CN105648407B - 一种高致密度钼铌合金靶材及其制备工艺 - Google Patents
一种高致密度钼铌合金靶材及其制备工艺 Download PDFInfo
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- CN105648407B CN105648407B CN201610054493.6A CN201610054493A CN105648407B CN 105648407 B CN105648407 B CN 105648407B CN 201610054493 A CN201610054493 A CN 201610054493A CN 105648407 B CN105648407 B CN 105648407B
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- molybdenum
- niobium
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- -1 molybdenum niobium Chemical compound 0.000 title claims abstract description 55
- 229910001257 Nb alloy Inorganic materials 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 109
- ZOKXTWBITQBERF-UHFFFAOYSA-N molybdenum Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 61
- 239000011733 molybdenum Substances 0.000 claims abstract description 61
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium Chemical compound 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[Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000010955 niobium Substances 0.000 claims abstract description 56
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 56
- KLGZELKXQMTEMM-UHFFFAOYSA-N hydride Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [H-] KLGZELKXQMTEMM-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims abstract description 8
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[Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
本发明公开了一种高致密度钼铌合金靶材及其制备工艺，首先按重量百分比计量称取以下组分：铌粉5%~15%，氢化锆0.1%~0.8%，余量为钼粉，研磨、混匀后采用冷等静压压制成型，再进行真空烧结，或者在氢气气氛中预烧结后再进行真空烧结，最后机加工，即得。本发明利用氢化锆的活化作用，采用普通的粉末冶金工艺直接制备高致密度的钼铌合金溅射靶材，工艺简单，成本低；同时避免了气孔造成的微粒飞溅，保证了镀膜质量；克服了熔炼铸造工艺组织粗大、成分不均，热压、热等静压工艺的渗碳、成本高，锻造或轧制加工流程长、成品率低的缺点。
Description
一种高致密度钼铌合金靶材及其制备工艺
技术领域
[0001] 本发明属于稀有金属技术领域，具体涉及一种添加氢化锆的高致密度钼铌合金靶 材及其制备工艺。
背景技术
[0002] 溅射是利用离子源产生的离子，在真空中加速聚集成高速离子流轰击固体表面， 使固体表面的原子离开靶材并沉积在基材表面，从而形成纳米(或微米)薄膜，被轰击的固 体称为溅射靶材。溅射镀膜是集成电路、平板显示器(包括液晶显示器和触摸屏等）、薄膜太 阳能电池和发光二极管(LED)等领域制备功能薄膜的基本手段，溅射靶材就成为了这些领 域不可缺少的基础材料。
[0003] 随着对电子产品综合性能和使用环境要求的不断提高，对溅射靶材的性能也提出 了越来越高的要求。虽然钼已成为较为理想的平面显示器、薄膜太阳能电池的电极和配线 材料以及半导体的阻挡层材料，但在应用中，发现钼在耐腐蚀性(变色）和密着性(膜的剥 离)方面仍存在问题。研究和实践表明，在钼溅射靶材中加入铌等合金元素，可使溅射后溅 射薄膜的比阻抗、应力、耐腐蚀性等各种性能达到均衡，愈来愈受到青睐。目前，钼铌合金溅 射靶材已在触摸屏(手机、公共领域显示器等）、液晶显示器等功能薄膜制备中开始应用，显 示了显著的优点和广阔的应用前景。
[0004] 通常，钼铌合金溅射靶材所采用的制备工艺包括：
[0005] 1)熔炼铸造工艺
[0006] 将一定配比的钼、铌原料熔炼，再将合金熔液浇注于模具中，得到铸锭，再经热处 理、锻造、挤压和乳制等制成靶材。此工艺存在的问题是:铸锭难免存在铸造缺陷，如缩孔、 缩松、夹杂、偏析等，且铸锭晶粒粗大，造成镀膜效率降低和薄膜质量下降，如果进一步加 工，成品率低、成本高；由于钼、铌皆属高熔点金属，通常需采用真空电弧熔炼或真空电子束 熔炼，设备条件要求高，成本高；很难获得成分均匀的钼铌合金靶材，即使采用二次重熔等 工艺，成分均匀性也很难达到要求，造成膜层成分均匀性降低。
[0007] 2)粉末冶金工艺
[0008] 对于钼铌合金靶材的制备，常用的粉末冶金工艺包括:①将一定量的钼粉和铌粉 混合后，经压制成形、真空烧结得到钼铌合金靶材。由于铌与氧的结合力较强，且在烧结过 程中钼粉中的氧杂质也被铌所吸收，造成来自钼粉和铌粉中的氧杂质挥发困难，阻止烧结 致密化，因此此种工艺得到的靶材相对密度仅有80〜89%，气孔率大，在溅射过程中产生微粒 飞溅，进而显著降低溅射镀膜的质量。②将一定量的钼粉和铌粉混合，经压制成形后进行真 空热压或热等静压获得钼铌合金靶材。此种工艺得到的靶材相对密度可以达到90〜97%，但 由于使用石墨模具而引起渗碳、所用设备复杂、昂贵。③将一定量的钼粉和铌粉混合，经压 制成形后烧结，再经热等静压获得钼铌合金靶材。此种工艺得到的靶材相对密度可达到98% 以上，但流程长、操作复杂、成本高。④采用“工艺①”制得烧结坯后，再经锻造或乳制加工， 得到高密度的靶材。但由于烧结坯密度低等问题，加工成品率低，而且工艺复杂，制备成本 尚。
[0009] 显然，粉末冶金工艺具有容易获得均匀细晶结构、节约原材料、生产效率高等优 点，若能通过技术措施，采用“工艺①”的常规粉末冶金工艺直接制备高致密度的钼铌合金 靶材，具有重要的意义。
发明内容
[0010] 基于现有技术的不足，本发明提供了一种高致密度钼铌合金靶材及其制备工艺， 通过在钼铌合金压制坯中添加适量的氢化锆，以达到采用简单、低成本的制备工艺获得高 致密度钼铌合金靶材的目的。
[0011] 为了实现上述目的，本发明采用的技术方案为：
[0012] —种高致密度钼铌合金靶材，由按重量百分比计量的以下组分组成:铌粉5%〜15%， 氢化锆0.1%〜0.8%，余量为钼粉。
[0013] 上述高致密度钼铌合金靶材的制备工艺，包括以下步骤：
[0014] (1)将按重量百分比称量的各组分研磨、混匀，得到混合粉末；
[0015] (2)将步骤（1)所得的混合粉末压制成型，得到压制坯;其中，压制压力为150〜300 兆帕；
[0016] (3)将步骤(2)所得的压制坯直接进行真空烧结，或者在氢气气氛中预烧结后再进 行真空烧结，得到烧结坯;其中，真空烧结的保温温度为1900〜2150Γ，保温时间为2〜8小时， 保温结束后随炉冷却至120°C以下，再出炉冷却至室温；
[0017] (4)将步骤(3)所得的烧结坯进行机加工，即得。
[0018] 优选地，步骤(3)中所述预烧结的升温速度不大于HTC/分钟。
[0019] 优选地，步骤(3)中所述真空烧结的升温速度不大于nrc/分钟，升温过程中真空 度保持在IX HT2Pa以下。
[0020] 其中，钼粉、银粉及氢化错(ZrH2)均为普通市售产品，钼粉的费氏粒度为2.4〜4.5μ m，钼粉的碳含量为100 ppm以下，铌粉的费氏粒度为5〜20微米(μπι)，铌粉的碳含量为6000 ppm以下，钼粉及铌粉的氧含量均为2500ppm以下;ZrH2的纯度为工业纯以上，费氏粒度1〜10 μηι〇
[0021] 本发明的有益效果为：利用ZrH2的活化作用，采用粉末冶金工艺直接制备高致密 度的钼铌合金溅射靶材，工艺简单，成本低；同时，避免了气孔造成的微粒飞溅，保证了镀膜 质量;克服了熔炼铸造工艺组织粗大、成分不均，热压、热等静压工艺的渗碳、成本高，锻造 或乳制加工流程长、成品率低的缺点。所制得的高致密度钼铌合金靶材可应用于触摸屏薄 膜电极层等功能薄膜制备。
具体实施方式
[0022] 以下通过优选实施例对本发明进一步详细说明，但本发明的保护范围并不局限于 此。
[0023] 实施例1
[0024] —种高致密度钼铌合金靶材，由按重量百分比计量的以下组分组成:铌粉9.97%， 氢化错0.3%，余量为钼粉。
[0025] 其中，钼粉、铌粉及氢化锆(ZrH2)均为普通市售产品，钼粉选用登封市钨钼材料厂 牌号为FMo-I的产品，钼粉的费氏粒度分别为2.6μηι，钼粉的碳含量为30ppm，钼粉的氧含量 为SOOppm;银粉选用株洲硬质合金集团有限公司牌号FNb-I的产品，银粉的费氏粒度分别为 8mi，铌粉的碳含量为130ppm，铌粉的氧含量为1500ppm; ZrH2选自上海水田材料科技有限公 司的产品，化学纯，费氏粒度2μπι。
[0026] 上述高致密度钼铌合金靶材的制备工艺，包括以下步骤：
[0027] (1)将按重量百分比的各组分加入球磨机中，研磨48小时、混合均匀，得到混合粉 末；
[0028] (2)将步骤(1)所得的混合粉末采用冷等静压压制成型，得到压制坯;其中，压制压 力为150兆帕；
[0029] (3)将步骤(2)所得的压制坯在真空炉中烧结，控制升温速度不大于6°C/min，并使 升温过程中真空度不大于8X l(T3Pa，升温至1950Γ进行保温，保温阶段真空度为I X HT3Pa 以下，保温4小时后随炉冷却，冷却过程中真空度为IX HT3Pa以下，冷却至80°C出炉，得到烧 结坯；
[0030] ⑷将步骤⑶所得的烧结坯进行机加工，即得。
[0031] 作为比较，采用与实施例1中上述相同的钼粉、铌粉及制备工艺来制备钼铌合金靶 材;其中，钼粉与铌粉的质量比为9:1，不添加ZrH2。
[0032] 采用排水法分别测定上述钼铌合金靶材的密度，测试并计算得到钼铌合金靶材的 密度及相对密度(实际密度/理论密度），如表1所示。
[0033] 实施例2
[0034] —种高致密度钼铌合金靶材，由按重量百分比计量的以下组分组成:铌粉9.96%， 氢化错0.4%，余量为钼粉。
[0035] 其中，钼粉、铌粉及氢化锆(ZrH2)均为普通市售产品，钼粉选用洛阳永卓钨钼材料 有限公司牌号为FMo-I的产品，钼粉的费氏粒度分别为3.2μπι，钼粉的碳含量为50ppm，钼粉 的氧含量为1200ppm;铌粉选自东方钽业股份有限公司牌号为FNb-I的产品，铌粉的费氏粒 度分别为l〇ym，铌粉的碳含量为500ppm，铌粉的氧含量为2000ppm;ZrH2选自锦州昊天钛粉 加工有限公司的产品，化学纯，费氏粒度3. Ομπι。
[0036] 上述高致密度钼铌合金靶材的制备工艺，包括以下步骤：
[0037] (1)将按重量百分比的各组分加入球磨机中，研磨40小时、混合均匀，得到混合粉 末；
[0038] (2)将步骤(1)所得的混合粉末采用冷等静压压制成型，得到压制坯;其中，压制压 力为180兆帕；
[0039] (3)将步骤(2)所得的压制坯在真空炉中烧结，控制升温速度不大于6°C/min，并使 升温过程中真空度不大于8X l(T3Pa，升温至2000°C进行保温，保温阶段真空度为I X HT3Pa 以下，保温5小时后随炉冷却，冷却过程中真空度为IX HT3Pa以下，冷却至80°C出炉，得到烧 结坯；
[0040] (4)将步骤(3)所得的烧结坯进行机加工，即得。
[0041] 作为比较，采用与实施例2中上述相同的钼粉、铌粉及制备工艺来制备钼铌合金靶 材;其中，钼粉与铌粉的质量比为9:1，不添加ZrH2。
[0042] 采用排水法分别测定上述钼铌合金靶材的密度，测试并计算得到钼铌合金靶材的 密度及相对密度，如表1所示。
[0043] 实施例3
[0044] 一种高致密度钼铌合金靶材，由按重量百分比计量的以下组分组成:铌粉5.982%， 氢化错0.3%，余量为钼粉。
[0045] 其中，钼粉、铌粉及氢化锆(ZrH2)均为普通市售产品，钼粉选用登封市钨钼材料厂 牌号为FMo-I的产品，钼粉的费氏粒度分别为2.6μηι，钼粉的碳含量为30ppm，钼粉的氧含量 为SOOppm;银粉选用株洲硬质合金集团有限公司牌号为FNb-I，银粉的费氏粒度分别为8μπι， 铌粉的碳含量为130ppm，铌粉的氧含量为1500ppm; ZrH2选用上海水田材料科技有限公司的 产品，化学纯，费氏粒度2μπι。
[0046] 上述高致密度钼铌合金靶材的制备工艺，包括以下步骤：
[0047] (1)将按重量百分比的各组分加入V型混料机中，混合46小时，得到混合粉末；
[0048] (2)将步骤(1)所得的混合粉末采用冷等静压压制成型，得到压制坯;其中，压制压 力为150兆帕；
[0049] (3)将步骤(2)所得的压制坯在真空炉中烧结，控制升温速度不大于4°C/min，并使 升温过程中真空度不大于5 X l(T3Pa，升温至1900°C进行保温，保温阶段真空度为I X HT3Pa 以下，保温5小时后随炉冷却，冷却过程中真空度为IX HT3Pa以下，冷却至80°C出炉，得到烧 结坯；
[0050] ⑷将步骤⑶所得的烧结坯进行机加工，即得。
[0051] 作为比较，采用与实施例3中上述相同的钼粉、铌粉及制备工艺来制备钼铌合金靶 材;其中，钼粉与铌粉的质量比为47:3，不添加ZrH2。
[0052] 采用排水法分别测定上述钼铌合金靶材的密度，测试并计算得到钼铌合金靶材的 密度及相对密度，如表1所示。
[0053] 实施例4
[0054] —种高致密度钼铌合金靶材，由按重量百分比计量的以下组分组成:铌粉5.964%， 氢化错0.6%，余量为钼粉。
[0055] 其中，钼粉、铌粉及氢化锆(ZrH2)均为普通市售产品，钼粉选用登封市钨钼材料厂 牌号为FM〇-2的产品，钼粉的费氏粒度分别为4.2μηι，钼粉的碳含量为36ppm，钼粉的氧含量 为ISOOppm;铌粉选用株洲硬质合金集团有限公司牌号为FNb-I的产品，铌粉的费氏粒度分 别为15μπι，铌粉的碳含量为220ppm，铌粉的氧含量为530ppm;ZrH2选用锦州昊天钛粉加工有 限公司的产品，ZrH2为工业纯，费氏粒度5μπι。
[0056] 上述高致密度钼铌合金靶材的制备工艺，包括以下步骤：
[0057] (1)将按重量百分比的各组分加入V型混料机中，混合12小时，得到混合粉末；
[0058] (2)将步骤(1)所得的混合粉末采用冷等静压压制成型，得到压制坯;其中，压制压 力为200兆帕；
[0059] (3)将步骤(2)所得的压制坯在真空炉中烧结，控制升温速度不大于4°C/min，并使 升温过程中真空度不大于5 X l(T3Pa，升温至2100°C进行保温，保温阶段真空度为I X HT3Pa 以下，保温6小时后随炉冷却，冷却过程中真空度为IX HT3Pa以下，冷却至80°C出炉，得到烧 结还；
[0060] ⑷将步骤⑶所得的烧结坯进行机加工，即得。
[0061] 作为比较，采用与实施例3中上述相同的钼粉、铌粉及制备工艺来制备钼铌合金靶 材;其中，钼粉与铌粉的质量比为47:3，不添加ZrH2。
[0062] 采用排水法分别测定上述钼铌合金靶材的密度，测试并计算得到钼铌合金靶材的 密度及相对密度，如表1所示。
[0063] 实施例5
[0064] —种高致密度钼铌合金靶材，由按重量百分比计量的以下组分组成:铌粉9.96%， 氢化错0.4%，余量为钼粉。
[0065] 其中，钼粉、铌粉及氢化锆(ZrH2)均为普通市售产品，钼粉选用洛阳永卓钨钼材料 有限公司牌号为FMo-I的产品，钼粉的费氏粒度分别为3.2μπι，钼粉的碳含量为50ppm，钼粉 的氧含量为1200ppm;铌粉选用东方钽业股份有限公司牌号为FNb-I的产品，铌粉的费氏粒 度分别为l〇ym，铌粉的碳含量为500ppm，铌粉的氧含量为2000ppm;ZrH2选用锦州昊天钛粉 加工有限公司的产品，化学纯，费氏粒度3. Ομπι。
[0066] 上述高致密度钼铌合金靶材的制备工艺，包括以下步骤：
[0067] (1)将按重量百分比的各组分加入球磨机中，研磨40小时、混合均匀，得到混合粉 末；
[0068] (2)将步骤(1)所得的混合粉末采用冷等静压压制成型，得到压制坯;其中，压制压 力为180兆帕；
[0069] (3)将步骤(2)所得的压制坯在中频炉中氢气气氛下预烧结，控制升温速度不大于 3°C/min，在1000°C保温2小时，冷却至100 °C出炉。然后在真空炉中烧结，控制升温速度不大 于5°C/min，并使升温过程中真空度不大于6/10^^，升温至2000°(：进行保温，保温阶段真 空度为IX KT3Pa以下，保温5小时后随炉冷却，冷却过程中真空度为IX HT3Pa以下，冷却至 80°C出炉，得到烧结坯；
[0070] ⑷将步骤⑶所得的烧结坯进行机加工，即得。
[0071] 作为比较，采用与实施例2中上述相同的钼粉、铌粉及制备工艺来制备钼铌合金靶 材;其中，钼粉与铌粉的质量比为9:1，不添加ZrH2。
[0072] 采用排水法分别测定上述钼铌合金靶材的密度，测试并计算得到钼铌合金靶材的 密度及相对密度，如表1所示。
[0073] 表1各实施例中钼铌合金靶材的密度和相对密度
[0074]
[0075] 从上表可以看出，采用本发明所述的制备工艺，添加有ZrH2钼铌合金靶材的相对 密度较未添加ZrH2钼铌合金靶材显著提高，本发明制得的钼铌合金靶材相对密度可以提高 至98%以上，在工艺简单、低成本制备的同时，显著降低了气孔率，从而制得高致密度钼铌合 金靶材，有利于获得高质量的溅射膜层。
Claims (3)
1. 一种高致密度钼铌合金靶材，其特征在于，由按重量百分比计量的以下组分组成:铌 粉5%〜15%，氢化锆0.1%〜0.8%，余量为钼粉； 所述高致密度钼铌合金靶材的制备工艺，包括以下步骤： (1) 将按重量百分比称量的各组分研磨、混匀，得到混合粉末； (2) 将步骤(1)所得的混合粉末压制成型，得到压制坯;其中，压制压力为150〜300兆帕； (3) 将步骤(2)所得的压制坯直接进行真空烧结，或者在氢气气氛中预烧结后再进行真 空烧结，得到烧结坯;其中，真空烧结的保温温度为1900〜2150Γ，保温时间为2〜8小时，保温 结束后随炉冷却至120°C以下，再出炉冷却至室温； (4) 将步骤(3)所得的烧结坯进行机加工，即得。
2. 根据权利要求1所述高致密度钼铌合金靶材，其特征在于：步骤(3)中所述预烧结的 升温速度不大于l〇°C/分钟。
3. 根据权利要求1所述高致密度钼铌合金靶材，其特征在于：步骤(3)中所述真空烧结 的升温速度不大于l〇°C/分钟，升温过程中真空度保持在IX HT2Pa以下。
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