CN113798495B - A high-entropy alloy sintering forming process with double-element equivalent transformation - Google Patents
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 92
- 238000005245 sintering Methods 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 34
- 230000009466 transformation Effects 0.000 title abstract description 10
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- 238000000465 moulding Methods 0.000 claims abstract description 9
- 229910052802 copper Inorganic materials 0.000 claims abstract description 5
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- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 6
- 229910052804 chromium Inorganic materials 0.000 abstract description 4
- 229910052742 iron Inorganic materials 0.000 abstract description 4
- 229910052759 nickel Inorganic materials 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000007731 hot pressing Methods 0.000 description 21
- 239000011812 mixed powder Substances 0.000 description 14
- 238000010586 diagram Methods 0.000 description 13
- 239000000463 material Substances 0.000 description 10
- 238000011056 performance test Methods 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 6
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- 238000004372 laser cladding Methods 0.000 description 2
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Abstract
本发明公开了一种双元素等量变换的高熵合金烧结成型工艺，具体按照如下步骤实施：步骤1，将Co、Cr、Fe、Ni、Cu、Ti单质粉末按照等原子百分比进行称量混合，将其配置成不同比例成分的CoCrFeNi(CuTi)x高熵合金粉末，其中x＝0.2‑1.0；步骤2，将步骤1配置的高熵合金粉末置于球磨罐中进行高能球磨，制备出所需成分均匀的不同比例成分的混合高熵合金粉末；步骤3，将步骤2得到的混合高熵合金粉末进行真空热压烧结或快速热压烧结成型，待其烧结冷却后脱模得到(CuTi)x双元素等量变换的高熵合金块体。本发明制备方法简单、生产成本低且得到的高熵合金致密度高、组织均匀。
The invention discloses a high-entropy alloy sintering molding process of double-element equivalent transformation, which is specifically implemented according to the following steps: Step 1, weighing and mixing Co, Cr, Fe, Ni, Cu, and Ti elemental powders according to equal atomic percentages , configure it into CoCrFeNi(CuTi) x high-entropy alloy powders of different proportions, wherein x=0.2-1.0; step 2, place the high-entropy alloy powder configured in step 1 in a ball mill jar for high-energy ball milling, and prepare the Mixed high-entropy alloy powders with different proportions of components that are uniform in composition are required; step 3, vacuum hot-press sintering or rapid hot-press sintering is performed on the mixed high-entropy alloy powder obtained in step 2, and after sintering and cooling, demoulding is obtained (CuTi) High-entropy alloy bulk with double-element equivalent transformation of x . The preparation method of the invention is simple, the production cost is low, and the obtained high-entropy alloy has high density and uniform structure.
Description
技术领域technical field
本发明属于高熵合金制备工艺技术领域，涉及一种双元素等量变换的高熵合金烧结成型工艺。The invention belongs to the technical field of high-entropy alloy preparation technology, and relates to a high-entropy alloy sintering molding process of double-element equivalent transformation.
背景技术Background technique
高熵合金是在非晶合金发展过程中衍生出来的一类新型合金，该合金具有高硬度、高耐腐蚀性、高耐磨性以及高的抗氧化性等优异性能而引起材料研究者的广泛关注。1995年，叶均蔚教授提出多主元高熵合金的设计理念：合金元素一般大于等于5种元素，且每种元素的原子百分比为5％～35％，熵值大于1.61R。这种新型合金设计理念的提出，打破了传统合金单一主元的设计观念，开创了合金设计领域的新思路。传统合金设计理念认为，合金组分越多，越易形成金属间化合物或复杂相。然而，研究表明，由多种主要元素组成的合金组分会产生高熵效应，该效应能促进具有体心立方或面心立方等固溶体相的形成，能抑制金属间化合物的形成，甚至能有利于非晶体结构的形成。High-entropy alloys are a new class of alloys derived from the development of amorphous alloys. The alloys have excellent properties such as high hardness, high corrosion resistance, high wear resistance, and high oxidation resistance, which have attracted wide attention from material researchers. focus on. In 1995, Professor Ye Junwei proposed the design concept of multi-principal high-entropy alloys: alloy elements are generally greater than or equal to 5 elements, and the atomic percentage of each element is 5% to 35%, and the entropy value is greater than 1.61R. The proposal of this new alloy design concept breaks the traditional design concept of single principal element of alloy and creates a new idea in the field of alloy design. The traditional alloy design concept holds that the more alloy components, the easier it is to form intermetallic compounds or complex phases. However, studies have shown that alloy components composed of multiple main elements can produce high entropy effects, which can promote the formation of solid solution phases with body-centered cubic or face-centered cubic, can inhibit the formation of intermetallic compounds, and can even favor Formation of non-crystalline structures.
迄今为止，高熵合金的制备工艺主要可分为四种，机械合金化法、粉末冶金法、真空熔炼法和激光熔覆法，然而，真空熔炼法和激光熔覆法等方法只适合于实验室研究且耗资巨大、设备复杂、工艺复杂、组织偏析不可避免等一系列缺点，使其对于高熵合金的未来商业化发展影响比较大，限制了高熵合金的批量化生产，不利于高熵合金的应用。然而机械合金化法往往和粉末冶金法相结合使用，并且其能有效改善组织偏析、生产成本低、可以大批量生产等，因此采用真空热压与快速热压烧结的烧结工艺探索对未来高熵合金的批量化生产至关重要。So far, the preparation processes of high-entropy alloys can be mainly divided into four types, mechanical alloying method, powder metallurgy method, vacuum melting method and laser cladding method. However, methods such as vacuum melting method and laser cladding method are only suitable for experiments. Laboratory research and a series of shortcomings such as huge cost, complicated equipment, complicated process, and inevitable structure segregation make it have a greater impact on the future commercial development of high-entropy alloys, which limits the mass production of high-entropy alloys and is not conducive to high-entropy alloys. alloy application. However, the mechanical alloying method is often used in combination with the powder metallurgy method, and it can effectively improve the structure segregation, low production cost, and mass production, etc. Mass production is very important.
发明内容Contents of the invention
本发明的目的是提供一种双元素等量变换的高熵合金烧结成型工艺，其制备方法简单、生产成本低且得到的高熵合金致密度高、组织均匀。The object of the present invention is to provide a high-entropy alloy sintering molding process with double-element equivalent transformation, the preparation method of which is simple, the production cost is low, and the obtained high-entropy alloy has high density and uniform structure.
本发明所采用的技术方案是，一种双元素等量变换的高熵合金烧结成型工艺，具体按照如下步骤实施：The technical solution adopted in the present invention is a high-entropy alloy sintering molding process with double-element equivalent transformation, which is specifically implemented according to the following steps:
步骤1，将Co、Cr、Fe、Ni、Cu、Ti单质粉末按照等原子百分比进行称量混合，将其配置成不同比例成分的CoCrFeNi(CuTi)x高熵合金混合粉末，其中x＝0.2-1.0；Step 1, weighing and mixing Co, Cr, Fe, Ni, Cu, and Ti elemental powders according to equal atomic percentages, and configuring them into CoCrFeNi(CuTi) x high-entropy alloy mixed powders with different proportions, where x=0.2- 1.0;
步骤2，将步骤1配置的高熵合金混合粉末置于球磨罐中进行高能球磨，制备出所需成分均匀的不同比例成分的混合高熵合金粉末；Step 2, placing the high-entropy alloy mixed powder configured in step 1 in a ball mill tank for high-energy ball milling to prepare mixed high-entropy alloy powders with uniform components in different proportions;
步骤3，将步骤2得到的混合高熵合金粉末进行真空热压烧结或快速热压烧结成型，待其烧结冷却后脱模得到(CuTi)x双元素等量变换的高熵合金块体。In step 3, the mixed high-entropy alloy powder obtained in step 2 is subjected to vacuum hot-press sintering or rapid hot-press sintering, and after sintering and cooling, demoulding is performed to obtain a high-entropy alloy block with (CuTi) x double-element equivalent transformation.
本发明的特征还在于，The present invention is also characterized in that,
步骤1中的Co、Cr、Fe、Ni、Cu、Ti单质粉末为纯度为99％、粒径为40um-48um的粉末。The Co, Cr, Fe, Ni, Cu, Ti elemental powders in step 1 are powders with a purity of 99% and a particle size of 40um-48um.
步骤2中球磨时球料质量比为8～12：1，球磨机转速为200～400r/min，球磨时间为20～24h。During the ball milling in step 2, the mass ratio of balls to materials is 8-12:1, the rotational speed of the ball mill is 200-400r/min, and the ball-milling time is 20-24h.
步骤2中球磨时磨球分为大、中、小三型且直径为9.5mm、5mm以及3mm三种磨球；的大、中、小三种磨球的质量比为2：3：5。During the ball milling in step 2, the grinding balls are divided into three types: large, medium and small, with diameters of 9.5 mm, 5 mm and 3 mm; the mass ratio of the large, medium and small grinding balls is 2:3:5.
步骤3中真空热压烧结的真空度为1.5x10-2pa，烧结压力为30～40MPa，烧结温度为1050℃～1200℃，保温时间为30～60min。In step 3, the vacuum degree of vacuum hot pressing sintering is 1.5x10 -2 pa, the sintering pressure is 30-40 MPa, the sintering temperature is 1050°C-1200°C, and the holding time is 30-60min.
真空热压烧结具体为：Vacuum hot pressing sintering is specifically:
将步骤2得到的混合高熵合金粉末在石墨磨具中先进行预压，然后将其置于烧结炉中施加压力至30～40Mpa，然后抽真空至真空度为1.5x10-2pa；以10℃/min的升温速率从室温升至300℃，在300℃保温10min；再以10℃/min的升温速率从300℃升至1050℃～1200℃，保温30～60min。The mixed high-entropy alloy powder obtained in step 2 is pre-pressed in a graphite grinding tool, then placed in a sintering furnace to apply a pressure of 30-40Mpa, and then vacuumed to a vacuum degree of 1.5x10 -2 Pa; The heating rate of ℃/min is raised from room temperature to 300 ℃, and the temperature is kept at 300 ℃ for 10 minutes; then the temperature is raised from 300 ℃ to 1050 ℃ ~ 1200 ℃ at a heating rate of 10 ℃ / min, and the temperature is kept for 30 ~ 60 minutes.
步骤3中的快速热压烧结的真空度为1.2pa，烧结压力为30～40MPa，烧结温度为950℃～1050℃，保温时间为30～60min。The vacuum degree of the rapid hot pressing sintering in step 3 is 1.2 Pa, the sintering pressure is 30-40 MPa, the sintering temperature is 950°C-1050°C, and the holding time is 30-60min.
步骤3中的快速热压烧结具体为：将步骤2得到的混合高熵合金粉末在石墨磨具中先进行预压，然后将其置于烧结炉中施加压力至30～40MPa；抽真空至真空度为1.2pa；以100℃/min的升温速率从室温升至300℃，在300℃保温10min；再以100℃/min的升温速率从300℃升至950℃～1050℃，保温30～60min。The rapid hot-press sintering in step 3 is as follows: pre-press the mixed high-entropy alloy powder obtained in step 2 in a graphite grinding tool, and then place it in a sintering furnace to apply a pressure of 30-40 MPa; vacuumize to a vacuum The temperature is 1.2pa; the temperature rises from room temperature to 300°C at a heating rate of 100°C/min, and is kept at 300°C for 10 minutes; 60min.
本发明的有益效果是：The beneficial effects of the present invention are:
本发明能快速的制备出所需的高致密度的高熵合金块体，其制备成本低、设备操作简单且适用于工业化批量生产。The invention can quickly prepare the required high-density high-entropy alloy bulk, has low preparation cost, simple equipment operation and is suitable for industrialized mass production.
本发明制备出的合金块体组织成分均匀有效避免了成分偏析。The composition of the alloy block prepared by the invention is uniform and effectively avoids composition segregation.
附图说明Description of drawings
图1为本发明实施例3的X＝0.4的CoCrFeNi(CuTi)x高熵合金块体材料的金相组织图与SEM扫描图；Fig. 1 is the metallographic structure diagram and the SEM scanning diagram of the CoCrFeNi (CuTi) x high-entropy alloy bulk material of X=0.4 of the embodiment of the present invention 3;
图2为本发明实施例5的X＝0.4的CoCrFeNi(CuTi)x高熵合金块体材料的金相组织图与SEM扫描图；Fig. 2 is the metallographic structure diagram and the SEM scanning diagram of the CoCrFeNi(CuTi) x high-entropy alloy bulk material of X=0.4 of the embodiment of the present invention;
图3为本发明实施例6的X＝0.4的CoCrFeNi(CuTi)x高熵合金块体材料的金相组织图与SEM扫描图；Fig. 3 is the metallographic structure diagram and the SEM scanning diagram of the CoCrFeNi(CuTi)x high-entropy alloy bulk material of X=0.4 of Example 6 of the present invention;
图4为本发明采用真空热压烧结的最佳烧结温度-时间曲线图；Fig. 4 adopts the best sintering temperature-time graph of the present invention for vacuum hot pressing sintering;
图5为本发明采用快速热压烧结的最佳烧结温度-时间曲线图。Fig. 5 is a curve diagram of optimum sintering temperature-time for rapid hot pressing sintering in the present invention.
具体实施方式Detailed ways
下面结合附图和具体实施方式对本发明进行详细说明。The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.
本发明一种双元素等量变换的高熵合金烧结成型工艺，具体按照如下步骤实施：A high-entropy alloy sintering molding process of double-element equivalent transformation of the present invention is specifically implemented according to the following steps:
步骤1，将纯度为99％、粒径为40um-48um的Co、Cr、Fe、Ni、Cu、Ti单质粉末按照等原子百分比进行称量混合，将其配置成不同比例成分的CoCrFeNi(CuTi)x高熵合金粉末，其中x＝0.2-1.0；Step 1, weighing and mixing Co, Cr, Fe, Ni, Cu, and Ti elemental powders with a purity of 99% and a particle size of 40um-48um according to equal atomic percentages, and configuring them into CoCrFeNi(CuTi) with different proportions x high-entropy alloy powder, wherein x=0.2-1.0;
步骤2，将步骤1配置的高熵合金粉末置于球磨罐中进行高能球磨，球磨时球料质量比为8～12：1，球磨机转速为200～400r/min，球磨时间为20～24h，磨球分为大、中、小三型且直径为9.5mm、5mm以及3mm三种磨球；的大、中、小三种磨球的质量比为2：3：5，制备出所需成分均匀的不同比例成分的混合高熵合金粉末；Step 2. Put the high-entropy alloy powder prepared in step 1 into a ball mill tank for high-energy ball milling. During ball milling, the mass ratio of ball to material is 8-12:1, the speed of ball mill is 200-400r/min, and the ball milling time is 20-24h. The grinding balls are divided into three types: large, medium and small, and the diameters are 9.5mm, 5mm and 3mm; the mass ratio of the large, medium and small grinding balls is 2:3:5, and the required composition is uniform Mixed high-entropy alloy powders with different proportions of components;
步骤3，将步骤2得到的混合高熵合金粉末进行真空热压烧结或快速热压烧结成型，待其烧结冷却后脱模得到(CuTi)x双元素等量变换的高熵合金块体；In step 3, the mixed high-entropy alloy powder obtained in step 2 is subjected to vacuum hot-pressing sintering or rapid hot-pressing sintering, and after it is sintered and cooled, it is released from the mold to obtain a high-entropy alloy block of (CuTi) x dual-element equivalent transformation;
若为真空热压烧结，则真空热压烧结的真空度为1.5x10-2pa，烧结压力为30～40MPa，烧结温度为1050℃～1200℃，保温时间为30～60min，具体为：If it is vacuum hot-press sintering, the vacuum degree of vacuum hot-press sintering is 1.5x10 -2 Pa, the sintering pressure is 30-40MPa, the sintering temperature is 1050°C-1200°C, and the holding time is 30-60min, specifically:
将步骤2得到的混合高熵合金粉末在石墨磨具中先进行预压，然后将其置于烧结炉中施加压力至30～40Mpa，然后抽真空至真空度为1.5x10-2pa；以10℃/min的升温速率从室温升至300℃，在300℃保温10min；再以10℃/min的升温速率从300℃升至1050℃～1200℃，保温30～60min。The mixed high-entropy alloy powder obtained in step 2 is pre-pressed in a graphite grinding tool, then placed in a sintering furnace to apply a pressure of 30-40Mpa, and then vacuumed to a vacuum degree of 1.5x10 -2 Pa; The heating rate of ℃/min is raised from room temperature to 300 ℃, and the temperature is kept at 300 ℃ for 10 minutes; then the temperature is raised from 300 ℃ to 1050 ℃ ~ 1200 ℃ at a heating rate of 10 ℃ / min, and the temperature is kept for 30 ~ 60 minutes.
若为快速热压烧结，则快速热压烧结的真空度为1.2pa，烧结压力为30～40MPa，烧结温度为950℃～1050℃，保温时间为30～60min，具体为：将步骤2得到的混合高熵合金粉末在石墨磨具中先进行预压，然后将其置于烧结炉中施加压力至30～40MPa；抽真空至真空度为1.2pa；以100℃/min的升温速率从室温升至300℃，在300℃保温10min；再以100℃/min的升温速率从300℃升至950℃～1050℃，保温30～60min。If it is rapid hot pressing sintering, the vacuum degree of rapid hot pressing sintering is 1.2pa, the sintering pressure is 30-40MPa, the sintering temperature is 950°C-1050°C, and the holding time is 30-60min. The mixed high-entropy alloy powder is pre-pressed in a graphite grinding tool, and then placed in a sintering furnace to apply a pressure of 30-40 MPa; vacuumize to a vacuum degree of 1.2 Pa; heat up from room temperature at a rate of 100 °C/min Raise to 300°C, keep at 300°C for 10 minutes; then raise the temperature from 300°C to 950°C-1050°C at a rate of 100°C/min, and keep hold for 30-60 minutes.
实施例1Example 1
针对合金成分为x＝0.4的CoCrFeNi(CuTi)x高熵合金粉末进行烧结对比试验。A sintering comparison test was carried out for the CoCrFeNi(CuTi) x high-entropy alloy powder with an alloy composition of x=0.4.
采用纯度为99％且粒径为44um的Co粉、Cr粉、Fe粉、Ni粉、Cu粉、Ti粉作为原料，按照等原子比进行称量混合，配置成Co:Cr:Fe:Ni:Cu:Ti＝1:1:1:1:0.4:0.4比例的高熵合金混合粉末，然后在球磨机中球磨20～24h。将混合好的粉末放入模具中，振动均匀且预压后，将模具置于真空热压烧结炉的炉腔内部进行加压烧结，烧结过程中压力维持在30～40MPa，抽真空至真空度为1.5x10-2pa，然后以10℃/min的升温速率从室温升至300℃，在300℃保温10min；再以10℃/min的升温速率从300℃升至1050℃，保温60min后降温卸压；将制备的毛胚依次进行表面磨削和去毛刺处理，制的真空热压烧结的x＝0.4的CoCrFeNi(CuTi)x高熵合金块体。Co powder, Cr powder, Fe powder, Ni powder, Cu powder, and Ti powder with a purity of 99% and a particle size of 44um are used as raw materials, weighed and mixed according to the equiatomic ratio, and configured as Co:Cr:Fe:Ni: Cu:Ti=1:1:1:1:0.4:0.4 high-entropy alloy mixed powder, and then ball milled in a ball mill for 20-24 hours. Put the mixed powder into the mold, vibrate evenly and pre-press, place the mold inside the cavity of the vacuum hot-press sintering furnace for pressure sintering, maintain the pressure at 30-40MPa during the sintering process, and evacuate to a vacuum degree 1.5x10 -2 Pa, then rise from room temperature to 300°C at a heating rate of 10°C/min, and keep at 300°C for 10 minutes; Lowering the temperature and releasing the pressure; performing surface grinding and deburring treatment on the prepared blank in sequence to prepare a CoCrFeNi(CuTi) x high-entropy alloy block with x=0.4 that was sintered by vacuum hot pressing.
其中球磨过程中过程控制剂的添加量为0.6％～1.2％，球料质量比为8～12：1，其中磨球分为大、中、小三型且直径为9.5mm、5mm以及3mm三种磨球；大、中、小三种磨球的质量比为2：3：5。The amount of process control agent added in the ball milling process is 0.6% to 1.2%, the mass ratio of ball to material is 8 to 12:1, and the grinding balls are divided into three types: large, medium and small, with diameters of 9.5mm, 5mm and 3mm. Grinding balls; the mass ratio of large, medium and small grinding balls is 2:3:5.
x＝0.4的CoCrFeNi(CuTi)x高熵合金材料试样打磨抛光后进行组织及性能测试，所得技术参数如表1所示；After the CoCrFeNi(CuTi) x high-entropy alloy material sample of x=0.4 was ground and polished, the microstructure and performance tests were carried out, and the obtained technical parameters are shown in Table 1;
表1实施例1制备的高熵合金材料的性能测试结果The performance test results of the high-entropy alloy material prepared in Table 1 Example 1
实施例2Example 2
针对合金成分为x＝0.4的CoCrFeNi(CuTi)x高熵合金粉末进行烧结对比试验。A sintering comparison test was carried out for the CoCrFeNi(CuTi) x high-entropy alloy powder with an alloy composition of x=0.4.
采用纯度为99％且粒径为44um的Co粉、Cr粉、Fe粉、Ni粉、Cu粉、Ti粉作为原料，按照等原子比进行称量混合，配置成Co:Cr:Fe:Ni:Cu:Ti＝1:1:1:1:0.4:0.4比例的高熵合金混合粉末，然后在球磨机中球磨20～24h。将混合好的粉末放入模具中，振动均匀且预压后，将模具置于真空热压烧结炉的炉腔内部进行加压烧结，烧结过程中压力维持在30～40MPa，抽真空至真空度为1.5x10-2pa，然后以10℃/min的升温速率从室温升至300℃，在300℃保温10min；再以10℃/min的升温速率从300℃升至1100℃，保温60min后降温卸压；将制备的毛胚依次进行表面磨削和去毛刺处理，制的真空热压烧结的x＝0.4的CoCrFeNi(CuTi)x高熵合金块体。Co powder, Cr powder, Fe powder, Ni powder, Cu powder, and Ti powder with a purity of 99% and a particle size of 44um are used as raw materials, weighed and mixed according to the equiatomic ratio, and configured as Co:Cr:Fe:Ni: Cu:Ti=1:1:1:1:0.4:0.4 high-entropy alloy mixed powder, and then ball milled in a ball mill for 20-24 hours. Put the mixed powder into the mold, vibrate evenly and pre-press, place the mold inside the cavity of the vacuum hot-press sintering furnace for pressure sintering, maintain the pressure at 30-40MPa during the sintering process, and evacuate to a vacuum degree 1.5x10 -2 Pa, then rise from room temperature to 300°C at a heating rate of 10°C/min, and keep at 300°C for 10 minutes; Lowering the temperature and releasing the pressure; performing surface grinding and deburring treatment on the prepared blank in sequence to prepare a CoCrFeNi(CuTi) x high-entropy alloy block with x=0.4 that was sintered by vacuum hot pressing.
其中球磨过程中过程控制剂的添加量为0.6％～1.2％，球料质量比为8～12：1，其中磨球分为大、中、小三型且直径为9.5mm、5mm以及3mm三种磨球；大、中、小三种磨球的质量比为2：3：5。The amount of process control agent added in the ball milling process is 0.6% to 1.2%, the mass ratio of ball to material is 8 to 12:1, and the grinding balls are divided into three types: large, medium and small, with diameters of 9.5mm, 5mm and 3mm. Grinding balls; the mass ratio of large, medium and small grinding balls is 2:3:5.
x＝0.4的CoCrFeNi(CuTi)x高熵合金材料试样打磨抛光后进行组织及性能测试，所得技术参数如表2所示；The CoCrFeNi(CuTi) x high-entropy alloy material sample of x=0.4 was ground and polished and tested for microstructure and performance, and the obtained technical parameters are shown in Table 2;
表2实施例1制备的高熵合金材料的性能测试结果The performance test results of the high-entropy alloy material prepared in Table 2 Example 1
实施例3Example 3
针对合金成分为x＝0.4的CoCrFeNi(CuTi)x高熵合金粉末进行烧结对比试验。A sintering comparison test was carried out for the CoCrFeNi(CuTi) x high-entropy alloy powder with an alloy composition of x=0.4.
采用纯度为99％且粒径为44um的Co粉、Cr粉、Fe粉、Ni粉、Cu粉、Ti粉作为原料，按照等原子比进行称量混合，配置成Co:Cr:Fe:Ni:Cu:Ti＝1:1:1:1:0.4:0.4比例的高熵合金混合粉末，然后在球磨机中球磨20～24h。将混合好的粉末放入模具中，振动均匀且预压后，将模具置于真空热压烧结炉的炉腔内部进行加压烧结，烧结过程中压力维持在30～40MPa，抽真空至真空度为1.5x10-2pa，然后以10℃/min的升温速率从室温升至300℃，在300℃保温10min；再以10℃/min的升温速率从300℃升至1150℃，保温60min后降温卸压；将制备的毛胚依次进行表面磨削和去毛刺处理，制的真空热压烧结的x＝0.4的CoCrFeNi(CuTi)x高熵合金块体。Co powder, Cr powder, Fe powder, Ni powder, Cu powder, and Ti powder with a purity of 99% and a particle size of 44um are used as raw materials, weighed and mixed according to the equiatomic ratio, and configured as Co:Cr:Fe:Ni: Cu:Ti=1:1:1:1:0.4:0.4 high-entropy alloy mixed powder, and then ball milled in a ball mill for 20-24 hours. Put the mixed powder into the mold, vibrate evenly and pre-press, place the mold inside the cavity of the vacuum hot-press sintering furnace for pressure sintering, maintain the pressure at 30-40MPa during the sintering process, and evacuate to a vacuum degree 1.5x10 -2 Pa, then rise from room temperature to 300°C at a heating rate of 10°C/min, and keep at 300°C for 10 minutes; Lowering the temperature and releasing the pressure; performing surface grinding and deburring treatment on the prepared rough blank in sequence to prepare a CoCrFeNi(CuTi)x high-entropy alloy block with x=0.4 and sintered by vacuum hot pressing.
其中球磨过程中过程控制剂的添加量为0.6％～1.2％，球料质量比为8～12：1，其中磨球分为大、中、小三型且直径为9.5mm、5mm以及3mm三种磨球；大、中、小三种磨球的质量比为2：3：5。The amount of process control agent added in the ball milling process is 0.6% to 1.2%, the mass ratio of ball to material is 8 to 12:1, and the grinding balls are divided into three types: large, medium and small, with diameters of 9.5mm, 5mm and 3mm. Grinding balls; the mass ratio of large, medium and small grinding balls is 2:3:5.
x＝0.4的CoCrFeNi(CuTi)x高熵合金材料试样打磨抛光后进行组织及性能测试，所得技术参数如表3所示；The CoCrFeNi(CuTi) x high-entropy alloy material sample of x=0.4 was ground and polished for microstructure and performance tests, and the obtained technical parameters are shown in Table 3;
表3实施例1制备的高熵合金材料的性能测试结果The performance test results of the high-entropy alloy material prepared in Table 3 Example 1
实施例4Example 4
针对合金成分为x＝0.4的CoCrFeNi(CuTi)x高熵合金粉末进行烧结对比试验。A sintering comparison test was carried out for the CoCrFeNi(CuTi) x high-entropy alloy powder with an alloy composition of x=0.4.
采用纯度为99％且粒径为44um的Co粉、Cr粉、Fe粉、Ni粉、Cu粉、Ti粉作为原料，按照等原子比进行称量混合，配置成Co:Cr:Fe:Ni:Cu:Ti＝1:1:1:1:0.4:0.4比例的高熵合金混合粉末，然后在球磨机中球磨20～24h。将混合好的粉末放入模具中，振动均匀且预压后，将模具置于真空热压烧结炉的炉腔内部进行加压烧结，烧结过程中压力维持在30～40MPa，抽真空至真空度为1.5x10-2pa，然后以10℃/min的升温速率从室温升至300℃，在300℃保温10min；再以10℃/min的升温速率从300℃升至1200℃，保温60min后降温卸压；将制备的毛胚依次进行表面磨削和去毛刺处理，制的真空热压烧结的x＝0.4的CoCrFeNi(CuTi)x高熵合金块体。Co powder, Cr powder, Fe powder, Ni powder, Cu powder, and Ti powder with a purity of 99% and a particle size of 44um are used as raw materials, weighed and mixed according to the equiatomic ratio, and configured as Co:Cr:Fe:Ni: Cu:Ti=1:1:1:1:0.4:0.4 high-entropy alloy mixed powder, and then ball milled in a ball mill for 20-24 hours. Put the mixed powder into the mold, vibrate evenly and pre-press, place the mold inside the cavity of the vacuum hot-press sintering furnace for pressure sintering, maintain the pressure at 30-40MPa during the sintering process, and evacuate to a vacuum degree 1.5x10 -2 Pa, then rise from room temperature to 300°C at a heating rate of 10°C/min, and keep at 300°C for 10 minutes; Lowering the temperature and releasing the pressure; performing surface grinding and deburring treatment on the prepared blank in sequence to prepare a CoCrFeNi(CuTi) x high-entropy alloy block with x=0.4 that was sintered by vacuum hot pressing.
其中球磨过程中过程控制剂的添加量为0.6％～1.2％，球料质量比为8～12：1，其中磨球分为大、中、小三型且直径为9.5mm、5mm以及3mm三种磨球；大、中、小三种磨球的质量比为2：3：5。The amount of process control agent added in the ball milling process is 0.6% to 1.2%, the mass ratio of ball to material is 8 to 12:1, and the grinding balls are divided into three types: large, medium and small, with diameters of 9.5mm, 5mm and 3mm. Grinding balls; the mass ratio of large, medium and small grinding balls is 2:3:5.
x＝0.4的CoCrFeNi(CuTi)x高熵合金材料试样打磨抛光后进行组织及性能测试，所得技术参数如表4所述；The CoCrFeNi(CuTi) x high-entropy alloy material sample of x=0.4 is ground and polished and tested for microstructure and performance, and the technical parameters obtained are as described in Table 4;
表4实施例1制备的高熵合金材料的性能测试结果The performance test results of the high-entropy alloy material prepared in Table 4 Example 1
实施例5Example 5
针对合金成分为x＝0.4的CoCrFeNi(CuTi)x高熵合金粉末进行烧结对比试验。A sintering comparison test was carried out for the CoCrFeNi(CuTi) x high-entropy alloy powder with an alloy composition of x=0.4.
采用纯度为99％且粒径为44um的Co粉、Cr粉、Fe粉、Ni粉、Cu粉、Ti粉作为原料，按照等原子比进行称量混合，配置成Co:Cr:Fe:Ni:Cu:Ti＝1:1:1:1:0.4:0.4比例的高熵合金混合粉末，然后在球磨机中球磨20～24h。将混合好的粉末放入模具中，振动均匀且预压后，将模具置于快速热压烧结炉的炉腔内部进行加压烧结，烧结过程中压力维持在30～40MPa，抽真空至真空度为1.2pa，然后以100℃/min的升温速率从室温升至300℃，在300℃保温10min；再以100℃/min的升温速率从300℃升至1000℃，保温30min后持续加压降温；将制备的毛胚依次进行表面磨削和去毛刺处理，制的真空热压烧结的x＝0.4的CoCrFeNi(CuTi)x高熵合金块体。Co powder, Cr powder, Fe powder, Ni powder, Cu powder, and Ti powder with a purity of 99% and a particle size of 44um are used as raw materials, weighed and mixed according to the equiatomic ratio, and configured as Co:Cr:Fe:Ni: Cu:Ti=1:1:1:1:0.4:0.4 high-entropy alloy mixed powder, and then ball milled in a ball mill for 20-24 hours. Put the mixed powder into the mold, vibrate evenly and pre-press, place the mold inside the cavity of the rapid hot-press sintering furnace for pressure sintering, maintain the pressure at 30-40MPa during the sintering process, and evacuate to a vacuum degree 1.2 Pa, then rise from room temperature to 300°C at a heating rate of 100°C/min, and keep at 300°C for 10 minutes; then rise at a heating rate of 100°C/min from 300°C to 1000°C, hold for 30 minutes and continue to pressurize Lowering the temperature; performing surface grinding and deburring treatment on the prepared blank in sequence to prepare a CoCrFeNi(CuTi) x high-entropy alloy block with x=0.4 that was sintered by vacuum hot pressing.
其中球磨过程中过程控制剂的添加量为0.6％～1.2％，球料质量比为8～12：1，其中磨球分为大、中、小三型且直径为9.5mm、5mm以及3mm三种磨球；大、中、小三种磨球的质量比为2：3：5。The amount of process control agent added in the ball milling process is 0.6% to 1.2%, the mass ratio of ball to material is 8 to 12:1, and the grinding balls are divided into three types: large, medium and small, with diameters of 9.5mm, 5mm and 3mm. Grinding balls; the mass ratio of large, medium and small grinding balls is 2:3:5.
x＝0.4的CoCrFeNi(CuTi)x高熵合金材料试样打磨抛光后进行组织及性能测试，所得技术参数如表5所示；The CoCrFeNi(CuTi) x high-entropy alloy material sample of x=0.4 was ground and polished and tested for microstructure and performance, and the obtained technical parameters are shown in Table 5;
表5实施例1制备的高熵合金材料的性能测试结果The performance test results of the high-entropy alloy material prepared in Table 5 Example 1
实施例6Example 6
针对合金成分为x＝0.4的CoCrFeNi(CuTi)x高熵合金粉末进行烧结对比试验。A sintering comparison test was carried out for the CoCrFeNi(CuTi) x high-entropy alloy powder with an alloy composition of x=0.4.
采用纯度为99％且粒径为44um的Co粉、Cr粉、Fe粉、Ni粉、Cu粉、Ti粉作为原料，按照等原子比进行称量混合，配置成Co:Cr:Fe:Ni:Cu:Ti＝1:1:1:1:0.4:0.4比例的高熵合金混合粉末，然后在球磨机中球磨20～24h。将混合好的粉末放入模具中，振动均匀且预压后，将模具置于快速热压烧结炉的炉腔内部进行加压烧结，烧结过程中压力维持在30～40MPa，抽真空至真空度为1.2pa，然后以100℃/min的升温速率从室温升至300℃，在300℃保温10min；再以100℃/min的升温速率从300℃升至1000℃，保温60min后持续加压降温；将制备的毛胚依次进行表面磨削和去毛刺处理，制的真空热压烧结的x＝0.4的CoCrFeNi(CuTi)x高熵合金块体。Co powder, Cr powder, Fe powder, Ni powder, Cu powder, and Ti powder with a purity of 99% and a particle size of 44um are used as raw materials, weighed and mixed according to the equiatomic ratio, and configured as Co:Cr:Fe:Ni: Cu:Ti=1:1:1:1:0.4:0.4 high-entropy alloy mixed powder, and then ball milled in a ball mill for 20-24 hours. Put the mixed powder into the mold, vibrate evenly and pre-press, place the mold inside the cavity of the rapid hot-press sintering furnace for pressure sintering, maintain the pressure at 30-40MPa during the sintering process, and evacuate to a vacuum degree 1.2pa, then rise from room temperature to 300°C at a heating rate of 100°C/min, and keep at 300°C for 10 minutes; then rise at a heating rate of 100°C/min from 300°C to 1000°C, hold for 60 minutes and continue to pressurize Lowering the temperature; performing surface grinding and deburring treatment on the prepared blank in sequence to prepare a CoCrFeNi(CuTi) x high-entropy alloy block with x=0.4 that was sintered by vacuum hot pressing.
其中球磨过程中过程控制剂的添加量为0.6％～1.2％，球料质量比为8～12：1，其中磨球分为大、中、小三型且直径为9.5mm、5mm以及3mm三种磨球；大、中、小三种磨球的质量比为2：3：5。The amount of process control agent added in the ball milling process is 0.6% to 1.2%, the mass ratio of ball to material is 8 to 12:1, and the grinding balls are divided into three types: large, medium and small, with diameters of 9.5mm, 5mm and 3mm. Grinding balls; the mass ratio of large, medium and small grinding balls is 2:3:5.
x＝0.4的CoCrFeNi(CuTi)x高熵合金材料试样打磨抛光后进行组织及性能测试，所得技术参数如表6所示；The CoCrFeNi(CuTi) x high-entropy alloy material sample of x=0.4 was ground and polished for microstructure and performance tests, and the obtained technical parameters are shown in Table 6;
表6实施例1制备的高熵合金材料的性能测试结果The performance test results of the high-entropy alloy material prepared in Table 6 Example 1
实施例3、实施例5以及实施例6制备的x＝0.4的CoCrFeNi(CuTi)x高熵合金的金相OM图和SEM图如图1、图2以及图3所示；其中，图1、图2以及图3中的a为金相图，图1、图2以及图3中的b为SEM图；其中图1(a)和(b)是实施例3的微观组织图，图2(a)和(b)是实施例5的微观组织图，图3(a)和(b)是实施例6的微观组织图，由图1、图2以及图3可以看出x＝0.4的CoCrFeNi(CuTi)x高熵合金块体组织非常均匀且致密度也越来越高，而且也发现真空热压烧结的最佳烧结温度要比快速热压烧结高150℃左右，究其原因可能与其两种设备的加热方式有关。The metallographic OM diagram and SEM diagram of the CoCrFeNi(CuTi) x high-entropy alloy of x=0.4 prepared in embodiment 3, embodiment 5 and embodiment 6 are shown in Fig. 1, Fig. 2 and Fig. 3; Wherein, Fig. 1, A among Fig. 2 and Fig. 3 is metallographic diagram, and b among Fig. 1, Fig. 2 and Fig. 3 is SEM figure; Wherein Fig. 1 (a) and (b) are the microstructure diagram of embodiment 3, Fig. 2 ( a) and (b) are microstructure diagrams of embodiment 5, and Fig. 3 (a) and (b) are microstructure diagrams of embodiment 6, as can be seen from Fig. 1, Fig. 2 and Fig. 3 CoCrFeNi of x=0.4 (CuTi) x high-entropy alloy bulk structure is very uniform and the density is getting higher and higher, and it is also found that the optimal sintering temperature of vacuum hot-pressing sintering is about 150 °C higher than that of rapid hot-pressing sintering. It depends on the heating method of the equipment.
本发明的双元素等量变换的高熵合金真空热压烧结与快速热压烧结成型工艺采用真空热压烧结和快速热压烧结两种烧结炉进行烧结，使球磨混合均匀的高熵合金粉末在热和力的共同作用下烧结成型，从而得到最佳烧结工艺，制备出所需的各种成分的合金块体。该方法制备的高熵合金块体致密度高、成分均匀、晶粒细小、成本低，能够满足大规模的产业化要求，为未来高熵合金产业化发展具有重要的研究指导价值。The high-entropy alloy vacuum hot-pressing sintering and rapid hot-pressing sintering molding process of the double-element equivalent transformation of the present invention adopts vacuum hot-pressing sintering and rapid hot-pressing sintering two sintering furnaces for sintering, so that the high-entropy alloy powder mixed uniformly by ball milling is Sintering and molding under the joint action of heat and force, so as to obtain the best sintering process, and prepare alloy blocks with various components required. The high-entropy alloy block prepared by this method has high density, uniform composition, fine grains, and low cost, which can meet the requirements of large-scale industrialization and has important research and guiding value for the future industrialization of high-entropy alloys.
本发明是一种短流程，成本低，粉末不易氧化，致密度高，能有效控制晶粒尺寸，成分均匀，规模尺寸大的高熵合金真空热压烧结与快速热压烧结成型工艺。The invention is a high-entropy alloy vacuum hot-press sintering and rapid hot-press sintering molding process with short process, low cost, difficult oxidation, high density, effective control of grain size, uniform composition and large scale.
本发明提供的制备方法简单，致密度高，生产成本低，组织均匀有效避免成分偏析且能够在较低的烧结温度下即可得到硬度和韧性均较高的CoCrFeNi基高熵合金块体材料。The preparation method provided by the invention is simple, high in density, low in production cost, uniform in structure, effectively avoids component segregation, and can obtain a CoCrFeNi-based high-entropy alloy block material with high hardness and toughness at a relatively low sintering temperature.
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