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CN116287861A - Titanium-tungsten alloy target plate and preparation method and application thereof - Google Patents

Titanium-tungsten alloy target plate and preparation method and application thereof Download PDF

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Publication number
CN116287861A
CN116287861A CN202310293706.0A CN202310293706A CN116287861A CN 116287861 A CN116287861 A CN 116287861A CN 202310293706 A CN202310293706 A CN 202310293706A CN 116287861 A CN116287861 A CN 116287861A
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CN
China
Prior art keywords
titanium
target plate
tungsten
tungsten alloy
alloy target
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.)
Pending
Application number
CN202310293706.0A
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Chinese (zh)
Inventor
李玉儒
李丽雯
马小红
汪洋
李文儒
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Baoji Hengxin Rare Metals Co ltd
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Baoji Hengxin Rare Metals Co ltd
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Priority to CN202310293706.0A priority Critical patent/CN116287861A/en
Publication of CN116287861A publication Critical patent/CN116287861A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • C22F1/183High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • 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
    • C23C14/34Sputtering
    • C23C14/3407Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a preparation method of a titanium-tungsten alloy target plate, which comprises the following steps: s1, manufacturing an ingot by adopting vacuum arc melting to Ti-20W titanium tungsten alloy target plate; s2, selecting a pure titanium plate with a certain thickness and purity of 99.7%, and preparing an electrode rod by dividing an ultrathin pure tungsten plate with a purity of 99.95% into multiple layers according to a ratio of 81:19, wherein the number of layers is more than 30, and the diagonal line of the electrode size is less than 280mm; and S3, assembling and welding electrodes, and smelting by adopting a high-power 3-ton vacuum consumable arc furnace with high vacuum degree and high current density.

Description

Titanium-tungsten alloy target plate and preparation method and application thereof
The application is a divisional application of 2021, 12/24/202111594983.2 entitled "processing technology of titanium tungsten alloy target plate".
Technical Field
The invention relates to the field of alloy target plate processing, in particular to a titanium tungsten alloy target plate and a preparation method and application thereof.
Background
With the increasing perfection of sputtering technology, vacuum sputtering coating technology has been greatly developed. The corresponding cathode target material is also greatly developed, and various pure metal target plates and various alloy target plates with different proportions are continuously emerging. The vacuum coating industry has two main uses: respectively functional plating and decorative plating. Titanium tungsten is used as a refractory metal, and can be used as decorative plating, such as different colors, and can be used as functional plating, such as high reflectivity. A cell phone, a display screen, a semiconductor, etc. The Ti-20W titanium tungsten alloy target plate is used as a cathode target with special functions and is widely applied to the priming coating of the LED alumina substrate. It has high adhesion rate and high plating rate. The great difference of melting points of titanium and tungsten (titanium 1668 ℃ and tungsten 3400 ℃) brings great difficulty to the manufacture of the alloy. The sintering temperature of the powder metallurgy method is not easy to master, and the defects such as tungsten clamping, segregation and the like often occur, so that the film coating process is unstable, and the film yield is poor. The preparation of Ti-20W titanium tungsten alloy target material belongs to the blank in China.
Disclosure of Invention
The invention aims to solve the problems, and designs a titanium-tungsten alloy target plate and a preparation method and application thereof.
The technical scheme of the invention for achieving the purpose is that the preparation method of the titanium-tungsten alloy target plate.
A preparation method of a titanium-tungsten alloy target plate comprises the following steps:
s1, manufacturing an ingot by adopting vacuum arc melting to Ti-20W titanium tungsten alloy target plate;
s2, selecting a pure titanium plate with a certain thickness and purity of 99.7%, and preparing an electrode rod by dividing an ultrathin pure tungsten sheet into multiple layers according to the proportion of 81:19; the number of layers of the electrode rod is more than 30; the diagonal line of the electrode size of the electrode rod is smaller than 280mm; the ultrathin pure tungsten sheet is an ultrathin pure tungsten sheet with the purity of 99.95 percent;
s3, assembling and welding electrodes, and smelting by adopting a high-power 3-ton vacuum consumable arc furnace with high vacuum degree and high current density;
s4, the tungsten content is 19-21%, and the tungsten content in the three analysis titanium-tungsten alloy plates is not more than 5%;
s5, forging and cogging the ingot, wherein the cogging temperature is 1200-1250 ℃, the final forging temperature is more than 850 ℃, and the ingot is manufactured into a slab with the thickness of 80-100mm, and the slab after planing is hot rolled by a rolling mill with the rolling force more than 1000 tons;
s6, plate annealing and straightening treatment after target plate rolling;
s7, blanking of the rolled target plate is interrupted, and planing, grinding and machining are carried out;
and S8, the size of the target plate is 15 x 127 x 606, the surface roughness of the target plate is 1.6 microns, and steps are processed on the periphery of the target material to obtain the titanium-tungsten alloy target plate.
Preferably, the smelting times in S3: 3-4 times, sampling and analyzing the ingot, and sampling points: and 5-6 parts of the ingot in the length direction.
Preferably, the hot rolling temperature in S5: 1050-1100 ℃, and the finishing temperature is more than 800 ℃.
Preferably, the forging cogging temperature in S5 is 1200 to 1250 ℃, and the final forging temperature is >850 ℃.
The invention also provides the titanium-tungsten alloy target plate prepared by the preparation method.
The invention also provides the titanium-tungsten alloy target plate prepared by the preparation method or application of the titanium-tungsten alloy target plate in the LED cathode target material.
The beneficial effects of the invention are as follows: the alloy target plate has higher reflectivity, high plating rate and very high yield, greatly improves the quality and the yield of the LED, and is the basis for producing high-performance LEDs. Has great economic benefit.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the drawings that are needed in the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural view of an alloy target plate according to the present invention.
Detailed Description
A processing technology of a titanium tungsten alloy target plate comprises the following steps:
s1, manufacturing an ingot by adopting vacuum arc melting to Ti-20W titanium tungsten alloy target plate;
s2, selecting a pure titanium plate with a certain thickness and purity of 99.7%, and preparing an electrode rod by dividing an ultrathin pure tungsten sheet into multiple layers according to the proportion of 81:19, wherein the diagonal line of the electrode size is smaller than 280mm;
s3, assembling and welding electrodes, and smelting by adopting a high-power 3-ton vacuum consumable arc furnace with high vacuum degree and high current density;
s4, the tungsten content is 19-21%, and the tungsten content in the three analysis titanium-tungsten alloy plates is not more than 5%;
s5, forging and cogging an ingot to prepare a slab with the thickness of 80-100mm, and hot rolling the planed slab, wherein the rolling force of a rolling mill is more than 1000 tons;
s6, plate annealing and straightening treatment after target plate rolling;
s7, blanking of the rolled target plate is interrupted, and planing, grinding and machining are carried out;
s8, processing steps on the periphery of the target material, wherein the size of the target plate is 15 x 127 x 606, the surface roughness of the target plate is 1.6 microns;
and S9, fixing the processed target on a coating machine for vacuum sputtering coating.
The smelting times in S3 are as follows: 3-4 times, the ingot is sampled and analyzed, and sampling points are: and 5-6 parts of the ingot in the length direction.
The ultra-thin pure tungsten sheet is an ultra-thin pure tungsten sheet with the purity of 99.95 percent.
Rolling temperature in S5: 1050-1100 ℃, and the finishing temperature is more than 800 ℃.
In the step S2, the number of layers of the electrode rod is more than 30;
and S5, cogging temperature is 1200-1250 ℃, and final forging temperature is more than 850 ℃.
The above technical solution only represents the preferred technical solution of the present invention, and some changes that may be made by those skilled in the art to some parts of the technical solution represent the principles of the present invention, and the technical solution falls within the scope of the present invention.

Claims (6)

1. A preparation method of a titanium-tungsten alloy target plate comprises the following steps:
s1, manufacturing an ingot by adopting vacuum arc melting to Ti-20W titanium tungsten alloy target plate;
s2, selecting a pure titanium plate with a certain thickness and purity of 99.7%, and preparing an electrode rod by dividing an ultrathin pure tungsten sheet into multiple layers according to the proportion of 81:19; the number of layers of the electrode rod is more than 30; the diagonal line of the electrode size of the electrode rod is smaller than 280mm; the ultrathin pure tungsten sheet is an ultrathin pure tungsten sheet with the purity of 99.95 percent;
s3, assembling and welding electrodes, and smelting by adopting a high-power 3-ton vacuum consumable arc furnace with high vacuum degree and high current density;
s4, the tungsten content is 19-21%, and the tungsten content in the three analysis titanium-tungsten alloy plates is not more than 5%;
s5, forging and cogging an ingot to prepare a slab with the thickness of 80-100mm, and hot rolling the slab after planing, wherein the rolling force of a rolling mill is more than 1000 tons;
s6, plate annealing and straightening treatment after target plate rolling;
s7, blanking of the rolled target plate is interrupted, and planing, grinding and machining are carried out;
and S8, the size of the target plate is 15 x 127 x 606, the surface roughness of the target plate is 1.6 microns, and steps are processed on the periphery of the target material to obtain the titanium-tungsten alloy target plate.
2. The method according to claim 1, wherein the number of times of smelting in S3: 3-4 times, sampling and analyzing the ingot, and sampling points: the length direction of the ingot is 5 to 6.
3. The method according to claim 1, wherein the hot rolling temperature in S5: 1050-1100 ℃, and the finishing temperature is more than 800 ℃.
4. The method according to claim 1, wherein the forging cogging temperature in S5 is 1200 to 1250 ℃ and the final forging temperature is >850 ℃.
5. The titanium-tungsten alloy target plate prepared by the preparation method of any one of claims 1 to 4.
6. The titanium-tungsten alloy target plate prepared by the preparation method of any one of claims 1 to 4 or the application of the titanium-tungsten alloy target plate in an LED cathode target material.
CN202310293706.0A 2021-12-24 2021-12-24 Titanium-tungsten alloy target plate and preparation method and application thereof Pending CN116287861A (en)

Priority Applications (1)

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CN202111594983.2A CN114480915A (en) 2021-12-24 2021-12-24 Processing technology of titanium-tungsten alloy target plate
CN202310293706.0A CN116287861A (en) 2021-12-24 2021-12-24 Titanium-tungsten alloy target plate and preparation method and application thereof

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1447864A (en) * 2000-08-15 2003-10-08 霍尼韦尔国际公司 Sputtering target
CN101967569A (en) * 2010-09-27 2011-02-09 西安西工大超晶科技发展有限责任公司 Tungsten-containing titanium alloy smelting method
CN102965531A (en) * 2012-12-14 2013-03-13 西北有色金属研究院 Preparation method of titanium alloy cast ingot containing high-melting-point elements
CN110295301A (en) * 2019-07-09 2019-10-01 中国兵器科学研究院宁波分院 A kind of preparation method of tungsten-titanium alloy
WO2019228963A1 (en) * 2018-05-28 2019-12-05 Life Vascular Devices Biotech, S.L. A beta-phase titanium and tungsten alloy

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1447864A (en) * 2000-08-15 2003-10-08 霍尼韦尔国际公司 Sputtering target
CN101967569A (en) * 2010-09-27 2011-02-09 西安西工大超晶科技发展有限责任公司 Tungsten-containing titanium alloy smelting method
CN102965531A (en) * 2012-12-14 2013-03-13 西北有色金属研究院 Preparation method of titanium alloy cast ingot containing high-melting-point elements
WO2019228963A1 (en) * 2018-05-28 2019-12-05 Life Vascular Devices Biotech, S.L. A beta-phase titanium and tungsten alloy
CN110295301A (en) * 2019-07-09 2019-10-01 中国兵器科学研究院宁波分院 A kind of preparation method of tungsten-titanium alloy

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