CN102086122A - Novel preparation method of ZrO2 ceramic target - Google Patents

Abstract

The invention provides a novel preparation method of a ZrO2 ceramic target. The method solves the technical problems that the currently used ZrO2 ceramic target is only used as a small thin piece for individual small-sized magnetic control sputtering equipment, the thermal barrier property of the ZrO2 ceramic target sprayed on the surface of a product is reduced, and the like. In the preparation method, industrial ZrO2 powder is used as a raw material, and partial electric smelting yttrium is added to stabilize the ZrO2 powder. The ZrO2 ceramic target is prepared by using a cold isostatic molding process and can meet various size requirements, and the volume density and porosity of the target are controlled by the final firing temperature. The density of the ZrO2 target prepared by the preparation method is 3.8-4.8g/cm<3>, the apparent porosity of the ZrO2 target is 12%-38%, and the ZrO2 target is suitable for physical vapor deposition of an electron beam. The technology adopted by the invention is reasonable, the process method is simple and practicable, the size requirements of various targets can be met, and the thermal barrier property of the ZrO2 coating is improved.

Description

A kind of new ZrO＜sub〉2＜/sub〉the ceramic target preparation method

Technical field:

The present invention relates to a kind of new ZrO ₂The ceramic target preparation method, this method adopts industrial ZrO ₂Powder is a raw material, and has added part electric smelting yttrium and stablized ZrO ₂Powder belongs to chemical building material manufacturing and applied technical field as auxiliary material.

Background technology:

The present ZrO that uses ₂Ceramic target is the ZrO of tight burning densification mostly ₂Material can only be used for indivedual small-sized magnetron sputtering equipment as Xiao Bao spare; When being used on the electro beam physics vapour deposition equipment as big thick, under the lasting bombardment of electron beam, owing to its thermal shock performance difference causes target crackle to occur, influence is used; Other has some incomplete agglomerating ZrO ₂Ceramic target can contain unsettled monocline crystalline phase usually, has reduced the thermal boundary performance that sprays to behind the product surface.

Summary of the invention:

The objective of the invention is at above-mentioned existing ZrO ₂The inherent defect of ceramic target provides a kind of new ZrO ₂The ceramic target preparation method when improving thermal shock performance, can provide stable cubic phase crystal, guarantees the performance of thermal barrier coating.

For achieving the above object, the present invention adopts following technical proposals: a kind of new ZrO ₂The ceramic target preparation method is with industrial ZrO ₂Powder is a basic raw material, and has added part electric smelting yttrium and stablized ZrO ₂Powder.This part addition material is suppressing ZrO ₂Phase transformation when stable tetragonal phase composite is provided, is also played the effect of regulating target void content and volume density, has improved the thermal shock performance of target.This ZrO ₂Ceramic target adopts the technology of cold isostatic compaction, can satisfy multiple dimensional requirement, and control the volume density and the void content of target by final firing temperature.

Concrete grammar:

(1) at industrial ZrO ₂In the powder stock, stablize ZrO in the ratio adding electric smelting yttrium of 5%～40% (weight %) ₂Powder mixes;

(2) in the mixed powder of (1) set by step preparation, add 60%～70% moisture content, 1%～3% caking agent, and carry out wet ball grinding 4～8h, make ZrO ₂Slip;

(3) to the ZrO of (2) set by step preparation ₂Slip carries out mist projection granulating to be handled, and makes ZrO ₂Granulation powder, its particle diameter are 75 μ～250 μ;

(4) to the ZrO of (3) set by step preparation ₂The granulation powder carries out cold isostatic compaction, and forming pressure is 40～150MPa, and the dwell time is 30s～240s, obtains ZrO ₂The blank of ceramic target;

(5) to the ZrO of (4) set by step preparation ₂The ceramic target blank carries out repaired biscuit to be handled, and is machined to and burns till perisystolic predetermined size, obtains neat appearance, accurate in size ZrO ₂The biscuit of ceramic target;

(6) the ZrO of (5) set by step preparation ₂The ceramic target biscuit is put into process furnace and is carried out high temperature sintering, and firing temperature is 1400 ℃～1650 ℃, and high-temperature holding time is 1～4h, is met the ZrO of performance requriements ₂Ceramic target.

The ZrO of the present invention's preparation ₂Ceramic target has following obvious advantage:

(1) reasonable in technology of the present invention's employing, processing method is simple, can satisfy the dimensional requirement of various different targets;

(2) ZrO of the present invention's preparation ₂The ceramic target performance is controlled, and its volume density is 3.80～4.80g/cm ³, apparent porosity is 12%～38%.

(3) ZrO of the present invention's preparation ₂Ceramic target had both solved existing ZrO ₂The problem of ceramic target thermal shock performance difference can provide stable cubic phase crystal again, guarantees the performance of thermal barrier coating.

Embodiment

Embodiment 1

At industrial ZrO ₂In the powder stock, the ratio in 5% adds the electric smelting yttrium and stablizes ZrO ₂Powder mixes; In mixed powder, add 1.0% caking agent, and according to material: water: ballstone=carry out wet ball grinding 8h at 1: 0.7: 2 makes ZrO ₂Slip; With these ZrO ₂Slip adopts the press spray drying tower to carry out mist projection granulating and handles, and makes ZrO ₂Granulation powder, its median size are 115 μ; ZrO ₂The granulation powder is packed into and is carried out cold isostatic compaction in the nitrile rubber mould, and forming pressure is 40MPa, thereby pressurize 240s obtains ZrO ₂The blank of ceramic target; Blank to target carries out the repaired biscuit processing, promptly uses the machined into profile to predetermined size, obtains accurate in size ZrO ₂The biscuit of ceramic target; At last biscuit is put into the Si-Mo rod high-temperature heater and carry out sintering, firing temperature is 1400 ℃, and insulation 1h obtains needed ZrO ₂Ceramic target.This ZrO ₂The volume density of target is 3.8g/cm ³, apparent porosity is 38%.

Embodiment 2

At industrial ZrO ₂In the powder stock, the ratio in 10% adds the electric smelting yttrium and stablizes ZrO ₂Powder mixes; In mixed powder, add 1.6% caking agent, and according to material: water: ballstone=carry out wet ball grinding 4h at 1: 0.7: 2 makes ZrO ₂Slip; With these ZrO ₂Slip adopts the press spray drying tower to carry out mist projection granulating and handles, and makes ZrO ₂Granulation powder, its median size are 150 μ; ZrO ₂The granulation powder is packed into and is carried out cold isostatic compaction in the nitrile rubber mould, and forming pressure is 50MPa, thereby pressurize 240s obtains ZrO ₂The blank of ceramic target; Blank to target carries out the repaired biscuit processing, promptly uses the machined into profile to predetermined size, obtains accurate in size ZrO ₂The biscuit of ceramic target; At last biscuit is put into the Si-Mo rod high-temperature heater and carry out sintering, firing temperature is 1650 ℃, and insulation 2h obtains needed ZrO ₂Ceramic target.This ZrO ₂The volume density of target is 4.8g/cm ³, apparent porosity is 12%.

Embodiment 3

At industrial ZrO ₂In the powder stock, the ratio in 15% adds the electric smelting yttrium and stablizes ZrO ₂Powder mixes; In mixed powder, add 1.5% caking agent, and according to material: water: ballstone=carry out wet ball grinding 4h at 1: 0.6: 2 makes ZrO ₂Slip; With these ZrO ₂Slip adopts the press spray drying tower to carry out mist projection granulating and handles, and makes ZrO ₂Granulation powder, its median size are 150 μ; ZrO ₂The granulation powder is packed into and is carried out cold isostatic compaction in the nitrile rubber mould, and forming pressure is 150MPa, pressurize 60s, thus obtain ZrO ₂The blank of ceramic target; Blank to target carries out the repaired biscuit processing, promptly uses the machined into profile to predetermined size, obtains accurate in size ZrO ₂The biscuit of ceramic target; At last biscuit is put into the Si-Mo rod high-temperature heater and carry out sintering, firing temperature is 1580 ℃, and insulation 2h obtains needed ZrO ₂Ceramic target.This ZrO ₂The volume density of target is 4.25g/cm ³, apparent porosity is 27.02%.

Embodiment 4

At industrial ZrO ₂In the powder stock, the ratio in 25% adds the electric smelting yttrium and stablizes ZrO ₂Powder mixes; In mixed powder, add 2.8% caking agent, and according to material: water: ballstone=carry out wet ball grinding 6h at 1: 0.6: 2 makes ZrO ₂Slip; With these ZrO ₂Slip adopts the press spray drying tower to carry out mist projection granulating and handles, and makes ZrO ₂Granulation powder, its median size are 140 μ; ZrO ₂The granulation powder is packed into and is carried out cold isostatic compaction in the nitrile rubber mould, and forming pressure is 150MPa, pressurize 30s, thus obtain ZrO ₂The blank of ceramic target; Blank to target carries out the repaired biscuit processing, promptly uses the machined into profile to predetermined size, obtains accurate in size ZrO ₂The biscuit of ceramic target; At last biscuit is put into the Si-Mo rod high-temperature heater and carry out sintering, firing temperature is 1650 ℃, and insulation 2h obtains needed ZrO ₂Ceramic target.This ZrO ₂The volume density of target is 4.08g/cm ³, apparent porosity is 30.23%.

Embodiment 5

At industrial ZrO ₂In the powder stock, the ratio in 40% adds the electric smelting yttrium and stablizes ZrO ₂Powder mixes; In mixed powder, add 3% caking agent, and according to material: water: ballstone=carry out wet ball grinding 4h at 1: 0.7: 2 makes ZrO ₂Slip; With these ZrO ₂Slip adopts the press spray drying tower to carry out mist projection granulating and handles, and makes ZrO ₂Granulation powder, its median size are 175 μ; ZrO ₂The granulation powder is packed into and is carried out cold isostatic compaction in the nitrile rubber mould, and forming pressure is 150MPa, thereby pressurize 120s obtains ZrO ₂The blank of ceramic target; Blank to target carries out the repaired biscuit processing, promptly uses the machined into profile to predetermined size, obtains accurate in size ZrO ₂The biscuit of ceramic target; At last biscuit is put into the Si-Mo rod high-temperature heater and carry out sintering, firing temperature is 1650 ℃, and insulation 4h obtains needed ZrO ₂Ceramic target.This ZrO ₂The volume density of target is 4.28g/cm ³, apparent porosity is 25%.

Claims (7)

1. new ZrO ₂Ceramic target preparation method, this method are with industrial ZrO ₂Powder is a basic raw material, and has added part electric smelting yttrium and stablized ZrO ₂Powder is as auxiliary material, and this part addition material is suppressing ZrO ₂Phase transformation when stable tetragonal phase composite is provided, is also played the effect of regulating target void content and volume density.

2. a kind of new ZrO as claimed in claim 1 ₂The ceramic target preparation method, it is realized by following steps:

(1) at industrial ZrO ₂In the powder stock, the ratio in 5%～40% adds the electric smelting yttrium and stablizes ZrO ₂Powder mixes;

(2) in the mixed powder of (1) set by step preparation, add 60%～70% moisture content, 1%～3% caking agent, and carry out wet ball grinding 4～8h, make ZrO ₂Slip;

(3) to the ZrO of (2) set by step preparation ₂Slip carries out mist projection granulating to be handled, and makes ZrO ₂Granulation powder, its particle diameter are 75 μ～250 μ;

(4) to the ZrO of (3) set by step preparation ₂The granulation powder carries out cold isostatic compaction, and forming pressure is 40～150MPa, and the dwell time is 30s～240s, obtains ZrO ₂The blank of ceramic target;

(5) to the ZrO of (4) set by step preparation ₂The ceramic target blank carries out repaired biscuit to be handled, and is machined to and burns till perisystolic predetermined size, obtains neat appearance, accurate in size ZrO ₂The biscuit of ceramic target;

(6) the ZrO of (5) set by step preparation ₂The ceramic target biscuit is put into process furnace and is carried out high temperature sintering, and firing temperature is 1400 ℃～1650 ℃, and high-temperature holding time is 1～4h, is met the ZrO of performance requriements ₂Ceramic target.

3. a kind of new ZrO as claimed in claim 2 ₂The ceramic target preparation method, it prepares by following concrete technical qualification:

At industrial ZrO ₂In the powder stock, the ratio in 5% adds the electric smelting yttrium and stablizes ZrO ₂Powder mixes; In mixed powder, add 1.0% caking agent, and according to material: water: ballstone=carry out wet ball grinding 8h at 1: 0.7: 2 makes ZrO ₂Slip; With these ZrO ₂Slip adopts the press spray drying tower to carry out mist projection granulating and handles, and makes ZrO ₂Granulation powder, its median size are 115 μ; ZrO ₂The granulation powder is packed into and is carried out cold isostatic compaction in the nitrile rubber mould, and forming pressure is 40MPa, thereby pressurize 240s obtains ZrO ₂The blank of ceramic target; Blank to target carries out the repaired biscuit processing, promptly uses the machined into profile to predetermined size, obtains accurate in size ZrO ₂The biscuit of ceramic target; At last biscuit is put into the Si-Mo rod high-temperature heater and carry out sintering, firing temperature is 1400 ℃, and insulation 1h obtains needed ZrO ₂Ceramic target.This ZrO ₂The volume density of target is 3.8g/cm ³, apparent porosity is 38%.

4. a kind of new ZrO as claimed in claim 2 ₂The ceramic target preparation method, it prepares by following concrete technical qualification:

At industrial ZrO ₂In the powder stock, the ratio in 10% adds the electric smelting yttrium and stablizes ZrO ₂Powder mixes; In mixed powder, add 1.6% caking agent, and according to material: water: ballstone=carry out wet ball grinding 4h at 1: 0.7: 2 makes ZrO ₂Slip; With these ZrO ₂Slip adopts the press spray drying tower to carry out mist projection granulating and handles, and makes ZrO ₂Granulation powder, its median size are 150 μ; ZrO ₂The granulation powder is packed into and is carried out cold isostatic compaction in the nitrile rubber mould, and forming pressure is 50MPa, thereby pressurize 240s obtains ZrO ₂The blank of ceramic target; Blank to target carries out the repaired biscuit processing, promptly uses the machined into profile to predetermined size, obtains accurate in size ZrO ₂The biscuit of ceramic target; At last biscuit is put into the Si-Mo rod high-temperature heater and carry out sintering, firing temperature is 1650 ℃, and insulation 2h obtains needed ZrO ₂Ceramic target.This ZrO ₂The volume density of target is 4.8g/cm ³, apparent porosity is 12%.

5. a kind of new ZrO as claimed in claim 2 ₂The ceramic target preparation method, it prepares by following concrete technical qualification:

At industrial ZrO ₂In the powder stock, the ratio in 15% adds the electric smelting yttrium and stablizes ZrO ₂Powder mixes; In mixed powder, add 1.5% caking agent, and according to material: water: ballstone=carry out wet ball grinding 4h at 1: 0.6: 2 makes ZrO ₂Slip; With these ZrO ₂Slip adopts the press spray drying tower to carry out mist projection granulating and handles, and makes ZrO ₂Granulation powder, its median size are 150 μ; ZrO ₂The granulation powder is packed into and is carried out cold isostatic compaction in the nitrile rubber mould, and forming pressure is 150MPa, pressurize 60s, thus obtain ZrO ₂The blank of ceramic target; Blank to target carries out the repaired biscuit processing, promptly uses the machined into profile to predetermined size, obtains accurate in size ZrO ₂The biscuit of ceramic target; At last biscuit is put into the Si-Mo rod high-temperature heater and carry out sintering, firing temperature is 1580 ℃, and insulation 2h obtains needed ZrO ₂Ceramic target.This ZrO ₂The volume density of target is 4.25g/cm ³, apparent porosity is 27.02%.

6. a kind of new ZrO as claimed in claim 2 ₂The ceramic target preparation method, it prepares by following concrete technical qualification:

At industrial ZrO ₂In the powder stock, the ratio in 25% adds the electric smelting yttrium and stablizes ZrO ₂Powder mixes; In mixed powder, add 2.8% caking agent, and according to material: water: ballstone=carry out wet ball grinding 6h at 1: 0.6: 2 makes ZrO ₂Slip; With these ZrO ₂Slip adopts the press spray drying tower to carry out mist projection granulating and handles, and makes ZrO ₂Granulation powder, its median size are 140 μ; ZrO ₂The granulation powder is packed into and is carried out cold isostatic compaction in the nitrile rubber mould, and forming pressure is 150MPa, pressurize 30s, thus obtain ZrO ₂The blank of ceramic target; Blank to target carries out the repaired biscuit processing, promptly uses the machined into profile to predetermined size, obtains accurate in size ZrO ₂The biscuit of ceramic target; At last biscuit is put into the Si-Mo rod high-temperature heater and carry out sintering, firing temperature is 1650 ℃, and insulation 2h obtains needed ZrO ₂Ceramic target.This ZrO ₂The volume density of target is 4.08g/cm ³, apparent porosity is 30.23%.

7. a kind of new ZrO as claimed in claim 2 ₂The ceramic target preparation method, it prepares by following concrete technical qualification:

At industrial ZrO ₂In the powder stock, the ratio in 40% adds the electric smelting yttrium and stablizes ZrO ₂Powder mixes; In mixed powder, add 3% caking agent, and according to material: water: ballstone=carry out wet ball grinding 4h at 1: 0.7: 2 makes ZrO ₂Slip; With these ZrO ₂Slip adopts the press spray drying tower to carry out mist projection granulating and handles, and makes ZrO ₂Granulation powder, its median size are 175 μ; ZrO ₂The granulation powder is packed into and is carried out cold isostatic compaction in the nitrile rubber mould, and forming pressure is 150MPa, thereby pressurize 120s obtains ZrO ₂The blank of ceramic target; Blank to target carries out the repaired biscuit processing, promptly uses the machined into profile to predetermined size, obtains accurate in size ZrO ₂The biscuit of ceramic target; At last biscuit is put into the Si-Mo rod high-temperature heater and carry out sintering, firing temperature is 1650 ℃, and insulation 4h obtains needed ZrO ₂Ceramic target.This ZrO ₂The volume density of target is 4.28g/cm ³, apparent porosity is 25%.