CN107385399A - A kind of pressing method of vanadium pipe target - Google Patents

A kind of pressing method of vanadium pipe target Download PDF

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Publication number
CN107385399A
CN107385399A CN201710611024.4A CN201710611024A CN107385399A CN 107385399 A CN107385399 A CN 107385399A CN 201710611024 A CN201710611024 A CN 201710611024A CN 107385399 A CN107385399 A CN 107385399A
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CN
China
Prior art keywords
vanadium
pipe
pressing method
pipe target
vanadium pipe
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
CN201710611024.4A
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Chinese (zh)
Inventor
王延龙
彭凌剑
李军
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Beijing Xing Rong Yuan Technology Co Ltd
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Beijing Xing Rong Yuan Technology Co Ltd
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Priority to CN201710611024.4A priority Critical patent/CN107385399A/en
Publication of CN107385399A publication Critical patent/CN107385399A/en
Pending legal-status Critical Current

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    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23PMETAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
    • B23P15/00Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials 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)

Abstract

The invention belongs to non-ferrous metal high temperature process manufacturing field.The invention provides a kind of pressing method of vanadium pipe target, and a diameter of 150~Φ of Φ 215mm high purity vanadium ingot, car light vanadium ingot outer surface are obtained by vacuum electron beam smelting metal vanadium block.Then a diameter of 50~Φ of Φ 125mm vanadium rod is drawn out by way of electric spark-erosion perforation and wire cutting.The inside and outside wall of vanadium pipe and end face are coated using sheath material, and welded seal.750~1000 degree are heated to, after being incubated 1~2hrs, by the vanadium blank of compressive zone jacket, obtains the vanadium pipe of intermediate sizes, handles and machine the finished product vanadium pipe target needed finally by alignment;Such a pressing method realizes the volume production of qualified vanadium pipe target.

Description

A kind of pressing method of vanadium pipe target
Technical field
The invention belongs to non-ferrous metal high temperature process manufacturing field, more particularly to a kind of manufacture method of vanadium pipe target.
Background technology
Vanadium dioxide (VO2) film is 68 DEG C for the phase transition temperature of metal phase by semiconductor phase in version, along with turning for phase Become, invertibity mutation occurs for the electrical and optical performance of VO2 films so that VO2 films turn into manufacture electricity, the reason of optics Think functional material.Such as it can be made into micro-metering bolometer, memory, photoswitch etc.., can be phase by film doping technology Temperature is reduced to room temperature, and when temperature changes, the transmission coefficient for producing phase transformation coating also changes therewith, particularly For smart window to be made, there is highly important meaning for saving the energy.
Currently, because in the market vanadium amount of target material is seldom, and its thermal deformation is easily ftractureed, so the vanadium target of the overwhelming majority is All it is flat target.It is well known that because planar targets only etch in sputter procedure along field circuit, in target Surface forms " runway ", and target utilization is at most 20%~30%, moreover, planar targets need frequently to change, it is difficult to carry out Continuous production, therefore target utilization is low, causes cost very high.
But for tubular target, rectangle magnetic field makes the uneven of fixed point by carrying out rotation sweep to tubular target Etching becomes the uniform etching of whole target outer surface, the utilization rate of tubular sputtering target has been brought up to 50%~65%. For noble metal plated film, the raising of target utilization is to reduce the most important method of cost.And it is tubular target in length Degree has splendid plating film uniformity on direction, and therefore, developing tubulose vanadium target both has good economic benefit, also to vanadium pipe Coating technique serves facilitation.
But because current vanadium pipe target overall consumption is few, more than external diameter 100mm high purity vanadium pipe, a domestic annual consumption is no more than 10, and vanadium metal price is very high (about 2000 yuan of per kilograms), easily cracking etc. is asked when also depositing at high temperature easily oxidation, deformation Topic, therefore few units and enterprise are ready to put into development costs exploitation vanadium pipe target.
The content of the invention
The technical problems to be solved by the invention are to be directed to above-mentioned the deficiencies in the prior art, answer the requirement of client, develop Go out it is a kind of can manufacture, the pressing method of the vanadium pipe target of stable performance.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is:Pass through the vanadium to electronic torch melting twice Ingot, processing is machined out, car light outer surface, centre bore is drawn out in inside.Then using sheath material by the inside and outside wall of vanadium pipe and End face coats, and welded seal.The vanadium pipe target for needing size is obtained by way of extruding after heating at high temperature.
Characterized in that, this method comprises the following steps:
Step 1: feed metal vanadium is used into 2 vacuum electron beam meltings, and a diameter of 150~215mm of Φ are cast into, Purity is more than 99.9% high purity vanadium ingot.
Step 2: vanadium ingot is machined out, car light outer surface:Then after beating the centre bores of Φ 3 using electric spark, line is passed through The mode of cutting, a diameter of 50~Φ of Φ 125mm vanadium rod is drawn out out from vanadium ingot center, obtains vanadium pipe crude green body.
Step 3: vanadium pipe crude green body surfaces externally and internally is cleaned using high temperature degreaser, it is ensured that without greasy residues;
Step 4: coating the inside and outside wall of vanadium blank using 8mm red copper soil weld, vanadium is coated using 2mm copper plate Blank end face, and welded seal, it is ensured that the surface of vanadium pipe crude green body is all covered by copper coin jacket.
Step 5: by the vanadium pipe crude green body of coated copper jacket, (in the atmosphere of hydrogeneous 2%), it is heated in nitrogen hydrogen mixeding gas 750~1000 degree, after being incubated 1~2hrs, by the vanadium pipe crude green body of compressive zone jacket, extrusion ratio is 1.5~4, and extrusion speed is 10~50mm/ minutes, it is Φ 120~Φ 180mm to obtain external diameter, and wall thickness is 8~20mm vanadium pipe;
Step 6: alignment is handled:After extruding, straightener is directly entered, alignment processing, straight line are carried out using the residual temperature of material Degree is less than 2mm;
Step 7: finally by machining, the copper-clad set of inner and outer surfaces is fallen in turning, the finished product vanadium pipe target needed;
The present invention compared with prior art, has advantages below:
1, the present invention obtains tubulose vanadium target using extrusion process, and the utilization rate of vanadium target improves 30~40%;
2, the present invention is using copper-clad set cladding vanadium pipe crude green body, it is therefore prevented that the oxidation of vanadium pipe, copper-clad set also increase extrusion process In mobility, the defects of avoiding vanadium pipe surface gouge;
Embodiment
With reference to specific embodiment, the present invention is described in detail, but the present invention is not limited thereto.
Step 1: the specification of niobium pipe target finished product manufactured in the present embodiment is:External diameter Φ 154, internal diameter Φ 125, length are 1590mm;
Step 2: using 2 vacuum electron beam meltings and being cast into diameter of phi 215mm, length 545mm, purity is more than 99.9% high purity vanadium ingot;
Step 3: vanadium ingot is machined out, car light outer surface.Then after beating the holes of Φ 3 using electric spark, wire cutting is passed through Mode, a diameter of Φ 123mm vanadium rod is drawn out out from vanadium ingot center, obtains external diameter Φ 213, internal diameter 123mm, length is 540mm vanadium pipe crude green body.
Step 4: under~60 degrees Celsius of water temperature, degreaser for metals is put into, cleans vanadium pipe crude green body surfaces externally and internally, it is ensured that There is no greasy residues, and dry.
Step 5: inside and outside wall and the end face of cladding vanadium blank are welded using 8mm copper coin, and welded seal, it is ensured that vanadium The surface of pipe crude green body is all covered by copper coin jacket.External diameter Φ 229, internal diameter 107mm are obtained, length is 544mm band jacket Vanadium pipe crude green body.
Step 5: by the vanadium pipe crude green body of coated copper jacket, (in the atmosphere of hydrogeneous 2%), it is heated in nitrogen hydrogen mixeding gas 850 degree, after being incubated 1 hour, the vanadium pipe crude green body of compressive zone jacket, extrusion ratio 3.1, extrusion speed is 15mm/ minutes, finally It is to the pipe ingot size with jacket skin:External diameter is Φ 164mm, and internal diameter 120mm, length is 1650mm semi-finished product;
Step 6: alignment is handled:After extruding, straightener is directly entered, alignment processing, straight line are carried out using the residual temperature of material Degree is less than 2mm;
Step 7: by machining, the copper-clad set of inner and outer surfaces is fallen in turning, and it is external diameter Φ 154, internal diameter Φ to obtain size 125, length is 1590mm finished product vanadium pipe targets;
It is described above, only it is the case study on implementation of the present invention, any restrictions is not done to the present invention, it is every according to of the invention real The technical parameter or the change of size etc. that matter is done, in mean technical solution of the present invention protection domain.

Claims (7)

  1. A kind of 1. pressing method of vanadium pipe target, it is characterised in that:Vanadium pipe target is successfully realized by the technique of sheathed extrusion Batch production;A diameter of 150~Φ of Φ 215mm high purity vanadium ingot is obtained particular by vacuum electron beam smelting metal vanadium block, And car light vanadium ingot outer surface;Then a diameter of 50~Φ of Φ 125mm vanadium is drawn out by way of electric spark-erosion perforation and wire cutting Rod;Vanadium pipe crude green body is obtained, and is cleaned up;The inside and outside wall of vanadium pipe crude green body and end face are coated using sheath material, and welded close Envelope;750~1000 degree are heated to, after being incubated 1~2hrs, by the vanadium blank of compressive zone jacket, obtains the vanadium of intermediate sizes Pipe, the finished product vanadium pipe target needed is handled and machined finally by alignment;Such a pressing method efficiently solves vanadium pipe The problem of handling ease is aoxidized and ftractureed under high temperature, successfully produce the vanadium pipe target of excellent performance.
  2. 2. the pressing method of a kind of vanadium pipe target according to claim 1, it is characterised in that described vacuum electron beam melts Refining is to use electronic torch melting twice.
  3. A kind of 3. pressing method of vanadium pipe target according to claim 1, it is characterised in that described high purity vanadium ingot, its Purity is more than 99.9%.
  4. 4. the pressing method of a kind of vanadium pipe target according to claim 1, it is characterised in that described uses sheath material The inside and outside wall of vanadium pipe crude green body and end face are coated, and welded seal, be using 8mm red copper soil weld cladding vanadium blank it is interior, Outer wall;Vanadium blank end face, and welded seal are coated using 2mm copper plate.
  5. A kind of 5. pressing method of vanadium pipe target according to claim 1, it is characterised in that it is described be heated to 750~ 1000 degree, refer to (in the atmosphere of hydrogeneous 2%), be heated to 750~1000 degree, the oxygen for preventing copper-clad from covering in nitrogen hydrogen mixeding gas Change.
  6. 6. the pressing method of a kind of vanadium pipe target according to claim 1, it is characterised in that described to pass through compressive zone bag The vanadium blank of set, obtains the vanadium pipe of intermediate sizes, and its extruding rate is that 10~20mm is per minute.
  7. A kind of 7. pressing method of vanadium pipe target according to claim 1, it is characterised in that described finished product vanadium pipe target Material, it is that size is that external diameter is Φ 100~Φ 200mm, wall thickness is 6~30mm, more than length 500mm vanadium pipe.
CN201710611024.4A 2017-07-25 2017-07-25 A kind of pressing method of vanadium pipe target Pending CN107385399A (en)

Priority Applications (1)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111530962A (en) * 2020-05-14 2020-08-14 成都先进金属材料产业技术研究院有限公司 Production method for small-caliber thick-wall titanium alloy seamless pipe
CN116460165A (en) * 2023-06-20 2023-07-21 西安聚能超导线材科技有限公司 Tantalum tube preparation method, tantalum tube and superconducting wire

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102489951A (en) * 2011-12-03 2012-06-13 西北有色金属研究院 Preparation method of niobium tubular target materials for sputtering
CN102794617A (en) * 2012-09-09 2012-11-28 西安方科新材料科技有限公司 Preparation method of tubular niobium target for magnetron sputtering
CN103009000A (en) * 2012-12-18 2013-04-03 宁夏东方钽业股份有限公司 Niobium target and preparation method of niobium target
CN103071791A (en) * 2013-01-18 2013-05-01 航天材料及工艺研究所 Forming method of TiAl pipe target material in large length-diameter ratio
CN103757592A (en) * 2014-02-19 2014-04-30 宁夏东方钽业股份有限公司 Niobium target preparation method
CN104480437A (en) * 2014-12-30 2015-04-01 山东昊轩电子陶瓷材料有限公司 Production method for integrally formed cylindrical target
CN106676484A (en) * 2015-11-10 2017-05-17 航天长征睿特科技有限公司 Binding method of chrome pipe target material

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102489951A (en) * 2011-12-03 2012-06-13 西北有色金属研究院 Preparation method of niobium tubular target materials for sputtering
CN102794617A (en) * 2012-09-09 2012-11-28 西安方科新材料科技有限公司 Preparation method of tubular niobium target for magnetron sputtering
CN103009000A (en) * 2012-12-18 2013-04-03 宁夏东方钽业股份有限公司 Niobium target and preparation method of niobium target
CN103071791A (en) * 2013-01-18 2013-05-01 航天材料及工艺研究所 Forming method of TiAl pipe target material in large length-diameter ratio
CN103757592A (en) * 2014-02-19 2014-04-30 宁夏东方钽业股份有限公司 Niobium target preparation method
CN104480437A (en) * 2014-12-30 2015-04-01 山东昊轩电子陶瓷材料有限公司 Production method for integrally formed cylindrical target
CN106676484A (en) * 2015-11-10 2017-05-17 航天长征睿特科技有限公司 Binding method of chrome pipe target material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111530962A (en) * 2020-05-14 2020-08-14 成都先进金属材料产业技术研究院有限公司 Production method for small-caliber thick-wall titanium alloy seamless pipe
CN116460165A (en) * 2023-06-20 2023-07-21 西安聚能超导线材科技有限公司 Tantalum tube preparation method, tantalum tube and superconducting wire
CN116460165B (en) * 2023-06-20 2024-03-19 西安聚能超导线材科技有限公司 Tantalum tube preparation method, tantalum tube and superconducting wire

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Application publication date: 20171124