CN113913637A - 一种具有室温韧性块体钨材料的制备方法 - Google Patents
一种具有室温韧性块体钨材料的制备方法 Download PDFInfo
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 82
- 239000010937 tungsten Substances 0.000 title claims abstract description 82
- 239000000463 material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 238000000137 annealing Methods 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 15
- 238000005242 forging Methods 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 10
- 229910001080 W alloy Inorganic materials 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000011812 mixed powder Substances 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 4
- 230000007704 transition Effects 0.000 abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 238000005728 strengthening Methods 0.000 description 5
- 229920001169 thermoplastic Polymers 0.000 description 4
- 239000004416 thermosoftening plastic Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- B22F3/10—Sintering only
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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
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- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
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- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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Abstract
本发明属于制备方法,具体涉及一种具有室温韧性块体钨材料的制备方法。一种具有室温韧性块体钨材料的制备方法,包括:步骤1:制备粉末及烧结;制备钨材料粉末,并将粉末烧结到指定尺寸,形成颗粒弥散强化钨合金棒;步骤2:加热;将烧结后产物加热并锻打加工;步骤3:退火;对锻打完成的产品进行退火。本发明的显著效果是:本发明能有效的降低钨材料中的氧含量,同时使钨材料塑性和强度得到显著提高。通过该工艺制备得到的钨块体材料具备明显的纤维织构,可以使钨材料的韧‑脆转变温度降低到室温,即在室温下就能发生明显的塑性变形。该工艺路线是在传统钨材料的制备方法上通过改良提到,适合进行规模化制备。
Description
技术领域
本发明属于制备方法,具体涉及一种具有室温韧性块体钨材料的制备方法。
背景技术
钨具有高的熔点、良好的热导率、低蒸汽压及低溅射率等优点,这使其成为国际热核聚变实验堆及未来聚变装置最有前景的面对等离子体材料之一。但是目前的纯钨及钨合金均存在烧结致密度较低、韧-脆转变温度高、加工性能差等缺陷,不能应对未来聚变堆中第一壁材料严酷的使用环境。虽然通过添加弥散强化物(主要是氧化物及碳化物)可以改善钨的部分性能,但钨合仍存在韧-脆转变温度过高的致命缺陷。
通过热塑性加工的方法可以提高钨及钨合金的致密度并能在一定程度上降低钨的韧-脆转变温度。但在钨材料制备过程中混入的杂质氧及在钨中添加的各种弥散颗粒会导致材料的硬度升高,从而使热塑性加工较为困难,且韧-脆转变温度的降低十分有限。
发明内容
本发明的内容是针对现有技术的缺陷,提供一种具有室温韧性块体钨材料的制备方法,使钨材料的韧-脆转变温度降低到室温并使钨材料具有很高的室温强度。
本发明是这样实现的:一种具有室温韧性块体钨材料的制备方法,包括:
步骤1:制备粉末及烧结
制备钨材料粉末,并将粉末烧结到指定尺寸,形成颗粒弥散强化钨合金棒;
步骤2:加热
将烧结后产物加热并锻打加工;
步骤3:退火
对锻打完成的产品进行退火。
如上所述的一种具有室温韧性块体钨材料的制备方法,其中,所述的制备粉末是指通过球磨方法制备粉末。
如上所述的一种具有室温韧性块体钨材料的制备方法,其中,所述的制备粉末是指制备出Y2O3质量比为0.7%的W-Y2O3混合粉末。
如上所述的一种具有室温韧性块体钨材料的制备方法,其中,所述的烧结是指在氢气烧结炉中进行烧结。
如上所述的一种具有室温韧性块体钨材料的制备方法,其中,所述的烧结是指烧结温度2150℃,时间3h。
如上所述的一种具有室温韧性块体钨材料的制备方法,其中,所述的烧结到指定尺寸是指烧结坯的致密度为95%;烧结坯尺寸为直径40mm,长度大于500mm。
如上所述的一种具有室温韧性块体钨材料的制备方法,其中,所述的加热锻打是指将烧结坯放入氢气炉中加热,加热温度1400~1600℃;然后将加热过的钨烧结坯放入旋锻设备上进行反复的锻打加工,每次变形量约为8%,最终钨烧结坯被锻打成直径16mm的细长钨棒,变形量约为65~85%。
如上所述的一种具有室温韧性块体钨材料的制备方法,其中,所述的退火是指将钨棒放入退火炉中进行去应力退火,在1100℃条件下退火1h。
如上所述的一种具有室温韧性块体钨材料的制备方法,其中,所述的颗粒弥散物为氧化物颗粒。
本发明的显著效果是:本发明能有效的降低钨材料中的氧含量,同时使钨材料塑性和强度得到显著提高。通过该工艺制备得到的钨块体材料具备明显的纤维织构,可以使钨材料的韧-脆转变温度降低到室温,即在室温下就能发生明显的塑性变形。该工艺路线是在传统钨材料的制备方法上通过改良提到,适合进行规模化制备。
具体实施方式
一种具有室温韧性的块体钨材料的制备方法,其特征在于通过氢气烧结制备出具有一定长度(>500mm)的颗粒弥散强化钨合金棒;将烧结坯在氢气气氛下整体加热至1400~1600℃,并通过旋锻方法进行热塑性加工,经多道次锻造加工后使钨材料的变形量为65~85%;旋锻完成后,将钨棒进行退火处理以消除残余应力,退火温度为1100℃。
所述的颗粒弥散物主要为氧化物颗粒。
需通过氢气气氛烧结的方法制备烧结坯。
烧结坯棒材的长度需大于500mm,以便于后期的旋锻处理。
先将钨棒加热至1400~1600℃后再进行多道次旋锻。
旋锻过程中钨棒温度低于1300℃时需再次加热钨棒后进行旋锻。
旋锻完成后钨棒的变形量为65~85%。
钨棒旋锻结束后需在1100℃条件下退火1h以去除内应力。
一种具有室温韧性的块体钨材料的制备方法,其特征在于通过氢气烧结制备出具有一定长度(>500mm)的颗粒弥散强化钨合金棒;将烧结坯在氢气气氛下整体加热至1400~1600℃,并通过旋锻方法进行热塑性加工,经多道次锻造加工后使钨材料的变形量达到65~85%;旋锻完成后,将钨棒进行退火处理以消除残余应力,退火温度为1100℃。
颗粒弥散强化钨合金,所述的颗粒为氧化物颗粒或碳化物颗粒,钨块体材料中所添加的弥散颗粒含量质量比应小于10%。
下面给出一个具体的例子。
实验例1:Y2O3弥散强化钨块体材料的制备
步骤1,通过喷雾制粉的方法制备出Y2O3质量比为1%的W-Y2O3混合粉末,并在氢气烧结炉中进行烧结,烧结温度2100℃,时间3h;烧结坯的致密度为96%;烧结坯尺寸为直径25mm,长度500mm。
步骤2,将烧结坯放入氢气炉中加热,加热温度1600℃,时间40min;然后将加热过的钨烧结坯放入旋锻设备上进行多道次的锻打加工,每次变形量约为10%,最终钨烧结坯被锻打成直径12mm的细长钨棒,变形量约为77%。
步骤3,旋锻工艺完成后,将钨棒放入退火炉中进行去应力退火,在1100℃条件下退火1h。
实验例2:TiC弥散强化钨块体材料的制备
步骤1,通过球磨方法制备出TiC质量比为1%的W-TiC混合粉末,并在氢气烧结炉中进行烧结,烧结温度2150℃,时间3h;烧结坯的致密度为95.5%;烧结坯尺寸为直径30mm,长度500mm。
步骤2,将烧结坯放入氢气炉中加热,加热温度1600℃,时间40min;然后将加热过的钨烧结坯放入旋锻设备上进行多道次的锻打加工,每次变形量约为10%,最终钨烧结坯被锻打成直径14mm的细长钨棒,变形量约为78%。
步骤3,旋锻工艺完成后,将钨棒放入退火炉中进行去应力退火,在1100℃条件下退火1h。
实验例3:Y2O3弥散强化钨块体材料的制备
步骤1,通过球磨方法制备出Y2O3质量比为0.7%的W-Y2O3混合粉末,并在氢气烧结炉中进行烧结,烧结温度2150℃,时间3h;烧结坯的致密度为95%;烧结坯尺寸为直径40mm,长度500mm。
步骤2,将烧结坯放入氢气炉中加热,加热温度1550℃,时间40min;然后将加热过的钨烧结坯放入旋锻设备上进行多道次的锻打加工,每次变形量约为8%,最终钨烧结坯被锻打成直径16mm的细长钨棒,变形量约为84%。
步骤3,旋锻工艺完成后,将钨棒放入退火炉中进行去应力退火,在1100℃条件下退火1h。
以上仅为本发明较佳实施例,不能以此限定本发明实施的范围,即依本发明申请专利范围及说明书内容所作的等效变化与修饰,皆应仍属本发明专利涵盖的范围。
Claims (9)
1.一种具有室温韧性块体钨材料的制备方法,其特征在于,包括:
步骤1:制备粉末及烧结
制备钨材料粉末,并将粉末烧结到指定尺寸,形成颗粒弥散强化钨合金棒;
步骤2:加热
将烧结后产物加热并锻打加工;
步骤3:退火
对锻打完成的产品进行退火。
2.如权利要求1所述的一种具有室温韧性块体钨材料的制备方法,其特征在于:所述的制备粉末是指通过球磨方法制备粉末。
3.如权利要求2所述的一种具有室温韧性块体钨材料的制备方法,其特征在于:所述的制备粉末是指制备出Y2O3质量比为0.7%的W-Y2O3混合粉末。
4.如权利要求3所述的一种具有室温韧性块体钨材料的制备方法,其特征在于:所述的烧结是指在氢气烧结炉中进行烧结。
5.如权利要求4所述的一种具有室温韧性块体钨材料的制备方法,其特征在于:所述的烧结是指烧结温度2150℃,时间3h。
6.如权利要求5所述的一种具有室温韧性块体钨材料的制备方法,其特征在于:所述的烧结到指定尺寸是指烧结坯的致密度为95%;烧结坯尺寸为直径40mm,长度大于500mm。
7.如权利要求6所述的一种具有室温韧性块体钨材料的制备方法,其特征在于:所述的加热锻打是指将烧结坯放入氢气炉中加热,加热温度1400~1600℃;然后将加热过的钨烧结坯放入旋锻设备上进行反复的锻打加工,每次变形量约为8%,最终钨烧结坯被锻打成直径16mm的细长钨棒,变形量约为65~85%。
8.如权利要求7所述的一种具有室温韧性块体钨材料的制备方法,其特征在于:所述的退火是指将钨棒放入退火炉中进行去应力退火,在1100℃条件下退火1h。
9.如权利要求8所述的一种具有室温韧性块体钨材料的制备方法,其特征在于:所述的颗粒弥散物为氧化物颗粒。
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