JP3088480B2 - Manufacturing method of non-evaporable getter - Google Patents
Manufacturing method of non-evaporable getterInfo
- Publication number
- JP3088480B2 JP3088480B2 JP10657191A JP10657191A JP3088480B2 JP 3088480 B2 JP3088480 B2 JP 3088480B2 JP 10657191 A JP10657191 A JP 10657191A JP 10657191 A JP10657191 A JP 10657191A JP 3088480 B2 JP3088480 B2 JP 3088480B2
- Authority
- JP
- Japan
- Prior art keywords
- getter
- evaporable getter
- gas
- adsorption
- evaporable
- 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.)
- Expired - Fee Related
Links
Landscapes
- Particle Accelerators (AREA)
- Thermally Insulated Containers For Foods (AREA)
- Manufacture Of Electron Tubes, Discharge Lamp Vessels, Lead-In Wires, And The Like (AREA)
- Common Detailed Techniques For Electron Tubes Or Discharge Tubes (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、真空容器中のガス吸着
などのために用いられるゲッターを製造する方法に関
し、特に、加速器などのように磁場中に設置されるコン
ダクタンスが小さく、複雑な形状の真空容器に用いられ
るものに適用した場合にとりわけ効果的な非蒸発型ゲッ
ターの製造方法について提案する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a getter used for adsorbing gas in a vacuum vessel, and more particularly to a method for manufacturing a getter having a small conductance and a complicated shape, such as an accelerator, installed in a magnetic field. A method of manufacturing a non-evaporable getter which is particularly effective when applied to a vacuum vessel is proposed.
【０００２】[0002]
【従来の技術】前記ゲッターは、真空管や魔法瓶などの
ような真空容器内を真空にするために、それらの内部に
直接もしくは間接に取付けて使用するものである。この
ようなゲッターには、バリウム系のような真空容器内で
蒸発する「蒸発型」と、Zr系に代表される「非蒸発型」
があり、最近では、取扱いが簡単で吸着能力の大きい非
蒸発型ゲッターと呼ばれているものが優勢であるが、こ
の非蒸発型ゲッターについてもその吸着能力をさらに大
きくするための研究、すなわち合金成分の改良や形状の
改良が行われている。2. Description of the Related Art The above-mentioned getter is used by directly or indirectly attaching it to a vacuum vessel such as a vacuum tube or a thermos in order to evacuate the inside thereof. There are two types of getters: "evaporation type" that evaporates in a vacuum vessel such as barium type and "non-evaporation type" represented by Zr type.
In recent years, non-evaporable getters that are easy to handle and have a large adsorption capacity are dominant, but studies on this non-evaporable getter to further increase its adsorption capacity, namely alloys Improvements in components and shapes have been made.
【０００３】従来、この非蒸発型ゲッターの形状として
は、タブレット状、リング状および板状の構造が知られ
ており、それらを真空容器内に取付ける方法としては、
金属製の保持容器または保持具を介して、タブレット状
またはリング状のゲッターを、真空容器内壁などに取付
ける方法（実公昭60−28号公報）や、板状ゲッターを、
直接に真空容器内壁に取付ける方法（実開平２−109543
号公報）が開示されている。Heretofore, as the shape of the non-evaporable getter, tablet, ring, and plate structures are known, and as a method of mounting them in a vacuum vessel,
A method of attaching a tablet or ring-shaped getter to the inner wall of a vacuum container or the like via a metal holding container or holding tool (Japanese Utility Model Publication No. 60-28), a plate-like getter,
Direct mounting on the inner wall of the vacuum vessel
Gazette).
【０００４】[0004]
【発明が解決しようとする課題】ところが、かかる従来
のゲッターは、ステンレスやコンスタンタンなどの２〜
３種の金属基材にゲッター材を被覆したもので、しか
も、上述したように金属保持具などに保持するか、ある
いは直接取付ける構造であるため、限られた金属で、か
つ単純な形状の材料にしか被覆できなかった。However, such conventional getters are made of stainless steel or constantan.
Since three types of metal base materials are covered with a getter material and, as described above, are held on a metal holder or the like, or are directly attached, the material is limited metal and has a simple shape. Could only be coated.
【０００５】また、ゲッターの吸着性能を改善したもの
として、金属板にゲッター材をロール押圧成型すること
により、板状ゲッターを得る方法が提案されているが、
用途によっては、ゲッターの吸着能力が充分とはいえな
い。[0005] As a method for improving the adsorbing performance of the getter, there has been proposed a method of obtaining a plate-like getter by roll-pressing a getter material on a metal plate.
Depending on the application, the adsorbability of the getter is not sufficient.
【０００６】本発明の目的は、材料や形状の影響を受け
ることなく、かつ吸着速度が速く、吸着量の大きい非蒸
発型ゲッターを得る方法を提供することにある。An object of the present invention is to provide a method for obtaining a non-evaporable getter which is not affected by the material and shape, has a high adsorption speed and a large amount of adsorption.
【０００７】[0007]
【課題を解決するための手段】上述のような従来技術が
抱えている問題点について検討した結果、本発明者ら
は、基材として従来の金属と比べて比較的自由な抵抗値
を選択できるとともに、ガス放出の少ない材料で超高真
空中のヒーター材料を兼ねるような基材に、ゲッター粉
末材料をプラズマ溶射することが有効であることを知見
し、次のような要旨構成の非蒸発型ゲッターの製造方法
に想到した。As a result of studying the problems of the prior art as described above, the present inventors can select a relatively free resistance value as a base material as compared with a conventional metal. At the same time, we found that it was effective to plasma-spray a getter powder material on a base material that also functions as a heater material in an ultra-high vacuum with a material that emits less gas. I arrived at a getter manufacturing method.
【０００８】すなわち、本発明は、基材表面に、ゲッタ
ー粉末材料を、プラズマ溶射被覆することを特徴とする
非蒸発型ゲッターの製造方法であり、特に、上記基材
は、Cu基合金および／または炭素繊維を含む複合炭素材
料であることが好ましく、また、上記ゲッター粉末材料
は、Ti,Zr,Cr,V,Nb,Ta,W,Mo,Th,Ca,Al,Ni,MnおよびFeの
うちから選ばれる一種以上の金属または合金からなるこ
とが好ましい。[0008] That is, the present invention is a method for producing a non-evaporable getter, characterized in that a getter powder material is plasma-sprayed on the surface of a substrate. Or a composite carbon material containing carbon fibers, and the getter powder material is Ti, Zr, Cr, V, Nb, Ta, W, Mo, Th, Ca, Al, Ni, Mn and Fe. It is preferable that it is made of one or more metals or alloys selected from among them.
【０００９】[0009]
【作用】本発明の非蒸発型ゲッターの製造方法は、例え
ば、図１に示すような高周波プラズマなどの減圧プラズ
マ発生装置１内に、ゲッター粉末材料２を、Ｈ2 やArな
どのキャリアガス３とともに導入し、ArやHeなどの不活
性ガス雰囲気としたブース４内に載置した基板５上に、
前記ゲッター粉末材料２を溶射することからなる。According to the method of manufacturing a non-evaporable getter of the present invention, for example, a getter powder material 2 is charged into a carrier gas 3 such as H 2 or Ar in a reduced-pressure plasma generator 1 such as a high-frequency plasma as shown in FIG. With the substrate 5 placed in the booth 4 in an inert gas atmosphere such as Ar or He,
The method comprises spraying the getter powder material 2.
【００１０】すなわち、本発明は、プラズマ溶射により
ゲッター粉末材料を基板上に被覆することであり、これ
により、真空容器中のガスを吸着するゲッターの表面積
が極めて大きくなる。その結果、ガスの速やかな吸着と
大きい吸着量が達成される。また、基材が自由に選べ真
空容器内が複雑な形状であってもその形状に合わせて所
定の形状とすることができるので、あらゆる真空容器に
適用できる。That is, the present invention is to coat a getter powder material on a substrate by plasma spraying, whereby the surface area of the getter that adsorbs gas in a vacuum vessel becomes extremely large. As a result, rapid adsorption of gas and a large adsorption amount are achieved. Further, the substrate can be freely selected, and even if the inside of the vacuum container has a complicated shape, it can be formed into a predetermined shape according to the shape, so that the present invention can be applied to any vacuum container.
【００１１】なお、ガス放出が少なく、超高真空中のヒ
ーターを兼ねることのできる材料としては、コンスタン
タンのようなCu−Ni系合金や C/Cコンポジットと称され
る炭素繊維と炭素の複合材料が好ましい。Examples of materials that emit little gas and can also serve as a heater in an ultra-high vacuum include Cu—Ni alloys such as constantan and carbon / carbon composite materials called C / C composites. Is preferred.
【００１２】この C/Cコンポジットは、超高真空中にお
ける加熱ヒーター材料として知られており、本発明の一
用途である加速器のような10-10Torr 以下の超高真空領
域で使われる場合においても充分使用できることを、ガ
ス放出率、放出ガスのマススペクトル等を検討した結
果、確認できた。その結果、 C/Cコンポジットは、加速
器の磁場中に配置されるゲッター材料のみならず、ベー
ク用ヒーター材料としても共用することができるので、
真空チャンバー内の有効アパーチャーの減少防止にも効
果的であることが判った。This C / C composite is known as a heater material in an ultra-high vacuum, and is used in an ultra-high vacuum region of 10 -10 Torr or less such as an accelerator which is one application of the present invention. As a result of examining the gas release rate, the mass spectrum of the released gas, and the like, it was confirmed that the compound could be used sufficiently. As a result, the C / C composite can be used not only as a getter material arranged in the magnetic field of the accelerator but also as a baking heater material,
It was found that it was also effective in preventing a decrease in the effective aperture in the vacuum chamber.
【００１３】[0013]
【実施例】図１に示すような高周波アークプラズマ（ア
ークガス (Ｈ2)70psi,キャリアガス(Ar)35psi ）内に、
Zr-V-Fe-Ni-Mn-Al合金粉末（エルジェニクス社HS−402
S）を導入し、表１に示すそれぞれの基板上に、前記合
金粉末を溶射した。得られた非蒸発型ゲッターの溶射後
重量および膜厚を測定した結果を表１に示す。DESCRIPTION OF THE PREFERRED EMBODIMENTS In a high-frequency arc plasma (arc gas (H 2 ) 70 psi, carrier gas (Ar) 35 psi) as shown in FIG.
Zr-V-Fe-Ni-Mn-Al alloy powder (Elgenix HS-402
S) was introduced, and the alloy powder was sprayed on each of the substrates shown in Table 1. Table 1 shows the measurement results of the weight and the film thickness of the obtained non-evaporable getter after thermal spraying.
【００１４】[0014]
【表１】 [Table 1]
【００１５】次に、得られた非蒸発型ゲッターを活性化
し、単位重量当りの水素および炭酸ガス吸着量を測定し
た。その結果を図２および図３に示す。図２および図３
から、特に、 C/Cコンポジットにゲッター粉末材料を溶
射したものは、測定開始後１時間以内の初期吸着速度が
非常に速いことがわかる。例えば、吸着開始後10分まで
を、通常のロール成型した非蒸発型ゲッターと比較する
と、水素ガスの吸着では、２倍以上、一酸化炭素ガスで
は、３倍以上吸着速度が速いことが確認できた。また、
ガス吸着量では、ロール成型品の約1.5倍の吸着量であ
った。これは、プラズマ溶射によりゲッター比表面積お
よび気孔率が大きくなっているためと考えられる。一
方、コンスタンタンに、ゲッター粉末材料を溶射したも
のは、 C/Cコンポジットほど初期吸着速度は速くない
が、ロール成型品より、ガス吸着が速く、ガス吸着量が
大きいことが確認できた。Next, the obtained non-evaporable getter was activated, and the amounts of hydrogen and carbon dioxide adsorbed per unit weight were measured. The results are shown in FIGS. 2 and 3
From the results, it can be seen that, in particular, when the getter powder material is sprayed on the C / C composite, the initial adsorption speed within one hour after the start of the measurement is extremely high. For example, up to 10 minutes after the start of adsorption, it can be confirmed that the adsorption rate is twice or more in the case of hydrogen gas adsorption and three times or more in the case of carbon monoxide gas when compared with a normal roll-formed non-evaporable getter. Was. Also,
The gas adsorption amount was about 1.5 times that of the rolled product. It is considered that this is because the getter specific surface area and the porosity are increased by the plasma spraying. On the other hand, when the getter powder material was sprayed on constantan, the initial adsorption speed was not as fast as that of the C / C composite, but it was confirmed that the gas adsorption was faster and the gas adsorption amount was larger than that of the roll-formed product.
【００１６】以上説明したように、本発明によれば、材
料や形状の影響を受けることなく、かつ吸着速度が非常
に速く、吸着量も大きい非蒸発型ゲッターを安定して製
造することができる。このようにして製造した非蒸発型
ゲッターは、加速器などのように磁場の影響を受けやす
く、複雑な形状の真空チャンバー中での利用に特に有効
である。もちろん、吸着速度が速いことと、吸着量が大
きいことから、通常のゲッターの代用としても有利なゲ
ッターである。As described above, according to the present invention, a non-evaporable getter having a very high adsorption speed and a large adsorption amount can be stably manufactured without being affected by the material and the shape. . The non-evaporable getter thus manufactured is easily affected by a magnetic field, such as an accelerator, and is particularly effective for use in a vacuum chamber having a complicated shape. Of course, since the adsorption speed is high and the adsorption amount is large, the getter is also advantageous as a substitute for a normal getter.
【００１７】なお、本発明によれば、プラズマ溶射によ
って充分なゲッター効果を得ることができるので、種々
の材料あるいは複雑な形状のものに対しても、ゲッター
材を成型することができ、応用領域が拡がることが期待
される。According to the present invention, since a sufficient getter effect can be obtained by plasma spraying, the getter material can be molded even for various materials or those having complicated shapes. Is expected to spread.
【図１】本発明にかかる製造方法の一実施例を示す説明
図である。FIG. 1 is an explanatory view showing one embodiment of a manufacturing method according to the present invention.
【図２】本発明によって得られた非蒸発型ゲッターの水
素ガス吸着特性を示す図である。FIG. 2 is a view showing hydrogen gas adsorption characteristics of a non-evaporable getter obtained by the present invention.
【図３】本発明によって得られた非蒸発型ゲッターの一
酸化炭素ガス吸着特性を示す図である。FIG. 3 is a graph showing carbon monoxide gas adsorption characteristics of a non-evaporable getter obtained by the present invention.
１ プラズマ発生装置 ２ ゲッター粉末材料 ３ キャリアガス ４ ブース ５ 基板 DESCRIPTION OF SYMBOLS 1 Plasma generator 2 Getter powder material 3 Carrier gas 4 Booth 5 Substrate
───────────────────────────────────────────────────── フロントページの続き (72)発明者 青木 史朗 千葉県浦安市弁天４−12−９ (72)発明者 角掛 繁 山形県西置賜郡小国町大字小国町字滝ノ 二重２の232番地 日本重化学工業株式 会社 小国開発センター内 (56)参考文献 特開 平２−290941（ＪＰ，Ａ) 特開 平４−313317（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) H01J 9/39 H01J 7/18 H05H 7/00 A47J 41/02 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Shiro Aoki 4-12-9 Benten, Urayasu-shi, Chiba Prefecture (72) Inventor Shigeru Kadake, Oguni-machi, Oguni-machi, Nishiokitama-gun, Yamagata Prefecture (56) References JP-A-2-29041 (JP, A) JP-A-4-313317 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB Name) H01J 9/39 H01J 7/18 H05H 7/00 A47J 41/02
Claims (3)
下でプラズマ溶射被覆することを特徴とする非蒸発型ゲ
ッターの製造方法。1. A method for producing a non-evaporable getter, wherein a getter powder material is coated by plasma spray coating on a substrate surface under vacuum.
素繊維を含む複合炭素材料である請求項１に記載の非蒸
発型ゲッターの製造方法。2. The method for producing a non-evaporable getter according to claim 1, wherein the base material is a composite carbon material containing a Cu-based alloy and / or a carbon fiber.
b,Ta,W,Mo,Th,Ca,Al,Ni,MnおよびFeのうちから選ばれる
一種以上の金属または合金からなる請求項１に記載の非
蒸発型ゲッターの製造方法。3. The getter powder material is Ti, Zr, Cr, V, N
2. The method for producing a non-evaporable getter according to claim 1, comprising at least one metal or alloy selected from b, Ta, W, Mo, Th, Ca, Al, Ni, Mn and Fe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10657191A JP3088480B2 (en) | 1991-04-12 | 1991-04-12 | Manufacturing method of non-evaporable getter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10657191A JP3088480B2 (en) | 1991-04-12 | 1991-04-12 | Manufacturing method of non-evaporable getter |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04315730A JPH04315730A (en) | 1992-11-06 |
| JP3088480B2 true JP3088480B2 (en) | 2000-09-18 |
Family
ID=14436939
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10657191A Expired - Fee Related JP3088480B2 (en) | 1991-04-12 | 1991-04-12 | Manufacturing method of non-evaporable getter |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3088480B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100320240B1 (en) * | 1999-06-29 | 2002-01-10 | 최인효 | manufacture way of getter and lamp make use of getter |
| KR100381960B1 (en) * | 2000-06-05 | 2003-05-01 | 주식회사 세종소재 | Getter |
| US7315115B1 (en) * | 2000-10-27 | 2008-01-01 | Canon Kabushiki Kaisha | Light-emitting and electron-emitting devices having getter regions |
| JP2009076242A (en) * | 2007-09-19 | 2009-04-09 | Toshiba Hokuto Electronics Corp | Magnetron |
-
1991
- 1991-04-12 JP JP10657191A patent/JP3088480B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH04315730A (en) | 1992-11-06 |
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