description 13
- 238000003723 Smelting Methods 0.000 abstract description 9
- 230000007797 corrosion Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 4
- 238000007711 solidification Methods 0.000 abstract description 4
- 230000008023 solidification Effects 0.000 abstract description 4
- 238000013461 design Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005275 alloying Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 9
- 239000010936 titanium Substances 0.000 description 9
- 238000005339 levitation Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000004781 supercooling Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000005242 forging Methods 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 229910010380 TiNi Inorganic materials 0.000 description 2
- 229910008651 TiZr Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000010353 genetic engineering Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
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- 239000007787 solid Substances 0.000 description 1
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- 239000002699 waste material Substances 0.000 description 1
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- 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
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- 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
- C22C1/02—Making non-ferrous alloys by melting
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- 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
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Abstract
Description
技术领域Technical field
本发明属于金属材料制备技术领域，具体涉及一种超细晶钛合金材料及其原位合成方法。The invention belongs to the technical field of metal material preparation, and specifically relates to an ultrafine-grained titanium alloy material and an in-situ synthesis method thereof.
背景技术Background technique
钛被誉为“第三金属”、“太空金属”、“海洋金属”。钛及钛合金是极其重要的轻质结构材料，也是比强度较高的金属材料之一，兼具优异的耐腐蚀性能、耐热性能、无磁等一系列特性，在航空、航天、舰船、化工、冶金、生物医疗、交通运输等领域得到了广阔的应用。自20世纪50年代以来，钛及钛合金已经历了70余年的发展历程，其种类已从最初的TC4合金发展到数百种。西北有色金属研究院独立创新研制的钛合金近50种，形成了高温、低温、高强、高韧、损伤容限、耐蚀、船用、阻燃、低成本和医用等钛合金系列，开发出钛合金的板、箔、管、棒、丝、锻件、压力容器、异形件、紧固件等产品。Titanium is known as the "third metal", "space metal" and "ocean metal". Titanium and titanium alloys are extremely important lightweight structural materials and one of the metal materials with higher relative strength. They have excellent corrosion resistance, heat resistance, non-magnetic and a series of properties. They are widely used in aviation, aerospace and ships. , chemical industry, metallurgy, biomedicine, transportation and other fields have been widely used. Since the 1950s, titanium and titanium alloys have experienced more than 70 years of development, and their types have developed from the original TC4 alloy to hundreds of types. Northwest Nonferrous Metals Research Institute has independently developed nearly 50 kinds of titanium alloys, forming high-temperature, low-temperature, high-strength, high-toughness, damage-tolerant, corrosion-resistant, marine, flame-retardant, low-cost and medical titanium alloy series, and developed titanium alloy series. Alloy plates, foils, tubes, rods, wires, forgings, pressure vessels, special-shaped parts, fasteners and other products.
目前，钛合金的主流制备方法仍然是熔炼法。由于钛合金熔体总是或多或少含有某些杂质，因此，凝固过程中的晶坯常常依附于这些固态杂质质点上形核。同时，钛合金熔体和模具壁面直接接触，也会依附于型壁直接形核。由此可见，钛合金的结晶过程主要按非均匀形核方式进行，且呈树枝晶生长方式。此外，相对于均匀形核，非均匀形核所需的形核功很小，所以在较小的过冷度条件下，当均匀形核还微不足道时，非均匀形核就明显开始了。研究表明，当过冷度约为0.02Tm时，非均匀形核具有最大的形核率，这只相当于均匀形核达到最大形核率时所需过冷度(0.2Tm)的1/10。为了改善钛合金的性能，常常希望获得细小等轴晶粒。因此，熔炼后的钛合金还需要经过锻造或轧制、热处理等工序，导致氧含量增加、材料利用率低，且生产周期长，制备成本高。At present, the mainstream preparation method of titanium alloy is still the smelting method. Since titanium alloy melt always contains more or less certain impurities, the crystal blank during the solidification process often nucleates on these solid impurity particles. At the same time, the titanium alloy melt is in direct contact with the mold wall and will also adhere to the mold wall for direct nucleation. It can be seen that the crystallization process of titanium alloy mainly proceeds in the form of non-uniform nucleation and dendritic growth. In addition, compared with uniform nucleation, the nucleation work required for non-uniform nucleation is very small, so under small supercooling conditions, when uniform nucleation is still insignificant, non-uniform nucleation starts obviously. Research shows that when the supercooling degree is about 0.02T m , non-uniform nucleation has the maximum nucleation rate, which is only equivalent to 1 of the supercooling degree (0.2T m ) required for uniform nucleation to reach the maximum nucleation rate. /10. In order to improve the properties of titanium alloys, it is often desirable to obtain fine equiaxed grains. Therefore, the smelted titanium alloy still needs to go through forging or rolling, heat treatment and other processes, resulting in increased oxygen content, low material utilization, long production cycle, and high preparation cost.
发明内容Contents of the invention
本发明所要解决的技术问题在于针对上述现有技术的不足，提供一种超细晶钛合金材料的原位合成方法。该方法通过混粉、压制、真空熔炼、静电悬浮加热原位合成超细晶钛合金材料，无需采用模具，使得金属熔体在凝固过程中均匀形核，且形成非常大的过冷度，显著增加均匀形核的形核率，使得金属形成超细等轴晶组织，有利于改善钛合金的性能，解决了现有通过后续加工工序获得细小等轴晶粒而导致材料氧含量增加、制备流程长及成本高的难题。The technical problem to be solved by the present invention is to provide an in-situ synthesis method of ultra-fine-grained titanium alloy materials in view of the above-mentioned deficiencies in the prior art. This method synthesizes ultra-fine-grained titanium alloy materials in situ through powder mixing, pressing, vacuum melting, and electrostatic suspension heating without the need for molds, allowing the metal melt to nucleate uniformly during the solidification process and form a very large degree of supercooling, significantly Increasing the nucleation rate of uniform nucleation enables the metal to form an ultra-fine equiaxed grain structure, which is conducive to improving the performance of titanium alloys and solving the existing problem of increased oxygen content and preparation process caused by obtaining fine equiaxed grains through subsequent processing procedures. Long-term and high-cost problems.
为解决上述技术问题，本发明采用的技术方案为：一种超细晶钛合金材料的原位合成方法，其特征在于，该方法包括以下步骤：In order to solve the above technical problems, the technical solution adopted by the present invention is: an in-situ synthesis method of ultra-fine-grained titanium alloy materials, which is characterized in that the method includes the following steps:
步骤一、按照目标产物超细晶钛合金材料的成分配比，称取相应的元素粉末，然后进行混合，得到混合金属粉末；Step 1: According to the component ratio of the target product ultra-fine-grained titanium alloy material, weigh the corresponding element powders and then mix them to obtain mixed metal powder;
步骤二、将步骤一中得到的混合金属粉末进行压制，得到生坯；Step 2: Press the mixed metal powder obtained in Step 1 to obtain a green body;
步骤三、将步骤二中得到的生坯进行激光真空熔炼，得到金属前驱体；Step 3: Perform laser vacuum melting on the green body obtained in Step 2 to obtain a metal precursor;
步骤四、将步骤三中得到的金属前驱体通过静电悬浮设备进行加热，待金属前驱体熔化并保温后冷却，得到超细晶钛合金材料。Step 4: Heat the metal precursor obtained in Step 3 through electrostatic levitation equipment. After the metal precursor is melted and kept warm, it is cooled to obtain an ultra-fine-grained titanium alloy material.
上述的一种超细晶钛合金材料的原位合成方法，其特征在于，步骤一中所述混合采用球磨法，球磨转速为200rpm～350rpm。本发明通过采用球磨法并控制球磨转速，在使得各粉末混合均匀的同时细化粉末颗粒，并避免转速过快导致钛粉末氧化爆炸，保证了混粉过程的安全性。The above-mentioned in-situ synthesis method of ultra-fine-grained titanium alloy materials is characterized in that the mixing described in step one adopts a ball milling method, and the ball milling speed is 200rpm to 350rpm. By adopting the ball milling method and controlling the ball milling speed, the present invention can refine the powder particles while mixing the powders uniformly, and avoid the oxidation and explosion of the titanium powder caused by excessive speed, thus ensuring the safety of the powder mixing process.
上述的一种超细晶钛合金材料的原位合成方法，其特征在于，步骤二中所述生坯为圆柱形或半球形。本发明通过限定生坯为圆柱形或半球形，以保证在后续激光真空熔炼过程中形成球形的金属前驱体，便于后续静电悬浮设备中工艺的进行同时缩短熔炼时间，节约能源，降低制备成本。The above-mentioned in-situ synthesis method of ultra-fine-grained titanium alloy material is characterized in that the green body in step two is cylindrical or hemispherical. By limiting the green body to a cylindrical or hemispherical shape, the present invention ensures that a spherical metal precursor is formed during the subsequent laser vacuum melting process, thereby facilitating the subsequent process in the electrostatic levitation equipment, shortening the melting time, saving energy, and reducing preparation costs.
上述的一种超细晶钛合金材料的原位合成方法，其特征在于，步骤四中所述保温的时间为2min～5min。本发明通过限定金属前驱体熔化后的保温时间，保证合金均匀化，同时避免保温时间过长浪费能源、增加合成成本。The above-mentioned in-situ synthesis method of ultra-fine-grained titanium alloy material is characterized in that the heat preservation time in step 4 is 2 to 5 minutes. The present invention ensures the homogenization of the alloy by limiting the heat preservation time after the metal precursor is melted, and at the same time avoids waste of energy and increased synthesis costs if the heat preservation time is too long.
上述的一种超细晶钛合金材料的原位合成方法，其特征在于，步骤四中所述加热方式为激光加热。激光加热的速度过快，且激光器方便调整位置，易于操作。The above-mentioned in-situ synthesis method of ultra-fine-grained titanium alloy material is characterized in that the heating method in step 4 is laser heating. The laser heating speed is too fast, and the laser is easy to adjust its position and easy to operate.
上述的一种超细晶钛合金材料的原位合成方法，其特征在于，步骤四中所述金属前驱体熔化的过热度为100℃～200℃。该过热度保证了金属前驱体完全熔化并合金化，避免过热度过大增加激光功率、浪费电能，同时造成合金元素挥发率增大、影响钛合金材料实际成分偏离设计成分。The above-mentioned in-situ synthesis method of ultra-fine-grained titanium alloy material is characterized in that the superheat of melting the metal precursor in step 4 is 100°C to 200°C. This degree of superheat ensures that the metal precursor is completely melted and alloyed, preventing excessive superheat from increasing laser power and wasting electrical energy. At the same time, it will increase the volatilization rate of alloy elements and affect the actual composition of the titanium alloy material to deviate from the designed composition.
上述的一种超细晶钛合金材料的原位合成方法，其特征在于，步骤四中所述冷却方式为在悬浮状态下随炉冷却。通过在悬浮状态下随炉冷却，使得熔融后的金属前驱体处于深过冷状态，增大了超细晶钛合金材料的形核速率，细化了晶粒，进而提高了超细晶钛合金材料的强韧性。The above-mentioned in-situ synthesis method of ultra-fine-grained titanium alloy material is characterized in that the cooling method in step 4 is furnace cooling in a suspended state. By cooling with the furnace in a suspended state, the molten metal precursor is in a deep supercooled state, which increases the nucleation rate of the ultra-fine-grained titanium alloy material, refines the grains, and thereby improves the quality of the ultra-fine-grained titanium alloy. The strength and toughness of the material.
上述的一种超细晶钛合金材料的原位合成方法，其特征在于，步骤四中所述超细晶钛合金材料的材质为Ti185合金、TiNi合金、TiZr合金、TiNbZr合金、TiNbVZr合金。更优选地为Ti185合金、TiNbZr合金和TiNbVZr合金。Ti185合金是一种低成本高强钛合金，可用于制备航空结构件，应用前景广阔；TiNbZr合金和TiNbVZr合金属于高熵合金，具有高熔点、高强度、高塑性、低温下高断裂韧性和热稳定性等优点，可广泛应用于航空航天、国防、军工等领域。本发明的合成方法应用范围广，使用价值高。The above-mentioned in-situ synthesis method of ultra-fine-grained titanium alloy material is characterized in that the material of the ultra-fine-grained titanium alloy material in step 4 is Ti185 alloy, TiNi alloy, TiZr alloy, TiNbZr alloy, and TiNbVZr alloy. More preferred are Ti185 alloy, TiNbZr alloy and TiNbVZr alloy. Ti185 alloy is a low-cost, high-strength titanium alloy that can be used to prepare aerospace structural parts and has broad application prospects; TiNbZr alloy and TiNbVZr alloy are high-entropy alloys with high melting point, high strength, high plasticity, high fracture toughness at low temperatures and thermal stability. Due to its advantages such as durability, it can be widely used in aerospace, national defense, military industry and other fields. The synthesis method of the present invention has a wide application range and high use value.
此外，本发明还公开了一种如上述的方法制备的超细晶钛合金材料。In addition, the invention also discloses an ultra-fine-grained titanium alloy material prepared by the above method.
本发明与现有技术相比具有以下优点：Compared with the prior art, the present invention has the following advantages:
1、本发明根据目标产物的成分配比选择元素粉末，经压制、真空熔炼、静电悬浮加热后原位合成超细晶钛合金材料，通过静电悬浮工艺无需采用模具，使得金属前驱体熔化形成的金属熔体在冷却凝固过程中不与型壁接触，只是依靠金属熔体的能量变化由晶坯直接形核，更接近于均匀形核方式，同时由于无需模具，金属熔体在冷却过程中形成非常大的过冷度(趋于0.2Tm)，其晶核的形核功显著降低，而形核率显著增大，从而使得金属形成超细等轴晶组织，得到超细晶钛合金材料。1. The present invention selects element powder according to the component ratio of the target product, and synthesizes ultra-fine-grained titanium alloy materials in situ after pressing, vacuum melting, and electrostatic suspension heating. The electrostatic suspension process does not require the use of molds, so that the metal precursor is melted to form The metal melt does not come into contact with the mold wall during the cooling and solidification process. It only relies on the energy change of the metal melt to nucleate directly from the crystal blank, which is closer to a uniform nucleation method. At the same time, because there is no need for a mold, the metal melt is formed during the cooling process. At a very large degree of supercooling (tending to 0.2T m ), the nucleation work of the crystal nucleus is significantly reduced, and the nucleation rate is significantly increased, thereby causing the metal to form an ultra-fine equiaxed crystal structure and obtaining ultra-fine grained titanium alloy materials. .
2、本发明根据目标产物的成分配比选择元素粉末进行后续合成工序，有利于钛合金成分的自由设计与配制，结合材料基因工程，可实现新型钛合金的快速设计与制备，缩短研制周期。2. The present invention selects element powder according to the component ratio of the target product for subsequent synthesis processes, which is conducive to the free design and preparation of titanium alloy components. Combined with material genetic engineering, it can achieve rapid design and preparation of new titanium alloys and shorten the development cycle.
3、本发明采用粉末冶金法和静电悬浮法相结合来制备钛合金材料，大幅降低了钛合金材料成分的偏析和杂质含量，使得钛合金材料成分更加均匀，材料的性能趋于理论值。3. The present invention uses a combination of powder metallurgy and electrostatic suspension methods to prepare titanium alloy materials, which greatly reduces the segregation and impurity content of the titanium alloy material components, making the titanium alloy material components more uniform and the material properties tend to be closer to theoretical values.
4、本发明制备的钛合金材料晶粒度非常小，为纳米尺度，远小于传统熔炼法制备的钛合金材料的晶粒度，显著提高了钛合金材料的强度和硬度，同时极大地改善了钛合金材料的塑性和韧性，使其兼具高比强度、高比模量、优异的耐腐蚀性、良好的强塑/韧性匹配等特点，解决了钛合金材料的强-塑性、强-韧性桎梏，有利于扩大钛合金材料的应用领域。4. The titanium alloy material prepared by the present invention has a very small grain size, which is in the nanometer scale, which is much smaller than the grain size of the titanium alloy material prepared by the traditional smelting method. It significantly improves the strength and hardness of the titanium alloy material, and at the same time greatly improves the The plasticity and toughness of titanium alloy materials enable them to combine high specific strength, high specific modulus, excellent corrosion resistance, and good strength-plasticity/toughness matching, which solves the problem of strong-plasticity and strong-toughness of titanium alloy materials. The shackles are conducive to expanding the application fields of titanium alloy materials.
5、本发明通过调控合成方法制备得到超细晶钛合金材料，无需后续采用多次熔炼、锻造、热处理等工序进行晶粒细化，大大缩短其制备流程，显著降低生产成本，同时可推广应用于制备其他合金材料。5. The present invention prepares ultra-fine-grained titanium alloy materials through a controlled synthesis method. It does not require subsequent steps such as multiple smelting, forging, and heat treatments for grain refinement, greatly shortening the preparation process, significantly reducing production costs, and at the same time, it can be promoted and applied. For the preparation of other alloy materials.
下面通过附图和实施例对本发明的技术方案作进一步的详细描述。The technical solution of the present invention will be described in further detail below through the drawings and examples.
附图说明Description of the drawings
图1为本发明实施例1制备的超细晶Ti185合金材料的微观组织图。Figure 1 is a microstructure diagram of the ultrafine-grained Ti185 alloy material prepared in Example 1 of the present invention.
图2为本发明对比例1制备的Ti185合金材料的微观组织图。Figure 2 is a microstructure diagram of the Ti185 alloy material prepared in Comparative Example 1 of the present invention.
具体实施方式Detailed ways
实施例1Example 1
本实施例包括以下步骤：This embodiment includes the following steps:
步骤一、按照目标产物超细晶Ti185(Ti-1Al-8V-5Fe)合金材料的成分配比，称取对应质量的Ti粉末、Al粉末、FeV80粉末和Fe粉末，然后采用行星式球磨机进行球磨混合，球磨转速为300rpm，球磨时间为3h，得到混合金属粉末；Step 1. According to the composition ratio of the target product ultra-fine grain Ti185 (Ti-1Al-8V-5Fe) alloy material, weigh the corresponding masses of Ti powder, Al powder, FeV80 powder and Fe powder, and then use a planetary ball mill for ball milling Mix, the ball milling speed is 300rpm, the ball milling time is 3h, and the mixed metal powder is obtained;
步骤二、将步骤一中得到的混合金属粉末进行压制，得到外形尺寸(直径×高度)为φ3.0mm×2mm的圆柱形生坯；Step 2: Press the mixed metal powder obtained in Step 1 to obtain a cylindrical green body with an outer size (diameter × height) of φ3.0mm × 2mm;
步骤三、将步骤二中得到的圆柱形生坯进行激光真空熔炼，得到球形金属前驱体；Step 3: Perform laser vacuum melting on the cylindrical green body obtained in Step 2 to obtain a spherical metal precursor;
步骤四、将步骤三中得到的球形金属前驱体通过静电悬浮设备进行激光加热，待金属前驱体熔化后继续加热到过热度为100℃并保温3min，关闭激光使其在悬浮状态下随炉冷却，得到超细晶Ti185合金材料。Step 4: Use the electrostatic levitation equipment to laser-heat the spherical metal precursor obtained in Step 3. After the metal precursor is melted, continue to heat it until the superheat is 100°C and keep it warm for 3 minutes. Turn off the laser and let it cool in the furnace in a suspended state. , obtaining ultra-fine grain Ti185 alloy material.
图1为本实施例制备的超细晶Ti185合金材料的微观组织图，从图1可以看出，该超细晶Ti185合金材料中的晶粒度非常小，为纳米尺度。Figure 1 is a microstructure diagram of the ultra-fine-grained Ti185 alloy material prepared in this embodiment. It can be seen from Figure 1 that the grain size in the ultra-fine-grained Ti185 alloy material is very small and is nanoscale.
本实施例步骤二中的生坯形状还可为半球形；步骤一和步骤四中的目标产物超细晶Ti185合金材料还可替换为超细晶TiNi合金材料或超细晶TiZr合金材料。The shape of the green body in step two of this embodiment can also be hemispherical; the target product ultrafine-grained Ti185 alloy material in steps one and four can also be replaced with ultrafine-grained TiNi alloy material or ultrafine-grained TiZr alloy material.
对比例1Comparative example 1
本对比例采用传统熔炼法包括以下步骤：This comparative example uses traditional smelting method including the following steps:
步骤一、按照目标产物超细晶Ti185(Ti-1Al-8V-5Fe)合金材料的成分配比，称取对应质量的海绵钛、铝颗粒、TiFe32颗粒、FeV80颗粒，然后压制成电极块；Step 1. According to the composition ratio of the target product ultra-fine grain Ti185 (Ti-1Al-8V-5Fe) alloy material, weigh the corresponding mass of sponge titanium, aluminum particles, TiFe32 particles, and FeV80 particles, and then press them into electrode blocks;
步骤二、将步骤一中制得的电极块进行一次真空感应熔炼，得到合金块；Step 2: Perform vacuum induction melting on the electrode block prepared in Step 1 to obtain an alloy block;
步骤三、将步骤二得到的合金块进行二次真空感应熔炼，得到Ti185合金材料。Step 3: Perform secondary vacuum induction melting on the alloy block obtained in Step 2 to obtain Ti185 alloy material.
采用粉末原料熔炼制备钛合金材料，由于粉末比表面积大，易因氧化引入杂质，故本对比例中的传统熔炼法采用金属或中间合金颗粒以降低原料成本，并采用多次熔炼以保证充分合金化均匀。Titanium alloy materials are prepared by smelting powder raw materials. Due to the large specific surface area of the powder, impurities are easily introduced due to oxidation. Therefore, the traditional smelting method in this comparative example uses metal or master alloy particles to reduce raw material costs, and multiple smelting is used to ensure sufficient alloying. Evenly.
图2为本对比例制备的Ti185合金材料的微观组织图，从图2可以看出，该Ti185合金材料的晶粒度非常粗大，为几百微米，远高于实施例1制备的超细晶Ti185合金材料的晶粒度。Figure 2 is a microstructure diagram of the Ti185 alloy material prepared in this comparative example. It can be seen from Figure 2 that the grain size of the Ti185 alloy material is very coarse, several hundred microns, which is much higher than the ultra-fine grain size prepared in Example 1. The grain size of Ti185 alloy material.
实施例2Example 2
本实施例包括以下步骤：This embodiment includes the following steps:
步骤一、按照目标产物超细晶Ti185(Ti-1Al-8V-5Fe)钛合金材料的成分配比，称取对应质量的Ti粉末、Al粉末、FeV80粉末和Fe粉末，然后采用行星式球磨机进行球磨混合，球磨转速为200rpm，球磨时间为4h，得到混合金属粉末；Step 1. According to the composition ratio of the target product ultra-fine grain Ti185 (Ti-1Al-8V-5Fe) titanium alloy material, weigh the corresponding masses of Ti powder, Al powder, FeV80 powder and Fe powder, and then use a planetary ball mill to process Mix by ball milling, the ball milling speed is 200rpm, and the ball milling time is 4h to obtain mixed metal powder;
步骤二、将步骤一中得到的混合金属粉末进行压制，得到外形尺寸(直径×高度)为φ4.0mm×1.1mm的圆柱形生坯；Step 2: Press the mixed metal powder obtained in Step 1 to obtain a cylindrical green body with an outer size (diameter × height) of φ4.0mm × 1.1mm;
步骤三、将步骤二中得到的圆柱形生坯进行激光真空熔炼，得到球形金属前驱体；Step 3: Perform laser vacuum melting on the cylindrical green body obtained in Step 2 to obtain a spherical metal precursor;
步骤四、将步骤三中得到的球形金属前驱体通过静电悬浮设备进行激光加热，待金属前驱体熔化后继续加热到过热度为130℃并保温2min，关闭激光使其在悬浮状态下随炉冷却，得到超细晶Ti185钛合金材料。Step 4: Use the electrostatic levitation equipment to laser-heat the spherical metal precursor obtained in Step 3. After the metal precursor is melted, continue to heat it until the superheat is 130°C and keep it warm for 2 minutes. Turn off the laser and let it cool in the furnace in a suspended state. , obtaining ultra-fine grained Ti185 titanium alloy material.
实施例3Example 3
本实施例包括以下步骤：This embodiment includes the following steps:
步骤一、按照目标产物超细晶TiNbVZr(原子比为1:1:1:1)合金材料的成分配比，称取对应质量的Ti粉末、Nb粉末、V粉末和Zr粉末，然后采用行星式球磨机进行球磨混合，球磨转速为350rpm，球磨时间为2h，得到混合金属粉末；Step 1. According to the composition ratio of the target product ultra-fine grain TiNbVZr (atomic ratio is 1:1:1:1) alloy material, weigh the corresponding masses of Ti powder, Nb powder, V powder and Zr powder, and then use the planetary method The ball mill is used for ball milling and mixing, the ball milling speed is 350rpm, the ball milling time is 2h, and the mixed metal powder is obtained;
步骤二、将步骤一中得到的混合金属粉末进行压制，得到外形尺寸(直径×高度)为φ2.5mm×2.9mm的圆柱形生坯；Step 2: Press the mixed metal powder obtained in Step 1 to obtain a cylindrical green body with an outer size (diameter × height) of φ2.5mm × 2.9mm;
步骤三、将步骤二中得到的圆柱形生坯进行激光真空熔炼，得到球形金属前驱体；Step 3: Perform laser vacuum melting on the cylindrical green body obtained in Step 2 to obtain a spherical metal precursor;
步骤四、将步骤三中得到的球形金属前驱体通过静电悬浮设备进行激光加热，待球形金属前驱体熔化后继续加热到过热度为200℃并保温3min，关闭激光使其在悬浮状态下随炉冷却，得到超细晶TiNbVZr合金材料。Step 4: Use the electrostatic levitation equipment to laser-heat the spherical metal precursor obtained in Step 3. After the spherical metal precursor is melted, continue to heat it until the superheat is 200°C and keep it warm for 3 minutes. Turn off the laser and let it float in the furnace. After cooling, ultra-fine grain TiNbVZr alloy material is obtained.
实施例4Example 4
本实施例包括以下步骤：This embodiment includes the following steps:
步骤一、按照目标产物超细晶TiNbVZr(原子比为2:1:1:1)合金材料的成分配比，称取对应质量的Ti粉末、Nb粉末、V粉末和Zr粉末，然后采用行星式球磨机进行球磨混合，球磨转速为300rpm，球磨时间为3h，得到混合金属粉末；Step 1. According to the composition ratio of the target product ultra-fine grain TiNbVZr (atomic ratio is 2:1:1:1) alloy material, weigh the corresponding masses of Ti powder, Nb powder, V powder and Zr powder, and then use the planetary method The ball mill is used for ball milling mixing, the ball milling speed is 300rpm, the ball milling time is 3h, and the mixed metal powder is obtained;
步骤二、将步骤一中得到的混合金属粉末进行压制，得到外形尺寸(直径×高度)为φ3.0mm×2mm的圆柱形生坯；Step 2: Press the mixed metal powder obtained in Step 1 to obtain a cylindrical green body with an outer size (diameter × height) of φ3.0mm × 2mm;
步骤三、将步骤二中得到的圆柱形生坯进行激光真空熔炼，得到球形金属前驱体；Step 3: Perform laser vacuum melting on the cylindrical green body obtained in Step 2 to obtain a spherical metal precursor;
步骤四、将步骤三中得到的球形金属前驱体通过静电悬浮设备进行激光加热，待球形金属前驱体熔化后继续加热到过热度为150℃并保温5min，关闭激光使其在悬浮状态下随炉冷却，得到超细晶TiNbVZr合金材料。Step 4: Use the electrostatic levitation equipment to laser-heat the spherical metal precursor obtained in Step 3. After the spherical metal precursor is melted, continue to heat it until the superheat is 150°C and keep it warm for 5 minutes. Turn off the laser and let it float in the furnace. After cooling, ultra-fine grain TiNbVZr alloy material is obtained.
实施例5Example 5
本实施例包括以下步骤：This embodiment includes the following steps:
步骤一、按照目标产物超细晶TiNbZr(原子比为1:1:1)合金材料的成分配比，称取对应质量的Ti粉末、Nb粉末和Zr粉末，然后采用行星式球磨机进行球磨混合，球磨转速为300rpm，球磨时间为3h，得到混合金属粉末；Step 1. According to the composition ratio of the target product ultra-fine crystal TiNbZr (atomic ratio is 1:1:1) alloy material, weigh the corresponding mass of Ti powder, Nb powder and Zr powder, and then use a planetary ball mill to ball mill and mix. The ball milling speed is 300rpm and the ball milling time is 3h to obtain mixed metal powder;
步骤二、将步骤一中得到的混合金属粉末进行压制，得到外形尺寸(直径×高度)为φ2.5mm×1.5mm的圆柱形生坯；Step 2: Press the mixed metal powder obtained in Step 1 to obtain a cylindrical green body with an outer size (diameter × height) of φ2.5mm × 1.5mm;
步骤三、将步骤二中得到的圆柱形生坯进行激光真空熔炼，得到球形金属前驱体；Step 3: Perform laser vacuum melting on the cylindrical green body obtained in Step 2 to obtain a spherical metal precursor;
步骤四、将步骤三中得到的球形金属前驱体通过静电悬浮设备进行激光加热，待金属前驱体熔化后继续加热到过热度为200℃并保温4min，关闭激光使其在悬浮状态下随炉冷却，得到超细晶TiNbZr合金材料。Step 4: Use the electrostatic levitation equipment to laser-heat the spherical metal precursor obtained in Step 3. After the metal precursor is melted, continue to heat it to a superheat of 200°C and keep it warm for 4 minutes. Turn off the laser and let it cool in the furnace in a suspended state. , obtaining ultrafine-grained TiNbZr alloy materials.
以上所述，仅是本发明的较佳实施例，并非对本发明作任何限制。凡是根据发明技术实质对以上实施例所作的任何简单修改、变更以及等效变化，均仍属于本发明技术方案的保护范围内。The above descriptions are only preferred embodiments of the present invention and do not limit the present invention in any way. Any simple modifications, changes and equivalent changes made to the above embodiments based on the technical essence of the invention still fall within the protection scope of the technical solution of the invention.
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