JPH01275780A - Clad vessel - Google Patents

Abstract

PURPOSE:To obtain a clad vessel having superior attrition resistance by cladding the inside or the inside and outside of a W or Ta vessel with a thin Ir or Ir alloy film contg. a dispersed nitride, carbide or boride. CONSTITUTION:A corrosion resistant thin alloy film having 0.1-100mum thickness and consisting of Ir or an Ir alloy as a base and 0.02-10vol.% dispersed nitride such as BN, HfN, TaN, ZrN or TiN, carbide such as B4C, TiC, ZrC, HfC, VC, NbC or TaC or boride such as TiB2, ZrB2, HfB2 or CrB2 is formed by sputtering or other method on the inside or the inside and outside of a W or Ta vessel. The mechanical strength of the film is prevented from being reduced by contamination by other element entering from the grain boundary and a clad vessel having a long service life is obtd.

Description

DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a clad container used at high temperatures.

(Prior art and its problems) Conventionally, clad containers made of a high-melting point metal such as WSTa and coated with Ir or Ir alloy have been used for applications such as crucibles for melting ores containing high-temperature glass and metal oxides. was considered.

By the way, the above-mentioned clad container has excellent oxidation resistance, but since it is used at high temperatures, the crystal grains of the Ir or Ir alloy coating become coarse over time, causing contamination and other elements to enter the coating from the grain boundaries. The life of the clad container was shortened due to the decrease in mechanical strength.

(Object of the Invention) The present invention was made to solve the above problems, and an object of the present invention is to provide a clad container with a long life.

(Means for solving the problems) The clad container of the present invention for solving the above problems includes:
The inner or outer surfaces of the container made of W or Ta are coated with a material containing Ir or Ir alloy as the main component and dispersed with any of nitrides, carbides, and borides. .

In the clad container of the present invention, the inner surface or both the inner and outer surfaces of the container made of W or Ta are coated with the above material because it suppresses coarsening of the crystal grains of the Ir or Ir alloy coating at high temperatures. It is.

The coating is preferably performed by sputtering. This is because it is difficult to disperse nitrides, carbides, and borides in Ir or Ir alloys by ion blasting, vacuum deposition, or wet plating.

Ir containing nitrides, carbides, and borides dispersed in this way
Or a clad container coated with a material made of Ir alloy,
It has excellent oxidation resistance, and the coating contains nitrides, carbides, and borides, which suppresses the growth of crystal grains at high temperatures. There is no infiltration of contamination or a decrease in the mechanical strength of the coating, resulting in a long service life.

Nitrides include BN, HfN, TaN, ZrN, Ti
N is used, and the carbides include B and C.

TiC, ZrC, HfC, VC, NbC5TaC are used, and as borides, T IB 2, ZrB2, H
fB2, CrB, is used.

The amount of dispersion of these nitrides, carbides, and borides is 0.
．． If the amount is less than 0.02% 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 effect of suppressing the growth of crystal grains will not change.
．． 02 to 10% by volume is preferred.

Furthermore, if the film thickness is less than 0.1 μm, the effect of preventing oxidation of W or Ta will be weak, and if it exceeds 100 μm, the ratio of coating time to longer life will increase, so the film thickness should be 0.1~ A range of 100 μm is preferred.

Specific examples and conventional examples will be described below.

(Example 1) Using two targets of Ir and BH at the same time,
++un, on the inner surface of a W crucible with a U-shaped cross section and a height of 100 mm and an inner diameter of 80 mm, 2.5 volume % of Ir-BN was sputtered simultaneously to a thickness of 5 μm under the following conditions,
Got a clad crucible.

Ar gas: 1. Qx 1O-3TorrIr:
DC2 to W1 sputtering speed 1000A/m1nBN
: RF IKW, sputtering speed 25 people/mi
n High frequency power source: 13.56 MHz Crucible made of W: Rotation and revolution (Example 2) Using two targets of Ir and TiC at the same time, wall thickness 5Il]ffl, height 100mm, inner diameter 8011110
Ir was applied to the inner and outer surfaces of a W crucible with a U-shaped cross section under the following conditions.
A clad crucible was obtained by dual-sputtering TiC2.5% by volume to a thickness of 10 μm.

Ar gas: 1O-3Torr Ir: DC2KW, sputtering speed 1000A/m1n
TiC: RF IKW, sputtering speed 25 people/min High frequency power source: 13.56 MHz W crucible: Autorotation (Example 3) Using two targets of Ir and ZrBz at the same time, a Ir-Z r B was applied to the inner surface of a Ta crucible with a U-shaped cross section under the following conditions.
, 5% by volume were simultaneously sputtered to a thickness of 20 μm to obtain a clad crucible.

Ar gas: 1O-3Torr Ir: DC2KW, sputtering speed 1000A/m1n
ZrL: RF 2KW, sputtering speed 508/min High frequency power source: 13.56MHz Ta crucible: Rotation (Example 4) Using three targets of IrSPt and TaN at the same time, wall thickness 5mm, height 100mm, inner diameter 80mm Ir and Pt were applied to the inner and outer surfaces of a Ta crucible with a U-shaped cross section.
20wt% and TaN1. Thickness 1 so that O volume %
A clad crucible was obtained by simultaneous three-dimensional sputtering down to 0 μm.

Ar gas: 10-'Torr Ir: DC2KW, sputtering speed 1000A
/m1nPt: DCO, 4KW, sputtering speed 200 people/m1nT aN: RF O, 5KW,
Sputtering speed: 12 people/min High frequency power supply: 13.
56! JHz Ta crucible: Rotation and revolution (conventional example) Ir was applied to the inner and outer surfaces of the W crucible used in Example 1 to a thickness of 1
A clad crucible was obtained by sputtering down to 0 μm.

However, 500 g of alkali zinc borosilicate glass was added to the clad crucibles of Examples 1 to 4 and the conventional clad crucible.
It was used in an Ar atmosphere at a temperature of 1500° C. for 1 hour. When this was repeated 10 times, the Ir coating was removed by 3 μm from the inner surface of the conventional clad crucible, whereas the Ir-BN coating was removed by 0.5 μm from the crucible of Example 1. The Ir-TiC coating was 0.4 μm in the crucible of Example 3, the Ir-ZrB2 coating was 0.5 μm, and the Ir-Pt-TaN coating was 0.5 μm in the crucible of Example 4. Ta.

Next, the bottoms of the clad crucibles of Examples 1 to 4 and the conventional example were directly heated in the atmosphere with a heater at a temperature of about 1000°C for 20 minutes.
In the conventional clad crucible, the weight of the Ir coating did not decrease after 10 hours, but the crystal grains of the Ir coating became extremely coarse, reaching a limit state, and after 20 hours, the Ir coating was destroyed, resulting in a weight loss of 8 g. On the other hand, in all of the clad crucibles of Examples 1 to 4, no growth of crystal grains in the coating was observed and no weight loss was observed.

These results show that the clad crucible of the present invention has a significantly longer life as a crucible for dissolving metal oxides than conventional clad crucibles, and has excellent wear resistance.

(Effects of the Invention) As detailed above, the clad container of the present invention suppresses the coarsening of the crystal grains in the coating, prevents contamination from entering from grain boundaries with other elements, and reduces the mechanical strength of the coating, so it can last for a long time. It is the lifespan. Furthermore, the coating does not lose weight even after long-term use, and has excellent wear resistance. Furthermore, if the entire container is completely coated, it will have a long life even in the atmosphere.

Applicant: Tanaka Kikinzoku Kogyo Co., Ltd.

Claims (1)

[Claims] 1. On the inner or outer surfaces of a container made of W or Ta, I
A cladding container characterized in that it is coated with a material containing an r or Ir alloy as a main component and one of nitrides, carbides, and borides dispersed therein.