CN104651787B - Manufacturing method for niobium tube target material - Google Patents
Manufacturing method for niobium tube target material Download PDFInfo
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- CN104651787B CN104651787B CN201310596413.6A CN201310596413A CN104651787B CN 104651787 B CN104651787 B CN 104651787B CN 201310596413 A CN201310596413 A CN 201310596413A CN 104651787 B CN104651787 B CN 104651787B
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- niobium
- ingot
- endoporus
- manufacture method
- heating
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
Abstract
The invention discloses a manufacturing method for a niobium tube target material. With a niobium ingot as the raw material, the method sequentially includes the steps of: primary machining, heating, inner hole expanding, extrusion, heat treatment, and secondary machining to obtain a finished product. The method has the advantages of simple process, high material utilization, low production cost, environmental protection and no pollution, etc.
Description
Technical field
The invention belongs to refractory metal deformation processing field, more particularly to a kind of manufacture method of niobium pipe target, the niobium pipe
Target is particularly suitable for magnetron sputtering use.
Background technology
With the fast development of flat pannel display and photovoltaic industry, niobium target market demand increasingly increases, due in target
During use, the utilization rate of tubular target is far above flat target utilization rate, be its more than 2 times, so exploitation plane shows and light
Volt industry is very urgent with large scale niobium pipe target.Nb2O5Thin film has excellent optical property, and its optical waveguide loss is little, in ripple
Conductivity type SHG（second-harmonic generation）Extensively apply in device.Due to Nb2O5Thin film has stronger ultraviolet suction
Receipts ability, can be used as the protecting film of ultraviolet sensitivity material.Due to Nb2O5Film refractive index is higher, with SiO2Tool can be prepared Deng cooperation
There is the thin film of different refractivity.In recent years, Nb2O5Thin film causes researcher as a kind of electrochromic material of function admirable
Broad interest.
2468 DEG C of the fusing point of niobium, 4742 DEG C of boiling point, 8.57 grams/cc of density, body-centered cubic structure.Under room temperature, niobium exists
It is stable in air, be not also fully oxidized during red heat in oxygen, with sulfur, nitrogen, the direct chemical combination of carbon under high temperature, can with titanium, zirconium,
Hafnium, tungsten form alloy.Do not act on mineral acid or alkali, be also insoluble in chloroazotic acid, but dissolve in Fluohydric acid..The oxidation state of niobium be -1 ,+
2nd ,+3 ,+4 and+5, wherein most stable with+5 valency compounds.Nb2O5The more and more extensive purposes of thin film, the demand of Nb targets are more next
It is more, in view of Nb prices are higher, and easily aoxidize, so development cost is cheap, large scale, the life of environment friendly and pollution-free niobium pipe target
Product method is very important.
At present, the method for manufacturing niobium pipe target mainly has two kinds, forging method and sheathed extrusion method.
（1）Forging method：To forge after the niobium ingot heating of vacuum melting, the cylindrical external diameter for being swaged to required pipe is recycled
The method of machining processes internal diameter to given size.The advantage of the method is process is simple, is easily realized；The shortcoming of the method
It is that stock utilization is low, high cost is affected by endoporus machining, and the length of finished product is restricted.
（2）Sheathed extrusion method：Method as described in the patent application of Publication No. CN102489951A：Using vacuum
The niobium ingot of melting, it is machined to draw endoporus（Hole size is slightly larger than finished product niobium bore, such as finished product niobium bore
128mm, drawn endoporus are 135mm）, jacket, heating, extruding, pickling（Remove jacket skin）, heat treatment, be machined into finished product.
The advantage of the method is to produce the niobium pipe target of all size size, uniform small grains；The shortcoming of the method is technique stream
Journey is long, complex process, and too substantially stock utilization is low for drawn hole size, and high cost, pickling have pollution to environment.
Also pickling is used in many other methods, environmental pollution is larger.
The content of the invention
For the deficiencies in the prior art, it is an object of the invention to provide a kind of manufacture method of niobium pipe target.The method
Process is simple, stock utilization are high, and low production cost is environment friendly and pollution-free, and the niobium pipe target obtained using the method is particularly suitable
In magnetron sputtering.
To achieve these goals, the present invention is employed the following technical solutions：
A kind of manufacture method of niobium pipe target, the method with niobium ingot as raw material, successively including one-time mechanical procedure of processing, plus
Hot step, expansion endoporus step, pressing steps, heat treatment step and secondary mechanical are processed into finished product step, wherein：
In the one-time mechanical procedure of processing, by extruding requirement by Raw material processing into the cylindrical ingot blank containing endoporus；
In the heating stepses, in the surface of ingot blank coating antioxidant coating Jing after one-time mechanical processing, then in 900
～1350 DEG C are incubated 0.5～2 hour；
In the pressing steps, having been expanded the ingot blank of endoporus is carried out after 0.1～0.5 hour in 900～1350 DEG C of insulations
Extrusion molding, deflection are not less than 70%；
In the heat treatment step, 900～1350 by the niobium hollow forging after extrusion molding in a vacuum or inert atmosphere
DEG C insulation 0.5～3 hour, then furnace cooling.
Said method is illustrated in order to more detailed, said method can be illustratively described as：
In the heating stepses, in the surface of ingot blank coating antioxidant coating Jing after one-time mechanical processing, then in 900
DEG C, 950 DEG C, 980 DEG C, 1100 DEG C, 1160 DEG C, 1200 DEG C, 1300 DEG C, be incubated under the conditions of 1340 DEG C or 1350 DEG C 0.5h, 1h,
1.5h or 1.8h；
In the pressing steps, expanded the ingot blank of endoporus 900 DEG C, 950 DEG C, 980 DEG C, 1100 DEG C, 1160 DEG C,
Extrusion molding is carried out after 0.2h, 0.3h, 0.4h or 0.5h are incubated under the conditions of 1200 DEG C, 1300 DEG C, 1340 DEG C or 1350 DEG C, is deformed
Amount 72%, 75%, 80%, 85% or 90%；
In the heat treatment step, by the niobium hollow forging after extrusion molding in a vacuum or inert atmosphere, 920 DEG C, 950
DEG C, 1050 DEG C, 1120 DEG C, 1290 DEG C, 1310 DEG C or 1340 DEG C insulation 0.5h, 0.8h, 1.5h, 2.3h or 2.8h, then with stove
Cooling.
In the above-mentioned methods, as a kind of preferred implementation, in the one-time mechanical procedure of processing, the ingot blank
Length is not more than 1100mm, and diameter of bore is 50～60mm, and exemplarily, length can be 900mm, 800mm or 700mm, interior
Bore dia is 50mm, 52mm, 55mm, 57mm, 58mm, 60mm.More preferably diameter of bore is 55～60mm.
In the above-mentioned methods, the antioxidant coating in the heating stepses can be any painting with anti-oxidation function
Material.
In the above-mentioned methods, the mode of heating in the heating stepses and the pressing steps is in the present invention without special
Limit, as a kind of preferred implementation, can be resistance heating or sensing heating.
In the above-mentioned methods, as a kind of preferred implementation, in the pressing steps, the deflection is 75%-
85%, material deformation can be made more thorough in the range of the deflection.
In the above-mentioned methods, the surface of ingot blank in the heating stepses is referred to and all in ingot blank can be arrived with air contact
Position, i.e., including ingot blank outer surface and bore area.
In the above-mentioned methods, the preparation method of the raw material niobium ingot has no particular limits, but in order to realize finished product target
The high-purity of material simultaneously has uniform grain structure, what the raw material niobium ingot was preferably obtained using vacuum smelting method.It is described
Vacuum smelting method is technique well known to those skilled in the art.
In the above-mentioned methods, the expansion endoporus step is carried out in staving press, it is preferable that ingot blank before and after expansion endoporus
Diameter of bore ratio is 1：2～4.
As niobium is very easy to oxidation under more than 400 DEG C of atmospheric condition, so anti-to surface of ingot blank coating before heating
Oxide covering；In order to save raw material, stock utilization is improved, before extrusion first reaming.
The present invention has process is simple compared with prior art, and stock utilization is high, low production cost, environment friendly and pollution-free etc.
Advantage.Above-mentioned advantage is specific as follows：Endoporus as 50～60mm can be only processed as when niobium ingot one-time mechanical is processed, so
The utilization rate of material is very high；Due to surface-coated antioxidant coating, jacket and pickling are eliminated, operation is shortened, is saved into
This, protects environment.
Description of the drawings
Fig. 1 is the metallographic structure figure of niobium pipe target prepared by the embodiment of the present invention 1.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail, but the present invention is not limited to this.
Embodiment 1-3 is to adopt vacuum melting according to the manufacture method of magnetron sputtering niobium pipe target of the present invention
Niobium ingot Jing extrusion processes prepare niobium pipe target, are prepared for the niobium pipe target of 3 kinds of specifications.Antioxidizing paint used in following examples is
Purchased from the prosperous auspicious HX-031 high-temp. resistant antioxidation coatings into Science and Technology Ltd. of Beijing remittance.
Embodiment 1
Niobium pipe target finished product manufactured in the present embodiment（I.e. hollow cylindrical target）Specification be：Cylindrical/diameter of bore
For 155/115mm；Length is 6200mm.
Concrete preparation method is as follows：
（1）The preparation of raw material niobium ingot：Using vacuum electron beam stove, vacuum is 10-3Pa, through secondary smelting, obtains
Niobium ingot purity is 99.98% or so.
（2）Once machine：Raw material niobium ingot is machined into into the cylindrical ingot blank containing endoporus, its ingot blank by extruding requirement
Cylindrical/diameter of bore be 300/60mm, length is 1100mm；
（3）Heating：By all surface of the niobium ingot of the cylinder with endoporus after once machining（Containing bore area）Apply
Antioxidant coating is covered, is then placed in heating furnace, 0.5 hour is incubated at 1350 DEG C；
（4）Expand endoporus：The niobium ingot for completing heating stepses is put in staving press carries out reaming, and the diameter for expanding endoporus is arrived
120mm；
（5）Extrusion molding：The niobium ingot for completing expansion endoporus is melted down again and is placed again into heating furnace（Mode of heating is resistance
Heating）In, being extruded in being put into extruder after being incubated 0.2 hour at 1350 DEG C, deflection is 85%, the niobium obtained after extruding
Cylindrical/the diameter of bore of hollow forging is 160/110mm.
（6）Heat treatment：The niobium hollow forging for having extruded is put in the annealing furnace of vacuum atmosphere, vacuum is 10-3Pa, 1350
DEG C insulation 0.5 hour, then furnace cooling；
（7）Secondary mechanical is processed：Niobium hollow forging through heat treatment is machined to the production tube of given size.
The production tube even tissue that the present embodiment is obtained, crystal grain are tiny, and its performance is shown in Table 1 with cost.Its metallographic structure figure
See Fig. 1.
Embodiment 2
Niobium pipe target finished product manufactured in the present embodiment（I.e. hollow cylindrical target）Specification be：Cylindrical/diameter of bore
For 73/60mm；Length is 2000mm.
Concrete preparation method is as follows：
（1）The preparation of raw material niobium ingot：Using vacuum electron beam stove, vacuum is 10-3Pa, through secondary
Melting, the niobium ingot purity for obtaining are 99.98% or so.
（2）Once machine：Raw material niobium ingot is machined into into the cylindrical ingot blank containing endoporus, its ingot blank by extruding requirement
Cylindrical/diameter of bore be 120/50mm, length is 600mm；
（3）Heating：By all surface of the niobium ingot of the cylinder with endoporus after once machining（Containing bore area）Apply
Antioxidant coating is covered, is then placed in heating furnace, 2 hours are incubated at 900 DEG C；
（4）Expand endoporus：The niobium ingot for completing heating stepses is put in staving press carries out reaming, and the diameter for expanding endoporus is arrived
65mm；
（5）Extrusion molding：The niobium ingot for completing expansion endoporus is melted down again and is placed again into heating furnace（Mode of heating is resistance
Heating）In, being extruded in being put into extruder after being incubated 0.5 hour at 900 DEG C, deflection is 75%, and the niobium obtained after extruding is waste
Cylindrical/the diameter of bore of pipe is 78/55mm.
（6）Heat treatment：The niobium hollow forging for having extruded is put in the annealing furnace of vacuum atmosphere, vacuum is 10-3Pa, 900
DEG C insulation 3 hours, then furnace cooling；
（7）Secondary mechanical is processed：Niobium hollow forging through heat treatment is machined to the production tube of given size.
The production tube even tissue that the present embodiment is obtained, crystal grain are tiny, and its performance is shown in Table 1 with cost.
Embodiment 3
Niobium pipe target finished product manufactured in the present embodiment（I.e. hollow cylindrical target）Specification be：Cylindrical/diameter of bore
For 235/200mm；Length is 4000mm.
Concrete preparation method is as follows：
（1）The preparation of raw material niobium ingot：Using vacuum electron beam stove, vacuum is 10-3Pa, through secondary
Melting, the purity of niobium ingot is 99.98% or so.
（2）Once machine：Raw material niobium ingot is machined into into the cylindrical ingot blank containing endoporus, its ingot blank by extruding requirement
Cylindrical/diameter of bore be 350/55mm, length is 700；
（3）Heating：By all surface of the niobium ingot of the cylinder with endoporus after once machining（Containing bore area）Apply
Antioxidant coating is covered, is then placed in heating furnace, 1 hour is incubated at 1100 DEG C；
（4）Expand endoporus：The niobium ingot for completing heating stepses is put in staving press carries out reaming, and the diameter for expanding endoporus is arrived
206mm；
（5）Extrusion molding：The niobium ingot for completing expansion endoporus is melted down again and is placed again into heating furnace（Mode of heating is resistance
Heating）In, being extruded in being put into extruder after being incubated 0.3 hour at 1100 DEG C, deflection is 84%%, the niobium obtained after extruding
Cylindrical/the diameter of bore of hollow forging is 240/195mm.
（6）Heat treatment：The niobium hollow forging for having extruded is put in the annealing furnace of vacuum atmosphere, vacuum is 10-3Pa, 1100
DEG C insulation 2 hours, then furnace cooling；
（7）Secondary mechanical is processed：Niobium hollow forging through heat treatment is machined to the production tube of given size.
The production tube even tissue that the present embodiment is obtained, crystal grain are tiny, and its performance is shown in Table 1 with cost.
In order to further illustrate advantages of the present invention, two comparative examples are as follows.
Comparative example 1
The specification of niobium pipe target prepared by the comparative example is：Cylindrical/diameter of bore is 155/115mm；Length is 1000mm.
Preparation method is as follows：
（1）The preparation of raw material niobium ingot：It is same as Example 1；
（2）Forging：Forging temperature is 1100 DEG C, and final forging temperature is not less than 900 DEG C, using 3 tons
Pneumatic hammer is forged.
（3）Machining makes finished product.
The performance and cost of the production tube that the comparative example is obtained is shown in Table 1.Cylindrical/endoporus is manufactured using the method for this comparative example
The niobium pipe target of a diameter of 155/115mm, its length are only capable of reaching 1000mm.
Comparative example 2
The specification of niobium pipe target prepared by the comparative example is：Cylindrical/diameter of bore is 148/96mm；Length is 2200mm.
Method of the preparation method described in the embodiment 5 of the patent application of publication number CN102489951A.
The performance of the production tube that the comparative example is obtained is shown in Table 1.The method of this comparative example is adopted to manufacture diameter of bore for 96mm
Niobium pipe target, need to draw out the core of diameter 100mm, and embodiment 1 prepare the niobium pipe target that diameter of bore is 115mm, only
The core of diameter 50mm, and pickling-free step of the present invention need to be removed, institute's low cost in the process of the present invention, stock utilization are high,
It is pollution-free.
The performance and cost statement of 1 embodiment of the present invention of table and comparative example product
Mean grain size is by GB/T6394-2002（Mean grain size is graded（Resection））Calculate.
It should be appreciated that the purposes of these embodiments is merely to illustrate the present invention and is not intended to limit the protection model of the present invention
Enclose.Additionally, it will also be appreciated that after the technology contents for having read the present invention, those skilled in the art can make each to the present invention
Plant and change, change and/or modification, all these equivalent form of value equally falls within the guarantor limited by the application appended claims
Within the scope of shield.
Claims (7)
1. a kind of manufacture method of niobium pipe target, it is characterised in that with niobium ingot as raw material, is walked including one-time mechanical processing successively
Suddenly, heating stepses, expansion endoporus step, pressing steps, heat treatment step and secondary mechanical are processed into finished product step, wherein：
In the one-time mechanical procedure of processing, by extruding requirement by Raw material processing into the cylindrical ingot blank containing endoporus；
In the heating stepses, in the surface of ingot blank coating antioxidant coating Jing after one-time mechanical processing, then in 900～
1350 DEG C are incubated 0.5～2 hour；
In the pressing steps, the ingot blank of endoporus is expanded and has been extruded after 0.1～0.5 hour in 900～1350 DEG C of insulations
Molding, deflection are not less than 70%；
In the heat treatment step, by the niobium hollow forging after extrusion molding in a vacuum or inert atmosphere, at 1100～1350 DEG C
0.5～3 hour is incubated, then furnace cooling.
2. manufacture method according to claim 1, it is characterised in that in the one-time mechanical procedure of processing, the ingot
The length of base is not more than 1100mm, and diameter of bore is 50～60mm.
3. manufacture method according to claim 2, it is characterised in that the diameter of bore is 55～60mm.
4. manufacture method according to claim 1, it is characterised in that it is in the heating stepses and the pressing steps plus
Hot mode is resistance heating or sensing heating.
5. manufacture method according to claim 1, it is characterised in that in the pressing steps, the deflection is
75%-85%.
6. manufacture method according to claim 1, it is characterised in that the raw material niobium ingot is obtained using vacuum smelting method
.
7. manufacture method according to claim 1, it is characterised in that the diameter of bore ratio for expanding ingot blank before and after endoporus is 1：2
～4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310596413.6A CN104651787B (en) | 2013-11-21 | 2013-11-21 | Manufacturing method for niobium tube target material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310596413.6A CN104651787B (en) | 2013-11-21 | 2013-11-21 | Manufacturing method for niobium tube target material |
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| Publication Number | Publication Date |
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| CN104651787A CN104651787A (en) | 2015-05-27 |
| CN104651787B true CN104651787B (en) | 2017-04-19 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109652778A (en) * | 2019-01-28 | 2019-04-19 | 西北有色金属研究院 | A kind of preparation method of the big specification fine grain niobium pipe target of plated film |
| CN109664078A (en) * | 2019-01-28 | 2019-04-23 | 西北有色金属研究院 | A kind of preparation method of the big specification niobium pipe target of fine grain |
| CN111744984A (en) * | 2020-06-18 | 2020-10-09 | 宁夏东方钽业股份有限公司 | Preparation method of tantalum alloy and niobium alloy tube blank |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| AT8697U1 (en) * | 2005-10-14 | 2006-11-15 | Plansee Se | TUBE TARGET |
| 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 |
| CN102974635B (en) * | 2012-12-12 | 2015-08-05 | 山西太钢不锈钢股份有限公司 | The pressing method of molybdenum alloy seamless pipe |
| CN103009000B (en) * | 2012-12-18 | 2015-05-27 | 宁夏东方钽业股份有限公司 | Niobium target and preparation method of niobium target |
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