JPH01132751A - Clad vessel - Google Patents

Clad vessel

Info

Publication number
JPH01132751A
JPH01132751A JP29019587A JP29019587A JPH01132751A JP H01132751 A JPH01132751 A JP H01132751A JP 29019587 A JP29019587 A JP 29019587A JP 29019587 A JP29019587 A JP 29019587A JP H01132751 A JPH01132751 A JP H01132751A
Authority
JP
Japan
Prior art keywords
oxides
vessel
dispersed
alloy
coating
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
Application number
JP29019587A
Other languages
Japanese (ja)
Other versions
JP2565938B2 (en
Inventor
Chiharu Ishikura
千春 石倉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tanaka Kikinzoku Kogyo KK
Original Assignee
Tanaka Kikinzoku Kogyo KK
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Tanaka Kikinzoku Kogyo KK filed Critical Tanaka Kikinzoku Kogyo KK
Priority to JP62290195A priority Critical patent/JP2565938B2/en
Publication of JPH01132751A publication Critical patent/JPH01132751A/en
Application granted granted Critical
Publication of JP2565938B2 publication Critical patent/JP2565938B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/243Crucibles for source material

Abstract

PURPOSE:To provide a vessel having a long service life in high-temp. use by coating a Ta-base metal with an Rh-base metal in which oxides are dispersed. CONSTITUTION:This clad vessel is formed by coating Ta or Ta alloy with Rh or Rh alloy in which oxides are dispersed. since this vessel has superior oxidation resistance, and further, oxides are dispersed in a coating film and grain growth at high temp. is inhibited, the service life of this vessel is prolonged. Moreover, Al2O3, ZrO2, Y2O3, etc., can be used as the above oxides, and it is preferable to regulate the amount of oxides to about 0.02-10vol.%, The above clad vessel can be manufactured, e.g., by simultaneously using two targets of Rh and Y2O3 and executing binary simultaneous sputtering of the above two targets onto the inner wall of a crucible made of Ta.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は、高温で使用するクラッド容器に関するもので
ある。
DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a clad container used at high temperatures.

(従来技術とその問題点) 従来、Ta又はTa合金にRh又はRh合金を被覆した
クラッド容器は高温ガラスや金属酸化物を含む鉱石溶解
用るつぼや真空蒸着用のトレー、ボートなどに広く用い
られていた。これは耐酸化性に優れているが、高温で使
用するので使用時間と共にRh又はI?h合金膜の結晶
粒が粗大化し、粒界からの他の元素による浸入汚染や膜
の機械的強度の低下でクラッド容器の寿命が短いという
欠点があった。
(Prior art and its problems) Conventionally, clad containers in which Ta or Ta alloy is coated with Rh or Rh alloy have been widely used in crucibles for melting ores containing high-temperature glass and metal oxides, trays for vacuum evaporation, boats, etc. was. This has excellent oxidation resistance, but since it is used at high temperatures, it becomes Rh or I over time. The crystal grains of the h-alloy film become coarse, contamination from other elements enters through the grain boundaries, and the mechanical strength of the film decreases, resulting in a short life span of the cladding container.

本発明は上記欠点に鑑みなされたものであり、長寿命の
容器を提供することを目的とする。
The present invention has been made in view of the above-mentioned drawbacks, and it is an object of the present invention to provide a container with a long life.

(問題点を解決するための手段) 本発明は、Ta又はTa合金に、酸化物を分散させたR
h又はRh合金が被覆されていることを特徴とするクラ
ッド容器である。
(Means for Solving the Problems) The present invention provides an R
This is a clad container characterized by being coated with h or Rh alloy.

本発明において、酸化物を分散させたRh又はRh合金
を用いるのは、Rhの融点が1960℃と高く、しかも
高温における結晶粒の粗大化が起こりにくいからである
。しかし、酸化物を分散させたRhやRh合金を板にす
るなどの加工が困難なため被覆することとした。被覆は
スパッタリングにて行うのが良い。これはイオンブレー
ティングや真空蒸着や湿式めっきでは、Rh又はRh合
金に酸化物を分散させるのが困難な為である。
In the present invention, Rh or Rh alloy in which oxides are dispersed is used because Rh has a high melting point of 1960° C. and grains are less likely to coarsen at high temperatures. However, since it is difficult to process Rh or Rh alloy in which oxides are dispersed into a plate, it was decided to coat the metal. The coating is preferably performed by sputtering. This is because it is difficult to disperse oxides in Rh or Rh alloys by ion blasting, vacuum deposition, or wet plating.

このように酸化物を分散させたRh又はRh合金を被覆
したるつぼは耐酸化性に優れ、しかも被膜中には酸化物
が分散していて高温での結晶粒の成長が抑えられている
ことから長寿命のものとなる。
A crucible coated with Rh or Rh alloy with oxides dispersed in this way has excellent oxidation resistance, and the oxides are dispersed in the coating, which suppresses the growth of crystal grains at high temperatures. It will have a long life.

なお、酸化物を分散したRh合金としては、Rh−pt
−酸化物、Rh−1r−酸化物などがある。
Note that Rh-pt is a Rh alloy with oxides dispersed in it.
-oxide, Rh-1r-oxide, etc.

また酸化物としてはAlzOi、ZrO,、Y z O
sなどがあり、その酸化物の分散量としては、0.02
体積%未満では高温での結晶粒の成長を抑制する効果が
薄く、10体積%を超えると酸化物がクラッド容器内で
溶かすガラス等と反応するので、酸化物の量としては、
0.02〜lO体積%が好ましい。さらに被膜の厚さと
しては、0.1μm未満ではTa又はTa合金の酸化を
防止する効果が薄く、100μmを超えると効果(長寿
命化)に対する被覆時間の割合が高くなるので、被膜の
厚さとしては0.1〜100μmの範囲が好ましい。
In addition, as oxides, AlzOi, ZrO, Y z O
s, etc., and the amount of dispersion of its oxide is 0.02
If it is less than 10% by volume, the effect of suppressing the growth of crystal grains at high temperatures will be weak, and if it exceeds 10% by volume, the oxide will react with the glass etc. to be melted in the cladding container, so the amount of oxide is as follows:
0.02 to 10% by volume is preferred. Furthermore, if the thickness of the coating is less than 0.1 μm, the effect of preventing oxidation of Ta or Ta alloy will be weak, and if it exceeds 100 μm, the ratio of coating time to the effect (longer life) will be high. The preferred range is 0.1 to 100 μm.

以下、実施例と従来例について説明する。Examples and conventional examples will be described below.

(実施例1) RhとY2O,の2つのターゲットを同時に用いて、肉
厚5m、高さ100mm、内径80mの断面コの字形T
a製るつぼの内壁に次の条件でRh  YzOi2.5
体積%を厚さ5μmまで2元同時スパッタリングした。
(Example 1) Using two targets Rh and Y2O at the same time, a U-shaped cross section T with a wall thickness of 5 m, a height of 100 mm, and an inner diameter of 80 m was prepared.
Rh YzOi2.5 was applied to the inner wall of a crucible made of A under the following conditions.
Two-dimensional simultaneous sputtering was performed to a thickness of 5 μm by volume.

Arガス   1.0xlO−’T o r rRh 
 DC2KW、スパッタ速度 1000人/m1nYz
O*  RF  I KW、スパッタ速度 25人/m
in高周波電源 13.56M Hz Ta製るつぼ 自公転 これを実施品lとする。
Ar gas 1.0xlO-'T o r rRh
DC2KW, sputtering speed 1000 people/m1nYz
O* RF I KW, sputtering speed 25 people/m
in high frequency power supply 13.56 MHz Ta crucible Rotation and revolution This is the actual product 1.

(実施例2) Rh  Zr0z0.1体積%のターゲットを用いて、
実施例1と同一形状のTa製るつぼの内外壁に次の条件
でRh−Zr0□0.1体積%を厚さ10μmマグネト
ロンスパッタリングした。
(Example 2) Using a target containing RhZr0z0.1% by volume,
Rh-Zr0□0.1% by volume was magnetron sputtered to a thickness of 10 μm on the inner and outer walls of a Ta crucible having the same shape as in Example 1 under the following conditions.

Arガス    1.0X10−3T o r rIr
 ”1rOt RF  I KW、スパッタ速度200
0人/min高周波電源  13.56M Hz Ta製るつぼ 自転 これを実施晶2とする。
Ar gas 1.0X10-3T or rIr
"1rOt RF I KW, sputtering speed 200
0 people/min High frequency power supply 13.56 MHz Ta crucible Rotation This is used as practical crystal 2.

(従来例) 実施例1で用いたTa製るつぼの内外壁にRhを10μ
mスパッタリングしたものを従来品とした。
(Conventional Example) 10μ of Rh was applied to the inner and outer walls of the Ta crucible used in Example 1.
The conventional product was one subjected to m-sputtering.

次に、上記実施品1.2と従来品にアルカリ亜鉛硼珪酸
ガラスを500g入れAr雰囲気、温度約り200℃×
60分間で使用した。これを10回くり返したところ、
従来品は5μmその容器の表面から削られたのに対し、
実施品1は2μm、実施品2は1μm削られたにとどま
った。
Next, 500 g of alkali zinc borosilicate glass was added to the above implementation product 1.2 and the conventional product in an Ar atmosphere at a temperature of about 200°C.
It was used for 60 minutes. After repeating this 10 times,
Whereas the conventional product had 5 μm removed from the surface of the container,
Execution product 1 was removed by 2 μm, and implementation product 2 was removed by only 1 μm.

次に、従来品、実施品2の容器の底部を大気中で直接ヒ
ーター加熱して温度約1000℃で20時間保持したと
ころ、従来品は10時間では減量しなかったが、Rh被
膜の結晶粒の粗大化が著しく限界状態となり、20時間
ではRh被膜が破壊されTaが殆んど酸化されたのに対
し、実施品2は被膜の結晶粒の成長は認められず、減量
もしなかった。
Next, when the bottoms of the containers of the conventional product and implementation product 2 were directly heated with a heater in the atmosphere and held at a temperature of approximately 1000°C for 20 hours, the conventional product did not lose weight in 10 hours, but the crystal grains of the Rh coating The coarsening of the film reached a critical limit, and after 20 hours, the Rh film was destroyed and most of the Ta was oxidized, whereas in Example 2, no growth of crystal grains in the film was observed and no weight loss was observed.

これらのことから本発明のクラッドるつぼは従来品に比
べて金属酸化物の溶解用るつぼとして著しく寿命が長く
、また耐消耗性にも優れていることがわかる。
From these results, it can be seen that the clad crucible of the present invention has a significantly longer service life as a crucible for dissolving metal oxides than conventional crucibles, and also has excellent wear resistance.

尚、上記実施例ではTaに酸化物を分散したRhを直接
被覆したが、必要に応じTaとRhの拡散を防止するた
めの拡散防止層を介在するようにしてもよいものである
In the above embodiment, Ta is directly coated with Rh in which an oxide is dispersed, but a diffusion prevention layer may be provided to prevent the diffusion of Ta and Rh, if necessary.

(発明の効果) 以上詳述したように本発明によれば、耐消耗性の優れた
長寿命のクラッド容器を提供することができる。しかも
、Ta製容器を完全に被覆すれば大気中でも長寿命のも
のかえられる。
(Effects of the Invention) As detailed above, according to the present invention, it is possible to provide a clad container with excellent wear resistance and long life. Moreover, if the Ta container is completely coated, it can have a long life even in the atmosphere.

出願人  田中貴金属工業株式会社Applicant: Tanaka Kikinzoku Kogyo Co., Ltd.

Claims (1)

【特許請求の範囲】[Claims] Ta又はTa合金に、酸化物を分散させたRh又はRh
合金が被覆されていることを特徴とするクラッド容器。
Rh or Rh with oxide dispersed in Ta or Ta alloy
A clad container characterized by being coated with an alloy.
JP62290195A 1987-11-17 1987-11-17 Clad container Expired - Lifetime JP2565938B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62290195A JP2565938B2 (en) 1987-11-17 1987-11-17 Clad container

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62290195A JP2565938B2 (en) 1987-11-17 1987-11-17 Clad container

Publications (2)

Publication Number Publication Date
JPH01132751A true JPH01132751A (en) 1989-05-25
JP2565938B2 JP2565938B2 (en) 1996-12-18

Family

ID=17752985

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62290195A Expired - Lifetime JP2565938B2 (en) 1987-11-17 1987-11-17 Clad container

Country Status (1)

Country Link
JP (1) JP2565938B2 (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5515550A (en) * 1978-07-18 1980-02-02 Matsushita Electric Works Ltd Smoke sensor
JPS60200978A (en) * 1984-03-26 1985-10-11 Tanaka Kikinzoku Kogyo Kk Clad vessel

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5515550A (en) * 1978-07-18 1980-02-02 Matsushita Electric Works Ltd Smoke sensor
JPS60200978A (en) * 1984-03-26 1985-10-11 Tanaka Kikinzoku Kogyo Kk Clad vessel

Also Published As

Publication number Publication date
JP2565938B2 (en) 1996-12-18

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