CN110465666A - The preparation method of nano-interface and ultra micro crystal grain tungsten alloy material - Google Patents
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- 229910001080 W alloy Inorganic materials 0.000 title claims abstract description 73
- 239000000956 alloy Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000013081 microcrystal Substances 0.000 title claims 10
- 238000005245 sintering Methods 0.000 claims abstract description 34
- 238000005098 hot rolling Methods 0.000 claims abstract description 28
- 238000011084 recovery Methods 0.000 claims abstract description 17
- 238000001953 recrystallisation Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 230000004913 activation Effects 0.000 claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims description 13
- 238000005452 bending Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 230000006835 compression Effects 0.000 claims 1
- 238000007906 compression Methods 0.000 claims 1
- 230000035485 pulse pressure Effects 0.000 abstract description 27
- 238000000034 method Methods 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 9
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 238000007731 hot pressing Methods 0.000 description 15
- 238000004321 preservation Methods 0.000 description 12
- 230000006872 improvement Effects 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 6
- 238000001994 activation Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
本发明公开了一种纳米界面与超微晶粒钨合金材料的制备方法，先将纳米钨粉进行三级对辊热轧处理，然后进行回复再结晶热处理，对得到的纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，最终得到纳米界面与超微晶粒钨合金材料材料。此方法具有成分控制精度高，工艺稳定性和重复性较强，可实现钨合金材料的高效回收利用和抗高温性能。The invention discloses a preparation method of a nano-interface and ultrafine-grain tungsten alloy material. First, the nano-tungsten powder is subjected to three-stage double-roll hot rolling treatment, and then the recovery and recrystallization heat treatment is performed, and the obtained nano-crystalline tungsten alloy sheet is subjected to Double-sided activation, and finally placed in a biaxial pulse pressure sintering device for rapid hot-press forming, and finally obtained a nano-interface and ultra-fine grain tungsten alloy material. This method has high composition control precision, strong process stability and repeatability, and can realize efficient recycling and high temperature resistance of tungsten alloy materials.
Description
技术领域technical field
本发明涉及钨合金制备技术领域，特别涉及一种纳米界面与超微晶粒钨合金材料的制备方法。The invention relates to the technical field of tungsten alloy preparation, in particular to a preparation method of a nano-interface and ultrafine grain tungsten alloy material.
背景技术Background technique
钨合金主要由单质钨和其他合金元素及化合物组成，广泛应用于航空航天、军工、核工业等领域。因合金化后的相组成较复杂，使其难以回收利用，造成钨资源浪费，并且低熔点合金组元限制钨合金的高温应用。因此，寻找一种新方法，解决钨合金难回收的问题，并提高其高温性能至关重要。Tungsten alloy is mainly composed of elemental tungsten and other alloy elements and compounds, and is widely used in aerospace, military, nuclear industry and other fields. Due to the complex phase composition after alloying, it is difficult to recycle, resulting in waste of tungsten resources, and the low melting point alloy components limit the high temperature application of tungsten alloys. Therefore, it is very important to find a new method to solve the problem of difficult recycling of tungsten alloy and improve its high temperature performance.
通过合金纯化设计、热加工处理、化学处理和热压烧结工艺，尽量实现合金元素的零添加，是解决钨合金难回收的问题，并提高其高温性能的关键手段。Through alloy purification design, thermal processing, chemical treatment and hot pressing sintering process, it is a key means to solve the problem of difficult recycling of tungsten alloy and improve its high temperature performance to achieve zero addition of alloy elements.
发明内容Contents of the invention
本发明是针对常见手段难以有效解决解决钨合金难回收的问题，并提高其高温性能的研发领域现状，提供一种纳米界面与超微晶粒钨合金材料的制备方法。The present invention is aimed at the current situation in the field of research and development in which common means are difficult to effectively solve the problem of difficult recovery of tungsten alloys and improve its high-temperature performance, and provides a preparation method of nano-interface and ultrafine-grain tungsten alloy materials.
为达到以上目的，本发明是采取如下技术方案予以实现的：To achieve the above object, the present invention is achieved by taking the following technical solutions:
一种纳米界面与超微晶粒钨合金材料的制备方法，包括以下步骤：A method for preparing a nano-interface and ultrafine-grain tungsten alloy material, comprising the following steps:
1)将纳米钨粉进行三级对辊热轧处理，然后进行回复再结晶热处理，得到纳米晶钨合金薄板；1) The nano-tungsten powder is subjected to three-stage double-roll hot rolling treatment, and then the recovery and recrystallization heat treatment is performed to obtain a nano-crystalline tungsten alloy sheet;
2)对纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，最终得到纳米界面与超微晶粒钨合金材料。2) Activate the nanocrystalline tungsten alloy sheet on both sides, and finally place it in a biaxial pulse pressure sintering device for rapid hot-press forming, and finally obtain a nano-interface and ultra-fine-grain tungsten alloy material.
作为本发明的进一步改进，对辊线速度0.2～0.32米/分。As a further improvement of the present invention, the line speed of the pair of rolls is 0.2-0.32 m/min.
作为本发明的进一步改进，三级热轧温度分别为450℃、550℃和760℃，辊缝宽度分别为12、10和6毫米。As a further improvement of the present invention, the three-stage hot rolling temperatures are 450°C, 550°C and 760°C respectively, and the roll gap widths are 12, 10 and 6 mm respectively.
作为本发明的进一步改进，回复再结晶温度1000～1250℃，时间80～110分钟。As a further improvement of the present invention, the recovery and recrystallization temperature is 1000-1250° C., and the time is 80-110 minutes.
作为本发明的进一步改进，薄板双面活化采用1:1的浓盐酸、浓硝酸溶液。As a further improvement of the present invention, a 1:1 solution of concentrated hydrochloric acid and concentrated nitric acid is used for activation of both sides of the thin plate.
作为本发明的进一步改进，双轴脉冲压力烧结温度1500～1650℃，压力15～25MPa，保温与保压时间14～22分钟。As a further improvement of the present invention, the biaxial pulse pressure sintering temperature is 1500-1650° C., the pressure is 15-25 MPa, and the heat preservation and pressure holding time is 14-22 minutes.
作为本发明的进一步改进，制得的钨合金材料具有纳米界面与超微晶结构，材料的冲击韧性大于等于28.5MPa·m1/2，显微硬度大于等于10.5GPa，弯曲强度大于等于1540MPa，高温(1000℃)抗压强度大于等于5250MPa。As a further improvement of the present invention, the prepared tungsten alloy material has a nano-interface and ultrafine crystal structure, the impact toughness of the material is greater than or equal to 28.5MPa·m 1/2 , the microhardness is greater than or equal to 10.5GPa, and the bending strength is greater than or equal to 1540MPa. High temperature (1000°C) compressive strength greater than or equal to 5250MPa.
与现有技术相比，本发明具有以下特点和优势：Compared with the prior art, the present invention has the following characteristics and advantages:
本发明先将纳米钨粉进行三级对辊热轧处理，然后进行回复再结晶热处理，对得到的纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形；其中三级对辊热轧处理有利于坯体的初始致密化，并通过较低轧制温度抑制钨晶粒长大，保存纳米尺度。合金薄板双面活化便于烧结时原子快速扩散，排除缺陷。双轴脉冲压力烧结装置可使钨合金坯体快速成形，达到良好的细晶效果。本发明制得的钨合金材料具有纳米界面与超微晶结构，材料的冲击韧性大于等于28.5MPa·m1/2，显微硬度大于等于10.5GPa，弯曲强度大于等于1540MPa，高温(1000℃)抗压强度大于等于5250MPa。此方法具有成分控制精度高，工艺稳定性和重复性较强，可实现钨合金材料的强韧化和耐高温性能。In the present invention, the nano-tungsten powder is subjected to three-stage double-roll hot rolling treatment, and then the recovery and recrystallization heat treatment is performed, and the obtained nano-crystalline tungsten alloy sheet is activated on both sides, and finally placed in a biaxial pulse pressure sintering device for rapid hot-press forming ; Among them, the three-stage double-roller hot rolling treatment is beneficial to the initial densification of the green body, and suppresses the growth of tungsten grains through the lower rolling temperature, and preserves the nanoscale. Double-sided activation of the alloy sheet facilitates the rapid diffusion of atoms during sintering and eliminates defects. The biaxial pulse pressure sintering device can make the tungsten alloy blank form rapidly and achieve a good fine grain effect. The tungsten alloy material prepared by the present invention has a nano-interface and an ultrafine crystal structure, the impact toughness of the material is greater than or equal to 28.5MPa·m 1/2 , the microhardness is greater than or equal to 10.5GPa, and the bending strength is greater than or equal to 1540MPa. The compressive strength is greater than or equal to 5250MPa. This method has high composition control precision, strong process stability and repeatability, and can realize the toughening and high temperature resistance of tungsten alloy materials.
进一步，在制备钨合金材料过程中，本发明为解决已有方法难以有效解决解决钨合金难回收的问题，并提高其高温性能的问题，而是采用一种合金纯化设计、热加工处理、化学处理和热压烧结工艺，研究热加工工艺、化学活化工艺、热压烧结工艺和钨合金强韧性、高温力学性能的关系，即：对于钨合金材料，保持较高强韧性和高温力学性能的最佳热加工工艺、化学活化工艺、热压烧结工艺。Further, in the process of preparing tungsten alloy materials, the present invention adopts an alloy purification design, thermal processing, chemical Treatment and hot-pressing sintering process, to study the relationship between thermal processing process, chemical activation process, hot-pressing sintering process and tungsten alloy strength, toughness, and high-temperature mechanical properties, that is, for tungsten alloy materials, the best way to maintain high strength, toughness, and high-temperature mechanical properties Thermal processing process, chemical activation process, hot pressing sintering process.
具体实施方式Detailed ways
本发明一种纳米界面与超微晶粒钨合金材料的制备方法，包括下述步骤：A method for preparing a nano-interface and ultrafine-grain tungsten alloy material of the present invention comprises the following steps:
(1)将纳米钨粉进行三级对辊热轧处理，对辊线速度0.2～0.32米/分，三级热轧温度分别为450℃、550℃和760℃，辊缝宽度分别为12、10和6毫米，然后在温度1000～1250℃下进行回复再结晶热处理，得到纳米晶钨合金薄板；(1) The nano-tungsten powder is subjected to three-stage hot-rolling treatment, the line speed of the pair of rolls is 0.2-0.32 m/min, the three-stage hot-rolling temperatures are 450°C, 550°C and 760°C, and the roll gap widths are 12, 10 and 6 mm, and then undergo recovery and recrystallization heat treatment at a temperature of 1000-1250 ° C to obtain nanocrystalline tungsten alloy sheets;
(2)采用1:1的浓盐酸、浓硝酸溶液对纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，双轴脉冲压力烧结温度1500～1650℃，压力15～25MPa，保温与保压时间14～22分钟，最终得到纳米界面与超微晶粒钨合金材料。(2) Use 1:1 concentrated hydrochloric acid and concentrated nitric acid solution to activate the nanocrystalline tungsten alloy sheet on both sides, and finally place it in a biaxial pulse pressure sintering device for rapid hot pressing. The biaxial pulse pressure sintering temperature is 1500-1650 °C , the pressure is 15-25 MPa, the heat preservation and pressure holding time is 14-22 minutes, and finally the nano-interface and ultra-fine grain tungsten alloy material is obtained.
以下实施例制备的钨合金材料的韧性和高温性能如表1所示。The toughness and high temperature properties of the tungsten alloy materials prepared in the following examples are shown in Table 1.
实施例1Example 1
(1)将纳米钨粉进行三级对辊热轧处理，对辊线速度0.2米/分，三级热轧温度分别为450℃、550℃和760℃，辊缝宽度分别为12、10和6毫米，然后在温度1000℃下进行回复再结晶热处理，得到纳米晶钨合金薄板；(1) The nano-tungsten powder is subjected to three-stage hot-rolling treatment, with a line speed of 0.2 m/min, three-stage hot-rolling temperatures of 450°C, 550°C, and 760°C, and roll gap widths of 12, 10, and 6 mm, and then undergo recovery and recrystallization heat treatment at a temperature of 1000 ° C to obtain a nanocrystalline tungsten alloy sheet;
(2)采用1:1的浓盐酸、浓硝酸溶液对纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，双轴脉冲压力烧结温度1500℃，压力15MPa，保温与保压时间14分钟，最终得到纳米界面与超微晶粒钨合金材料。(2) Use 1:1 concentrated hydrochloric acid and concentrated nitric acid solution to activate the nanocrystalline tungsten alloy sheet on both sides, and finally place it in a biaxial pulse pressure sintering device for rapid hot pressing. The biaxial pulse pressure sintering temperature is 1500 ° C, the pressure 15MPa, heat preservation and pressure holding time of 14 minutes, finally obtained nano-interface and ultra-fine grain tungsten alloy material.
实施例2Example 2
(1)将纳米钨粉进行三级对辊热轧处理，对辊线速度0.22米/分，三级热轧温度分别为450℃、550℃和760℃，辊缝宽度分别为12、10和6毫米，然后在温度1050℃下进行回复再结晶热处理，得到纳米晶钨合金薄板；(1) The nano-tungsten powder is subjected to three-stage hot-rolling treatment, the line speed of the pair of rolls is 0.22 m/min, the three-stage hot-rolling temperatures are 450 ° C, 550 ° C and 760 ° C, and the roll gap widths are 12, 10 and 10 respectively. 6 mm, and then undergo recovery and recrystallization heat treatment at a temperature of 1050 ° C to obtain a nanocrystalline tungsten alloy sheet;
(2)采用1:1的浓盐酸、浓硝酸溶液对纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，双轴脉冲压力烧结温度1550℃，压力17MPa，保温与保压时间16分钟，最终得到纳米界面与超微晶粒钨合金材料。(2) Use 1:1 concentrated hydrochloric acid and concentrated nitric acid solution to activate the nanocrystalline tungsten alloy sheet on both sides, and finally place it in a biaxial pulse pressure sintering device for rapid hot pressing. The biaxial pulse pressure sintering temperature is 1550 °C and the pressure 17MPa, heat preservation and pressure holding time of 16 minutes, finally obtained nano-interface and ultra-fine grain tungsten alloy material.
实施例3Example 3
(1)将纳米钨粉进行三级对辊热轧处理，对辊线速度0.24米/分，三级热轧温度分别为450℃、550℃和760℃，辊缝宽度分别为12、10和6毫米，然后在温度1100℃下进行回复再结晶热处理，得到纳米晶钨合金薄板；(1) The nano-tungsten powder is subjected to three-stage hot-rolling treatment, the line speed of the pair of rolls is 0.24 m/min, the three-stage hot-rolling temperatures are 450°C, 550°C and 760°C, and the roll gap widths are 12, 10 and 10 respectively. 6 mm, and then undergo recovery and recrystallization heat treatment at a temperature of 1100 ° C to obtain a nanocrystalline tungsten alloy sheet;
(2)采用1:1的浓盐酸、浓硝酸溶液对纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，双轴脉冲压力烧结温度1600℃，压力19MPa，保温与保压时间18分钟，最终得到纳米界面与超微晶粒钨合金材料。(2) Use 1:1 concentrated hydrochloric acid and concentrated nitric acid solution to activate the nanocrystalline tungsten alloy sheet on both sides, and finally place it in a biaxial pulse pressure sintering device for rapid hot pressing. The biaxial pulse pressure sintering temperature is 1600 °C and the pressure 19MPa, heat preservation and pressure holding time of 18 minutes, finally obtained nano-interface and ultra-fine grain tungsten alloy material.
实施例4Example 4
(1)将纳米钨粉进行三级对辊热轧处理，对辊线速度0.26米/分，三级热轧温度分别为450℃、550℃和760℃，辊缝宽度分别为12、10和6毫米，然后在温度1150℃下进行回复再结晶热处理，得到纳米晶钨合金薄板；(1) The nano-tungsten powder is subjected to three-stage hot-rolling treatment, with a line speed of 0.26 m/min, three-stage hot-rolling temperatures of 450°C, 550°C, and 760°C, and roll gap widths of 12, 10, and 6 mm, and then undergo recovery and recrystallization heat treatment at a temperature of 1150 ° C to obtain a nanocrystalline tungsten alloy sheet;
(2)采用1:1的浓盐酸、浓硝酸溶液对纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，双轴脉冲压力烧结温度1550℃，压力15MPa，保温与保压时间19分钟，最终得到纳米界面与超微晶粒钨合金材料。(2) Use 1:1 concentrated hydrochloric acid and concentrated nitric acid solution to activate the nanocrystalline tungsten alloy sheet on both sides, and finally place it in a biaxial pulse pressure sintering device for rapid hot pressing. The biaxial pulse pressure sintering temperature is 1550 °C and the pressure 15MPa, heat preservation and pressure holding time of 19 minutes, finally obtained nano-interface and ultra-fine grain tungsten alloy material.
实施例1～4制备钨合金材料的性能参数见表1所示：Embodiment 1～4 prepares the performance parameter of tungsten alloy material as shown in Table 1:
表1Table 1
从上表可以得出，本发明制得的钨合金材料具有纳米界面与超微晶结构，材料的冲击韧性大于等于28.5MPa·m1/2，显微硬度大于等于10.5GPa，弯曲强度大于等于1540MPa，高温(1000℃)抗压强度大于等于5250MPa。It can be concluded from the above table that the tungsten alloy material prepared by the present invention has nano interface and ultrafine crystal structure, the impact toughness of the material is greater than or equal to 28.5MPa·m 1/2 , the microhardness is greater than or equal to 10.5GPa, and the bending strength is greater than or equal to 1540MPa, high temperature (1000°C) compressive strength greater than or equal to 5250MPa.
实施例5Example 5
(1)将纳米钨粉进行三级对辊热轧处理，对辊线速度0.28米/分，三级热轧温度分别为450℃、550℃和760℃，辊缝宽度分别为12、10和6毫米，然后在温度1250℃下进行回复再结晶热处理，得到纳米晶钨合金薄板；(1) The nano-tungsten powder is subjected to three-stage hot-rolling treatment, the line speed of the pair of rolls is 0.28 m/min, the three-stage hot-rolling temperatures are 450°C, 550°C and 760°C, and the roll gap widths are 12, 10 and 10 respectively. 6 mm, and then undergo recovery and recrystallization heat treatment at a temperature of 1250 ° C to obtain a nanocrystalline tungsten alloy sheet;
(2)采用1:1的浓盐酸、浓硝酸溶液对纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，双轴脉冲压力烧结温度1650℃，压力25MPa，保温与保压时间22分钟，最终得到纳米界面与超微晶粒钨合金材料。(2) Use 1:1 concentrated hydrochloric acid and concentrated nitric acid solution to activate the nanocrystalline tungsten alloy sheet on both sides, and finally place it in a biaxial pulse pressure sintering device for rapid hot pressing. The biaxial pulse pressure sintering temperature is 1650 ° C, pressure 25MPa, heat preservation and pressure holding time of 22 minutes, finally obtained nano-interface and ultra-fine grain tungsten alloy material.
实施例6Example 6
(1)将纳米钨粉进行三级对辊热轧处理，对辊线速度0.3米/分，三级热轧温度分别为450℃、550℃和760℃，辊缝宽度分别为12、10和6毫米，然后在温度1250℃下进行回复再结晶热处理，得到纳米晶钨合金薄板；(1) The nano-tungsten powder is subjected to three-stage hot-rolling treatment, with a line speed of 0.3 m/min, three-stage hot-rolling temperatures of 450°C, 550°C, and 760°C, and roll gap widths of 12, 10, and 6 mm, and then undergo recovery and recrystallization heat treatment at a temperature of 1250 ° C to obtain a nanocrystalline tungsten alloy sheet;
(2)采用1:1的浓盐酸、浓硝酸溶液对纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，双轴脉冲压力烧结温度1570℃，压力19MPa，保温与保压时间18分钟，最终得到纳米界面与超微晶粒钨合金材料。(2) Use 1:1 concentrated hydrochloric acid and concentrated nitric acid solution to activate the nanocrystalline tungsten alloy sheet on both sides, and finally place it in a biaxial pulse pressure sintering device for rapid hot pressing. The biaxial pulse pressure sintering temperature is 1570 °C and the pressure 19MPa, heat preservation and pressure holding time of 18 minutes, finally obtained nano-interface and ultra-fine grain tungsten alloy material.
实施例7Example 7
(1)将纳米钨粉进行三级对辊热轧处理，对辊线速度0.32米/分，三级热轧温度分别为450℃、550℃和760℃，辊缝宽度分别为12、10和6毫米，然后在温度1250℃下进行回复再结晶热处理，得到纳米晶钨合金薄板；(1) The nano-tungsten powder is subjected to three-stage hot-rolling treatment, with a line speed of 0.32 m/min, three-stage hot-rolling temperatures of 450°C, 550°C, and 760°C, and roll gap widths of 12, 10, and 6 mm, and then undergo recovery and recrystallization heat treatment at a temperature of 1250 ° C to obtain a nanocrystalline tungsten alloy sheet;
(2)采用1:1的浓盐酸、浓硝酸溶液对纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，双轴脉冲压力烧结温度1650℃，压力25MPa，保温与保压时间22分钟，最终得到纳米界面与超微晶粒钨合金材料。(2) Use 1:1 concentrated hydrochloric acid and concentrated nitric acid solution to activate the nanocrystalline tungsten alloy sheet on both sides, and finally place it in a biaxial pulse pressure sintering device for rapid hot pressing. The biaxial pulse pressure sintering temperature is 1650 ° C, pressure 25MPa, heat preservation and pressure holding time of 22 minutes, finally obtained nano-interface and ultra-fine grain tungsten alloy material.
实施例8Example 8
(1)将纳米钨粉进行三级对辊热轧处理，对辊线速度0.32米/分，三级热轧温度分别为450℃、550℃和760℃，辊缝宽度分别为12、10和6毫米，然后在温度1210℃下进行回复再结晶热处理，得到纳米晶钨合金薄板；(1) The nano-tungsten powder is subjected to three-stage hot-rolling treatment, with a line speed of 0.32 m/min, three-stage hot-rolling temperatures of 450°C, 550°C, and 760°C, and roll gap widths of 12, 10, and 6 mm, and then undergo recovery and recrystallization heat treatment at a temperature of 1210 ° C to obtain a nanocrystalline tungsten alloy sheet;
(2)采用1:1的浓盐酸、浓硝酸溶液对纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，双轴脉冲压力烧结温度1630℃，压力25MPa，保温与保压时间22分钟，最终得到纳米界面与超微晶粒钨合金材料。(2) Use 1:1 concentrated hydrochloric acid and concentrated nitric acid solution to activate the nanocrystalline tungsten alloy sheet on both sides, and finally place it in a biaxial pulse pressure sintering device for rapid hot pressing. The biaxial pulse pressure sintering temperature is 1630 ° C, the pressure 25MPa, heat preservation and pressure holding time of 22 minutes, finally obtained nano-interface and ultra-fine grain tungsten alloy material.
实施例9Example 9
(1)将纳米钨粉进行三级对辊热轧处理，对辊线速度0.2米/分，三级热轧温度分别为450℃、550℃和760℃，辊缝宽度分别为12、10和6毫米，然后在温度1000℃下进行回复再结晶热处理，得到纳米晶钨合金薄板；(1) The nano-tungsten powder is subjected to three-stage hot-rolling treatment, with a line speed of 0.2 m/min, three-stage hot-rolling temperatures of 450°C, 550°C, and 760°C, and roll gap widths of 12, 10, and 6 mm, and then undergo recovery and recrystallization heat treatment at a temperature of 1000 ° C to obtain a nanocrystalline tungsten alloy sheet;
(2)采用1:1的浓盐酸、浓硝酸溶液对纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，双轴脉冲压力烧结温度1500℃，压力15MPa，保温与保压时间14分钟，最终得到纳米界面与超微晶粒钨合金材料。(2) Use 1:1 concentrated hydrochloric acid and concentrated nitric acid solution to activate the nanocrystalline tungsten alloy sheet on both sides, and finally place it in a biaxial pulse pressure sintering device for rapid hot pressing. The biaxial pulse pressure sintering temperature is 1500 ° C, the pressure 15MPa, heat preservation and pressure holding time of 14 minutes, finally obtained nano-interface and ultra-fine grain tungsten alloy material.
实施例10Example 10
(1)将纳米钨粉进行三级对辊热轧处理，对辊线速度0.32米/分，三级热轧温度分别为450℃、550℃和760℃，辊缝宽度分别为12、10和6毫米，然后在温度1250℃下进行回复再结晶热处理，得到纳米晶钨合金薄板；(1) The nano-tungsten powder is subjected to three-stage hot-rolling treatment, with a line speed of 0.32 m/min, three-stage hot-rolling temperatures of 450°C, 550°C, and 760°C, and roll gap widths of 12, 10, and 6 mm, and then undergo recovery and recrystallization heat treatment at a temperature of 1250 ° C to obtain a nanocrystalline tungsten alloy sheet;
(2)采用1:1的浓盐酸、浓硝酸溶液对纳米晶钨合金薄板进行双面活化，最后置于双轴脉冲压力烧结装置中快速热压成形，双轴脉冲压力烧结温度1650℃，压力25MPa，保温与保压时间22分钟，最终得到纳米界面与超微晶粒钨合金材料。(2) Use 1:1 concentrated hydrochloric acid and concentrated nitric acid solution to activate the nanocrystalline tungsten alloy sheet on both sides, and finally place it in a biaxial pulse pressure sintering device for rapid hot pressing. The biaxial pulse pressure sintering temperature is 1650 ° C, pressure 25MPa, heat preservation and pressure holding time of 22 minutes, finally obtained nano-interface and ultra-fine grain tungsten alloy material.
实施例5～10制备钨合金材料的性能参数见表2所示：Embodiment 5～10 prepares the performance parameter of tungsten alloy material as shown in Table 2:
表2Table 2
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以作出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。The above is only a preferred embodiment of the present invention, it should be pointed out that for those of ordinary skill in the art, without departing from the principle of the present invention, some improvements and modifications can also be made, and these improvements and modifications should also be It is regarded as the protection scope of the present invention.
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