JPS616197A - Single crystal of tungsten and its production - Google Patents
Single crystal of tungsten and its productionInfo
- Publication number
- JPS616197A JPS616197A JP59126326A JP12632684A JPS616197A JP S616197 A JPS616197 A JP S616197A JP 59126326 A JP59126326 A JP 59126326A JP 12632684 A JP12632684 A JP 12632684A JP S616197 A JPS616197 A JP S616197A
- Authority
- JP
- Japan
- Prior art keywords
- tungsten
- single crystal
- grain
- magnesium
- crystal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000013078 crystal Substances 0.000 title claims description 27
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims description 24
- 229910052721 tungsten Inorganic materials 0.000 title claims description 24
- 239000010937 tungsten Substances 0.000 title claims description 24
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 9
- 229910052749 magnesium Inorganic materials 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 9
- 238000000137 annealing Methods 0.000 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 230000004927 fusion Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000003779 heat-resistant material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 150000003657 tungsten Chemical class 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はタングステン単結晶とその製造方法する。[Detailed description of the invention] [Industrial application field] The present invention relates to a tungsten single crystal and a method for manufacturing the same.
耐熱性拐料としては、高温強度に優れた多結晶タングス
テンが知られているが、この多結晶タングステンの欠点
は結晶粒界が脆いことである。さらに、多結晶タングス
テンは室温以下での成型加工性が極めて悪く、また高温
での使用時において、結晶粒が粗大化して、再結晶脆性
を引き起すため、耐熱材料としての特性を十分に発揮す
ることができない。従って多結晶タングステンの用途は
限られてしまう。Polycrystalline tungsten, which has excellent high-temperature strength, is known as a heat-resistant material, but the drawback of this polycrystalline tungsten is that its grain boundaries are brittle. Furthermore, polycrystalline tungsten has extremely poor moldability at temperatures below room temperature, and when used at high temperatures, its crystal grains become coarse and recrystallization embrittlement occurs, making it unable to fully demonstrate its properties as a heat-resistant material. I can't. Therefore, the uses of polycrystalline tungsten are limited.
従って結晶粒界がないかあるいは極めて少ない、しかも
任意形状に成型加工後においてもタングステン単結晶を
提供することができれは。Therefore, it would be possible to provide a tungsten single crystal with no or very few grain boundaries, even after being formed into an arbitrary shape.
大出力レーサ反射鏡、 ＩＣ基板材料、原子核融合炉
の炉利、原子炉の発熱体、ルツボ及び電子部品等に用い
た場合、結晶粒界脆性によって機械的に破損することな
く、消耗するまで使用が可能となり、利用分野が著しく
拡大される。この種のタングステン材料として巨大粒を
含むタングステン拐料あるいは単結晶タングステン材料
が考えられる。When used in high-power laser reflectors, IC substrate materials, nuclear fusion reactor reactors, nuclear reactor heating elements, crucibles, electronic components, etc., it can be used until it wears out without mechanical damage due to grain boundary embrittlement. This makes it possible to significantly expand the field of use. As this type of tungsten material, a tungsten powder containing giant grains or a single crystal tungsten material can be considered.
ところで、従来からタングステン単結晶は帯域溶融法等
によって作製可能であるけれども形状あるいは製造規模
が制約され、さらには製造技術に熟練を要するという問
題点がある。Incidentally, although tungsten single crystals have conventionally been able to be produced by a zone melting method or the like, there have been problems in that the shape or production scale is limited, and furthermore, the production technique requires skill.
本発明の目的は結晶粒界脆性による破土がか生じること
なく任意の形状を有するタンゲス−１ノ単結晶を提供す
ることにある。An object of the present invention is to provide a single crystal of TANGES-1 having an arbitrary shape without causing fracture due to grain boundary brittleness.
本発明の他の目的は熟練を要せず、従って極めて容易に
上記のタングステン単結晶を製造できる製造方法を提供
することである。Another object of the present invention is to provide a manufacturing method that does not require any skill and therefore can produce the above-mentioned tungsten single crystal very easily.
本発明によるタングステン単結晶はカルンウム及びマグ
ネシウムヂ少なくとも一方を総量で０．００７乃至００
９０原子・ζ−，セント含有している。The tungsten single crystal according to the present invention contains at least one of carunium and magnesium in a total amount of 0.007 to 0.00.
It contains 90 atoms ζ-, cents.
またこのタングステン単結晶はカル／ラム及びマグネシ
ウムの少なくとも一方を総量で０００７乃至００９０原
子パーセント含むタングステン多結晶体を予め定められ
た形状に成型し、この成型体を予め定められた雰囲気に
おいて焼鈍することによって得られる。Further, this tungsten single crystal is obtained by molding a tungsten polycrystal containing at least one of Cal/Ram and magnesium in a total amount of 0007 to 0090 atomic percent into a predetermined shape, and annealing this molded body in a predetermined atmosphere. obtained by.
以下本発明（（ついて実施例に基づいて説明する。 The present invention will be described below based on examples.
タングステン酸化物の粉末に１戸〕示すように試料番号
１〜６に示す曇カ港種々の割合でカル／ラム及びマグ不
ソウムを湿式法によって添体とした。烙らにこの焼結体
に熱間加工（温度１６００〜１２００℃）及び温間加工
（１０００〜５００℃）を施し、最終の圧延率が７０係
昇上となるようにして１〜２喘（厚さ）Ｘ３０ｍｍ（幅
） Ｘ １５Ｄ＋ａ＋ （長さ）５時間焼鈍を行った。As shown in Sample Nos. 1 to 6, Cal/Rum and Magnolium were added to tungsten oxide powder in various proportions by a wet method. This sintered body was then subjected to hot working (at a temperature of 1,600 to 1,200°C) and warm working (at a temperature of 1,000 to 500°C) to increase the final rolling reduction by 70%, and then roll it by 1 to 2 mm ( Thickness) x 30mm (width) x 15D+a+ (length) Annealing was performed for 5 hours.
表−１
備考 ＊１．細粒とは板状試料の厚さ未満の粒径を言う
（平均粒径）
＊２．巨大粒とは板状試料の厚さの１０〜２０倍の粒径
を持つ結晶粒を言う（平均
粒径）
＊３ 単結晶とは板状試料のすべてが１つの結晶粒で覆
われた状態を言う。Table-1 Notes *1. Fine grain refers to a grain size that is less than the thickness of a plate-shaped sample (average grain size) *2. A giant grain is a crystal grain with a grain size that is 10 to 20 times the thickness of a plate-shaped sample (average grain size) *3 A single crystal is a state in which the entire plate-shaped sample is covered with one crystal grain. say.
上記の表から明らかなように試料番号１の板状試料の結
晶状態は細粒てあり、試料番号２及び６の板状試料の結
晶状態は巨大粒を含む実質的に単結晶を形成している。As is clear from the table above, the crystalline state of the plate-like sample No. 1 is fine-grained, and the crystalline state of the plate-like samples No. 2 and 6 is substantially single crystal containing giant grains. There is.
また試料番号３．４及び５の板状試料の結晶状態は単結
晶である。Further, the crystal state of the plate-like samples of sample numbers 3.4 and 5 is single crystal.
発−考らの実験によれば、カル／ウム、マグネ／ウムの
含有量が糺、量て０００７原子チ未満であると結晶状態
を結晶粒界のない巨大粒あるいは単結晶とすることが難
しく、またカル／ラム。According to our experiments, when the content of Cal/Umium or Magne/Umium is less than 0,007 atoms, it is difficult to make the crystal state into giant grains or single crystals without grain boundaries. , also Cal/Ram.
マグネシウムの含有量が総量で００９０原子係を超える
と、結晶状態はカル／ツノ・、マグネシウムを添加しな
い場合よりも悪くなることがわかっ、ｇ−、（即ちより
細粒状態となってしまう。）。It was found that when the total content of magnesium exceeds 0090 atoms, the crystalline state becomes worse than when no magnesium is added (i.e., the crystalline state becomes finer). .
カルンウム、マグネシウムの含有量が総量で００９０原
子チを超えた場合には正常結晶粒成長に対するピンニン
グ効果が強力となり１粒成長を抑制するためと考えられ
る。This is considered to be because when the total content of carunium and magnesium exceeds 0,090 atoms, the pinning effect on normal crystal grain growth becomes strong and suppresses single grain growth.
なお、上述の実施例では粉末冶金法によって所定量のカ
ルンウム、マグネ／ウムを含有する形
タングステンを成塑、加工を行ったが、溶融法を用いて
もよい。ただし溶融法を用いる場合はマグネシウム及び
カル７ウムの蒸気圧が高いため含有量を調整することも
、その後の加工も容易でない。In the above-described embodiment, tungsten containing a predetermined amount of carunium and magnesium was molded and processed by a powder metallurgy method, but a melting method may also be used. However, when using the melting method, it is difficult to adjust the content and subsequent processing because the vapor pressure of magnesium and calcium is high.
また上述の実施例においてはカルー／ウム、マグネンウ
ム両者を添加し、総量か０００７乃至００９０原子幅の
場合について説明したか１表−２及び表−５に示すよう
にカル／ウム、マグネシウムどちらか一方か０．００７
乃至０．０９０原子俤の範囲でもよいことがわかった。In addition, in the above-mentioned example, the case where both Cal/ium and Magnenium were added and the total amount was 0007 to 0090 atoms wide was explained. or 0.007
It has been found that a range of 0.090 to 0.090 atoms may be sufficient.
なお、この場合の焼鈍温度、焼鈍時間等は前述の表−１
の実施例と同様である。The annealing temperature, annealing time, etc. in this case are shown in Table 1 above.
This is similar to the embodiment.
表−２ 表−６ イガ６考： 表−２１表−６において。Table-2 Table-6 Iga 6 thoughts: In Table-21 Table-6.
巨
＊２濶大粒とは板状試料の厚さの１０〜２０倍の粒径を
持つ結晶粒を言う。Giant*2 large grains refer to crystal grains with a grain size that is 10 to 20 times the thickness of the plate-shaped sample.
＊３ 単結晶とは板状試料のすべてが１つの結晶粒て段
われだ状態を言う。*3 Single crystal refers to a state in which all of the plate-shaped specimens are made up of one crystal grain.
以上説明したように本発明ではカル／ラムまたはマグネ
／ラムの少なくとも一方を総量で０００７乃至００９０
原子パーセント含むタングステン圧粉体を焼結させて、
所定の形状に加工した後、焼鈍させて粒界のない巨大粒
または単結晶のタングステン材料を得ることができる。As explained above, in the present invention, the total amount of at least one of Cal/Rum or Magne/Rum is 0007 to 0090.
By sintering a tungsten compact containing atomic percent,
After processing into a predetermined shape, it can be annealed to obtain a giant grain or single crystal tungsten material without grain boundaries.
従ってカル／ラムまたはマグネ／ラムの少なくとも一方
を総量で０．００７乃至０．０９０ 県子ノ々−セント
含むタングステン単結晶は高温状態においても脆性を引
き起すことなく、大出力レーサー反射鏡、 ＩＣＣ基
板科料原子炉、核融合炉の炉材。Therefore, a tungsten single crystal containing at least one of Cal/Ram or Magne/Ram in a total amount of 0.007 to 0.090 Kenshi Nono-Sent does not cause brittleness even under high temperature conditions, and can be used as a high-power laser reflector or ICC. Substrate materials for nuclear reactors and fusion reactors.
電気炉等の通常炉に用いられる発熱体、ルツボ及び電子
部品なとに利用することができる。It can be used for heating elements, crucibles, electronic parts, etc. used in ordinary furnaces such as electric furnaces.
Claims (1)
くとも一方を総量で０．００７乃至０．０９０原子パー
セント含有するタングステン単結晶。 ２、タングステン多結晶体を予め定められた形状に成型
し、この成型体を焼鈍することを特徴とするタングステ
ン単結晶の製造方法。 ３、特許請求の範囲第２項の記載において、前記タング
ステン多結晶体はカルシウム及びマグネシウムの少なく
とも一方を総量で０．００７乃至０．０９０原子パーセ
ント含有していることを特徴とするタングステン単結晶
の製造方法。[Scope of Claims] 1. A tungsten single crystal containing at least one of calcium and magnesium in a total amount of 0.007 to 0.090 atomic percent in tungsten. 2. A method for producing a tungsten single crystal, which comprises molding a tungsten polycrystal into a predetermined shape and annealing the molded body. 3. The tungsten single crystal according to claim 2, wherein the tungsten polycrystal contains at least one of calcium and magnesium in a total amount of 0.007 to 0.090 atomic percent. Production method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59126326A JPS616197A (en) | 1984-06-21 | 1984-06-21 | Single crystal of tungsten and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59126326A JPS616197A (en) | 1984-06-21 | 1984-06-21 | Single crystal of tungsten and its production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS616197A true JPS616197A (en) | 1986-01-11 |
| JPH0351676B2 JPH0351676B2 (en) | 1991-08-07 |
Family
ID=14932415
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59126326A Granted JPS616197A (en) | 1984-06-21 | 1984-06-21 | Single crystal of tungsten and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS616197A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5916363A (en) * | 1996-07-08 | 1999-06-29 | National Research Institute For Metals | Oriented molybdenum or tungsten single crystal and manufacturing method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS582289A (en) * | 1981-06-30 | 1983-01-07 | Matsushita Electric Ind Co Ltd | Manufacture of single crystal body |
-
1984
- 1984-06-21 JP JP59126326A patent/JPS616197A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS582289A (en) * | 1981-06-30 | 1983-01-07 | Matsushita Electric Ind Co Ltd | Manufacture of single crystal body |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5916363A (en) * | 1996-07-08 | 1999-06-29 | National Research Institute For Metals | Oriented molybdenum or tungsten single crystal and manufacturing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0351676B2 (en) | 1991-08-07 |
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| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |