CN103861982A - Forging method of Nb (Niobium) rotary target cast ingot - Google Patents
Forging method of Nb (Niobium) rotary target cast ingot Download PDFInfo
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Abstract
The invention provides a forging method of an Nb (Niobium) rotary target cast ingot. The method comprises the steps of preheating the Nb cast ingot at the first time, and coating a first antioxidant coating on the surface of the preheated Nb cast ingot; thermally forging the Nb cast ingot at the first time after the Nb cast ingot is coated with the first antioxidant coating, and thermally processing the Nb cast ingot at the first time after the first thermally forging; thermally forging the Nb cast ingot at the second time after the first thermally processing, and thermally processing the Nb cast ingot at the second time after the Nb cast ingot is thermally processed at the second time. On the one hand, the Nb cast ingot can be processed by mainly adopting a forging way, so that columnar zones in the middle and core of the cast ingot are fully crushed, and the non-uniformity of casting state tissues of the Nb cast ingot can be improved; on the other hand, the bad tissues, such as Nb cast ingot forging state dendritic crystals, crystal zones, non-isometric crystal and coarse-grain can be eliminated, so that the grain structures inside the Nb ingot can be fully thinned; and finally the Nb blank for the Nb rotary target with uniform inner grains can be finally obtained.
Description
Technical field
The present invention relates to target production technical field, relate in particular to a kind of forging method of niobium rotary target material ingot casting.
Background technology
Target is the material that is used as negative electrode in sputter-deposition technology, and this material can be redeposited at anode surface with the form disengaging negative electrode of molecule, atom or ion under positively charged cation clashes into.Target is as a kind of extraordinary electronic material with high added value, and it is widely used in the thin-film material of sputter sophisticated technology.According to application, target mainly comprises target for semiconductor applications, target for recording medium, show target, advanced touch screen and display, optics target and superconducting target etc. for film.
Magnetron sputtering is one of major technique of preparing thin-film material, it utilizes ion gun to produce ion, the ion producing is assembled through accelerating in vacuum environment, thereby form the ion beam current of energy at a high speed, the bombardment surface of solids, the exchange of ion and surface of solids atom generation kinetic energy, makes the atom of the surface of solids leave the surface of solids and be deposited on matrix surface.The solid being bombarded is with the raw material of sputtering method deposit film, is called sputtering target material.
The shape of sputtering target material has cuboid, square, cylinder and irregularly shaped.Cuboid, square and cylindrical shape target are solid, in sputter procedure, round ring magnet is set up toroidal magnetic field at target material surface, on the equidistant annular surface of between centers, form etched area, its shortcoming is that thin film deposition thickness evenness is wayward, the utilization rate of target is lower, is only 20% ~ 30%.All applying rotation hollow circular-tube magnetic controlled sputtering target both at home and abroad at present, its advantage is that this hollow circular-tube target can rotate around fixing bar magnet assembly, thereby 360 ° of target surfaces can be by even etching, and utilization rate is up to 80%.In general, the crystallite dimension of sputtering target material must be controlled at below 100 microns, and even the taxis of its crystalline texture also must be subject to strict control.
Niobium rotary target material is as the important source material of preparing niobium and alloy film material thereof, in the corrosive environments such as the photoelectric fields such as liquid crystal flat panel display, optical lens, electronic imaging, information storage, solar cell and coating film on glass and boats and ships, chemical industry, has a wide range of applications.Niobium rotary target material requires the whole axial direction homogeneous grain size of product consistent, crystallite dimension 50 ~ 100 μ m, and therefore researcher conducts in-depth research the production method of niobium target.For example: publication number is the preparation method that the Chinese patent of CN 102489951A discloses a kind of niobium tubular target materials for sputtering, and the method comprises the following steps: prepare niobium pipe; Adopt steel capsule by closely coated to inside and outside niobium pipe wall and two, welded seal, then carries out hot extrusion, obtains niobium pipe target; Niobium pipe target is carried out to pickling and heat treatment, obtain niobium tubular target.Said method just adopts the method for hot extrusion to process niobium pipe, thereby cannot ensure the inner grain structure uniformity of niobium rotary target material.
Summary of the invention
The technical problem that the present invention solves is to provide the forging method of the uniform niobium rotary target material of a kind of inner grain structure ingot casting.
In view of this, the invention provides a kind of forging method of niobium rotary target material ingot casting, comprise the following steps:
By the preheating for the first time of niobium ingot casting, the niobium ingot casting surface after preheating applies the first ORC;
The niobium ingot casting applying after the first ORC is carried out to forge hot for the first time, the niobium ingot casting after forge hot is for the first time carried out to heat treatment for the first time;
Niobium ingot casting after heat treatment is for the first time carried out to forge hot for the second time, the niobium ingot casting after forge hot is for the second time carried out to heat treatment for the second time.
Preferably, the temperature of described preheating is for the first time 150 DEG C ~ 250 DEG C.
Preferably, described the first ORC is glass dust, and the thickness of described ORC is 1mm ~ 1.5mm.
Preferably, the step that applies niobium ingot casting after the first ORC and carry out forge hot is for the first time specially:
The niobium ingot casting that applies the first ORC is heated to 365 DEG C ~ 472 DEG C for the first time, be incubated for the first time 2h ~ 4.5h, niobium ingot casting after insulation is carried out to jumping-up and for the first time pulling for the first time, and the general working rate of described jumping-up for the first time and pulling is for the first time 40% ~ 65%.
Preferably, after described forge hot for the first time with before described heat treatment for the first time, also comprise:
Niobium ingot casting after forge hot is for the first time carried out to pickling for the first time.
Preferably, the acid solution of described pickling is for the first time the mixed solution of hydrochloric acid, hydrofluoric acid and sulfuric acid, and the time of described pickling is 5min ~ 10min.
Preferably, described the first heat treated temperature is 930 DEG C ~ 1300 DEG C, and the described heat treated time is for the first time 60min ~ 100min.
Preferably, after described heat treatment for the first time with before described forge hot for the second time, also comprise:
Niobium ingot casting after heat treatment is for the first time carried out to preheating for the second time, and the niobium ingot casting surface after preheating for the second time applies the second ORC.
Preferably, after described forge hot for the second time with before described heat treatment for the second time, also comprise:
Niobium ingot casting after forge hot is for the second time carried out to pickling for the second time.
The step of preferably, the niobium ingot casting after heat treatment for the first time being carried out to forge hot is for the second time specially:
Niobium ingot casting after heat treatment is for the first time heated to 365 DEG C ~ 472 DEG C for the second time, is incubated for the second time 2h ~ 4.5h, the niobium ingot casting after insulation is for the second time carried out to jumping-up and for the second time pulling for the second time, the working modulus of described jumping-up is for the second time 35% ~ 50%.
The forging method that the invention provides a kind of niobium rotary target material ingot casting, first carries out preheating by niobium ingot casting, and the niobium ingot casting surface after preheating applies ORC; Then carry out for the first time warm and hot forging and heat-treat, thereby obtaining the niobium ingot casting of the preliminary refinement of crystal grain; Then carry out forge hot for the second time, thereby thoroughly smash inner grain structure, obtain the niobium ingot casting of grain refinement, finally again heat-treat, to eliminate the internal stress in forging process and to impel the recrystallization again of organizing after forging, thereby obtain the niobium rotary target material niobium base of uniform crystal particles refinement.In niobium rotary target material ingot casting production process, the present invention mainly adopts the mode of forging, makes the columnar zone of ingot casting middle part and heart portion obtain abundant fragmentation, thereby improves the degree of irregularity of niobium ingot casting casting state tissue; On the other hand, by twice forging, eliminate the existence of the harmful structure such as dendrite, crystal zone, non-equiax crystal and coarse-grain of niobium ingot casting casting state, made the inside grain structure of niobium ingot casting obtain abundant refinement, finally obtained the niobium rotary target material niobium base of inner uniform crystal particles refinement.
Detailed description of the invention
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The forging method that the embodiment of the invention discloses a kind of niobium rotary target material ingot casting, comprises the following steps:
By the preheating for the first time of niobium ingot casting, the niobium ingot casting surface after preheating applies the first ORC;
The niobium ingot casting applying after the first ORC is carried out to forge hot for the first time, the niobium ingot casting after forge hot is for the first time carried out to heat treatment for the first time;
Niobium ingot casting after heat treatment is for the first time carried out to forge hot for the second time, the niobium ingot casting after forge hot is for the second time carried out to heat treatment for the second time.
According to the present invention, for the processing method of niobium ingot casting, first by niobium ingot casting preheating, the niobium ingot casting surface after preheating applies ORC, to prevent the suction hydrogen oxygen uptake of niobium ingot casting; Then niobium ingot casting is carried out to forge hot for the first time, by the fragmentation of niobium ingot casting crystal grain interior tissue, after forge hot, heat-treat for the first time, obtain the niobium ingot casting of the preliminary refinement of crystal grain; Carry out subsequently forge hot for the second time, niobium inside ingot crystal grain is fully broken, thus guarantee niobium inside ingot is organized the uniformity of crystal grain, again heat-treats, thereby obtains the tiny niobium base of uniform crystal particles.
First the present invention carries out preheating by niobium ingot casting, and preheating is conducive to ORC and the niobium ingot casting surface bonding on niobium ingot casting surface.The temperature of described preheating is preferably 150 ~ 250 DEG C, more preferably 175 ~ 225 DEG C, most preferably is 200 DEG C.In order to prevent the suction hydrogen oxygen uptake of niobium ingot casting in hot forging process, will after niobium ingot casting preheating, apply ORC on niobium ingot casting surface.The thickness of described ORC is preferably 1 ~ 1.5mm, to ensure that ORC can apply evenly on niobium ingot casting surface.
Niobium ingot casting surface is applied after ORC, niobium ingot casting is carried out to forge hot for the first time.According to the present invention, in order to improve the plasticity in niobium ingot casting forging process, ensure the saturating property of forging of niobium ingot casting and the adequacy of crystal grain fragmentation, the present invention has selected the forging mode of forge hot.The concrete steps of described forge hot are for the first time: the niobium ingot casting that applies ORC is heated to 365 ~ 472 DEG C, after insulation 2 ~ 4.5h, niobium ingot casting is carried out for the first time to axially jumping-up and for the first time axially forging of pulling, the general working rate of forging is 40% ~ 65%.Well known to those skilled in the art, ingot casting is to adopt electron beam furnace melting, and the direction of melting is axial, i.e. ingot casting length direction, and prolonging in axial fusion process is the direction that produces coarse-grain, dendrite and crystal zone, this direction is also the good direction of plasticity.And the axial jumping-up processing tissue such as coarse-grain, dendrite of broken casting state in the axial direction makes grain refinement, axially jumping-up and axial pulling niobium ingot casting are easily out of shape simultaneously, not easy to crack.
After warm and hot forging completes for the first time, impact for fear of the vaporization of ORC in follow-up heat treatment process on niobium ingot surface quality, the present invention preferably carries out pickling by the niobium ingot casting after heat treatment for the first time, so that the ORC on niobium ingot casting surface is removed.The acid solution of described pickling is preferably the mixed solution of hydrofluoric acid, hydrochloric acid and sulfuric acid.Described hydrofluoric acid is commercially available hydrofluoric acid, its mass fraction is 35.35wt%, described hydrochloric acid is commercially available hydrochloric acid, its concentration is 37%, described sulfuric acid is the commercially available concentrated sulfuric acid, and its concentration is 98%, and the volume ratio of described hydrochloric acid, hydrofluoric acid and sulfuric acid is preferably 5:3:2, the temperature of described acid solution is preferably 55 DEG C ~ 75 DEG C, more preferably 60 ~ 70 DEG C.。Can washes clean for the glass dust that makes niobium ingot casting surface, the time of described pickling is preferably 5 ~ 10min.
In order to eliminate the residualinternal stress of niobium inside ingot in process, the present invention, after forge hot completes for the first time, has carried out heat treatment by niobium ingot casting.In forging process, niobium ingot casting can produce work hardening, if do not heat-treat the difficulty that can increase forge hot for the second time, even can cause processing cracking, simultaneously for the niobium ingot casting after making to forge for the first time obtains recrystallized structure again, coordinate and carry out crystal grain fragmentation again with follow-up forge hot for the second time, the present invention heat-treats the niobium ingot casting after forge hot for the first time.Described heat treated temperature is preferably 930 ~ 1300 DEG C, more preferably 1100 ~ 1200 DEG C; The described heat treated time is preferably 60 ~ 100min, more preferably 80 ~ 90min.
According to the present invention, niobium ingot casting carries out after heat treatment for the first time, the niobium ingot casting after heat treatment is carried out to forge hot for the second time.As only adopted once axially jumping-up just to finish forging process with axial pulling, not high to the degree of grain refinement of niobium ingot casting, do not reach final tissue effect, therefore, the present invention has carried out forge hot for the second time.The present invention carries out the sufficient broken niobium inside ingot grain structure again of forge hot for the second time, reaches the effect of crystal grain thinning.Described concrete steps of forging are for the second time: the niobium ingot casting after heat treatment is for the first time heated to 365 ~ 472 DEG C for the second time, be incubated for the second time 2 ~ 4.5h, niobium ingot casting after insulation is for the second time carried out to jumping-up and for the second time pulling for the second time, and the working modulus of described jumping-up is for the second time 35% ~ 50%.For the number of times forging can also be three times four times even more times, the not special restriction of the present invention, but for the consideration of cost and efficiency, the present invention has preferably carried out twice forging.
In order to prevent that niobium ingot casting from inhaling hydrogen oxygen uptake in forging process, as preferred version, before described forge hot for the second time, also comprise: the niobium ingot casting after heat treatment is for the first time carried out to preheating for the second time, and the niobium ingot casting surface after preheating for the second time applies the second ORC.The temperature of described preheating is for the second time preferably 150 ~ 250 DEG C, more preferably 180 ~ 230 DEG C, most preferably is 200 DEG C.
According to the present invention, after warm and hot forging completes for the second time, in order to eliminate the residual stress in forging process, make the interior tissue of niobium ingot casting evenly tiny, the niobium ingot casting after forge hot is for the second time carried out to heat treatment for the second time.Described heat treated temperature is for the second time preferably 930 ~ 1300 DEG C, more preferably 1000 ~ 1200 DEG C; The described heat treated time is for the second time preferably 60 ~ 100min, more preferably 80 ~ 90min.
The forging method that the invention provides a kind of niobium rotary target material ingot casting, first carries out preheating by niobium ingot casting, and the niobium ingot casting surface after preheating applies ORC; Then carry out for the first time warm and hot forging and heat-treat, thereby obtaining the niobium ingot casting of the preliminary refinement of crystal grain; Then carry out forge hot for the second time, thereby thoroughly smash inner grain structure, obtain the niobium ingot casting of grain refinement, finally again heat-treat, to eliminate the internal stress in forging process, thereby obtain the niobium ingot casting after the forging of uniform crystal particles refinement, the niobium base using the niobium ingot casting obtaining before extrusion process, is conducive to obtain the niobium target of uniform crystal particles refinement.The present invention mainly adopts the mode of forging, makes the columnar zone of ingot casting middle part and heart portion obtain abundant fragmentation, thereby improves the degree of irregularity of niobium ingot casting casting state tissue; On the other hand, by twice forging, eliminate the existence of the harmful structure such as dendrite, crystal zone, non-equiax crystal and coarse-grain of niobium ingot casting casting state, made the inside grain structure of niobium ingot casting obtain abundant refinement, finally obtained the niobium rotary target material niobium base of inner uniform crystal particles refinement.
In order further to understand the present invention, below in conjunction with embodiment, the forging method of niobium ingot casting provided by the invention is elaborated, protection scope of the present invention is not limited by the following examples.
Embodiment 1
1) melting diameter is that 190mm, length are 350mm, the niobium ingot that chemical composition is Nb >=99.95%, twice of electronic torch melting;
2) 200 DEG C of niobium ingot preheatings step 1) being obtained, smear glass dust, 400 DEG C of ingot heating, and insulation 3h, carries out axial jumping-up to 200mm to niobium ingot, and pulling is to 200 × 200 × 245mm;
3) by step 2) the niobium ingot that obtains carries out pickling: HCl:HF:H
2sO
4=5:3:2(volume ratio), pickling time 10min, removes surface impurity and glass dust, visually observes visible niobium metal gloss without assorted spot;
4) niobium ingot step 3) being obtained is heat-treated: heat treatment temperature is 1000 DEG C, and temperature retention time is 60min;
5) niobium ingot step 4) being obtained is preheated to 200 DEG C, smears 1.5mm glass dust;
6) niobium ingot jumping-up step 5) being obtained, to 160mm, forges the side of beating 190 × 190mm, finally forges and beats circle to Φ 200mm;
7) the niobium ingot obtaining in step 6) is carried out to pickling HCl:HF:H
2sO
4=5:3:2(volume ratio), pickling time 10 minutes, removes surface impurity and glass dust, visually observes visible niobium metal gloss and heat-treats after without assorted spot, and heat treated temperature is 1000 DEG C, and temperature retention time is 60min, obtains niobium sputtering target niobium base.
Embodiment 2
1) melting diameter is 290mm, length 650mm, the niobium ingot that chemical composition is Nb >=99.95%, electronic torch melting 2 times;
2) by step 2) 220 DEG C of the niobium ingot preheatings that obtain, smear glass dust, 380 DEG C of ingot heating, insulation 2h.Niobium ingot is carried out to axial jumping-up to 380mm, and pulling is to 290 × 290 × 510mm;
3) by step 2) the niobium ingot that obtains carries out pickling: HCl:HF:H
2sO
4=5:3:2(volume ratio), pickling time 8min, removes surface impurity and glass dust, visually observes visible niobium metal gloss without assorted spot;
4) niobium ingot step 3) being obtained is heat-treated: heat treatment temperature is 950 DEG C, and temperature retention time is 80min;
5) niobium ingot step 4) being obtained carries out jumping-up to 350mm, forges the side of beating 250 × 250mm, finally forges and beats circle to Φ 265mm;
6) niobium ingot step 5) being obtained is heat-treated, and temperature is 1000 DEG C, and temperature retention time is 100min, obtains niobium sputtering target niobium base.Embodiment 3
1) melting diameter is 480mm, length 500mm, the niobium ingot that chemical composition is Nb >=99.95%, electronic torch melting 2 times;
2) 250 DEG C of niobium ingot preheatings step 1) being obtained, smear glass dust, 450 DEG C of ingot heating, insulation 4.5h.Niobium ingot is carried out to axial jumping-up to 300mm, and pulling is to 480 × 480 × 390mm;
3) by step 2) the niobium ingot that obtains carries out pickling: HCl:HF:H
2sO
4=5:3:2(volume ratio), pickling time 10min, removes surface impurity and glass dust, visually observes visible niobium metal gloss without assorted spot;
4) niobium ingot step 3) being obtained is heat-treated: heat treatment temperature is 1200 DEG C, and temperature retention time is 100min;
5) niobium ingot step 4) being obtained is preheated to 230 DEG C, smears 1mm glass dust;
6) niobium ingot step 5) being obtained carries out jumping-up to 270mm, forges the side of beating 290 × 290mm, finally forges and beats circle to Φ 300mm;
7) niobium ingot step 6) being obtained carries out pickling HCl:HF:H
2sO
4=5:3:2(volume ratio), pickling time 10 minutes, removes surface impurity and glass dust, visually observes visible niobium metal gloss and heat-treats after without assorted spot, and heat treated temperature is 1200 DEG C, and temperature retention time is 100min, obtains niobium sputtering target niobium base.
The explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, make professional and technical personnel in the field can realize or use the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiment, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a forging method for niobium rotary target material ingot casting, comprises the following steps:
By the preheating for the first time of niobium ingot casting, the niobium ingot casting surface after preheating applies the first ORC;
The niobium ingot casting applying after the first ORC is carried out to forge hot for the first time, the niobium ingot casting after forge hot is for the first time carried out to heat treatment for the first time;
Niobium ingot casting after heat treatment is for the first time carried out to forge hot for the second time, the niobium ingot casting after forge hot is for the second time carried out to heat treatment for the second time.
2. forging method according to claim 1, is characterized in that, the temperature of described preheating is for the first time 150 DEG C ~ 250 DEG C.
3. forging method according to claim 1, is characterized in that, described the first ORC is glass dust, and the thickness of described ORC is 1mm ~ 1.5mm.
4. forging method according to claim 1, is characterized in that, the step of the niobium ingot casting after coating the first ORC being carried out to forge hot is for the first time specially:
The niobium ingot casting that applies the first ORC is heated to 365 DEG C ~ 472 DEG C for the first time, is incubated for the first time 2h ~ 4.5h, the niobium ingot casting after insulation is carried out to jumping-up and for the first time pulling for the first time, the general working rate of jumping-up and pulling is for the first time 40% ~ 65% for the first time.
5. forging method according to claim 1, is characterized in that, after described forge hot for the first time with before described heat treatment for the first time, also comprises:
Niobium ingot casting after forge hot is for the first time carried out to pickling for the first time.
6. forging method according to claim 5, is characterized in that, the acid solution of described pickling is for the first time the mixed solution of hydrochloric acid, hydrofluoric acid and sulfuric acid, and the time of described pickling is 5min ~ 10min.
7. forging method according to claim 1, is characterized in that, described the first heat treated temperature is 930 DEG C ~ 1300 DEG C, and the described heat treated time is for the first time 60min ~ 100min.
8. forging method according to claim 1, is characterized in that, after described heat treatment for the first time with before described forge hot for the second time, also comprises:
Niobium ingot casting after heat treatment is for the first time carried out to preheating for the second time, and the niobium ingot casting surface after preheating for the second time applies the second ORC.
9. forging method according to claim 8, is characterized in that, after described forge hot for the second time with before described heat treatment for the second time, also comprises:
Niobium ingot casting after forge hot is for the second time carried out to pickling for the second time.
10. according to the forging method described in claim 1 or 9, it is characterized in that, the step of the niobium ingot casting after heat treatment for the first time being carried out to forge hot is for the second time specially:
Niobium ingot casting after heat treatment is for the first time heated to 365 DEG C ~ 472 DEG C for the second time, is incubated for the second time 2h ~ 4.5h, the niobium ingot casting after insulation is for the second time carried out to jumping-up and for the second time pulling for the second time, the working modulus of described jumping-up is for the second time 35% ~ 50%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104593708A (en) * | 2015-01-16 | 2015-05-06 | 宁夏东方钽业股份有限公司 | Preparation method of planar niobium target |
| CN106378591A (en) * | 2016-11-28 | 2017-02-08 | 西安诺博尔稀贵金属材料有限公司 | Processing method for small-size and high-strength niobium-hafnium alloy bar |
| CN112548495A (en) * | 2020-11-26 | 2021-03-26 | 西北有色金属研究院 | Forging method of plate blank for superconducting wire barrier layer niobium sheet |
| CN113523012A (en) * | 2021-07-14 | 2021-10-22 | 山西太钢不锈钢股份有限公司 | Hot processing method of niobium-containing high-alloy austenitic heat-resistant stainless steel bar |
| CN113718110A (en) * | 2021-08-11 | 2021-11-30 | 九江有色金属冶炼有限公司 | Preparation method of high-quality niobium plate for controlling plate structure by accumulated energy |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002070765A1 (en) * | 2001-02-20 | 2002-09-12 | H. C. Starck, Inc. | Refractory metal plates with uniform texture and methods of making the same |
| CN101660130A (en) * | 2009-09-29 | 2010-03-03 | 西部金属材料股份有限公司 | Method for preparing niobium sputtering target |
| CN102699247A (en) * | 2012-05-18 | 2012-10-03 | 宁夏东方钽业股份有限公司 | Forging method for superconducting tantalum bar |
| 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 |
-
2012
- 2012-12-18 CN CN201210551252.4A patent/CN103861982B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002070765A1 (en) * | 2001-02-20 | 2002-09-12 | H. C. Starck, Inc. | Refractory metal plates with uniform texture and methods of making the same |
| CN101660130A (en) * | 2009-09-29 | 2010-03-03 | 西部金属材料股份有限公司 | Method for preparing niobium sputtering target |
| CN102699247A (en) * | 2012-05-18 | 2012-10-03 | 宁夏东方钽业股份有限公司 | Forging method for superconducting tantalum bar |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 李兆博等: "溅射镀膜用铌靶材晶粒尺寸控制工艺研究", 《材料开发与应用》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104593708A (en) * | 2015-01-16 | 2015-05-06 | 宁夏东方钽业股份有限公司 | Preparation method of planar niobium target |
| CN106378591A (en) * | 2016-11-28 | 2017-02-08 | 西安诺博尔稀贵金属材料有限公司 | Processing method for small-size and high-strength niobium-hafnium alloy bar |
| CN112548495A (en) * | 2020-11-26 | 2021-03-26 | 西北有色金属研究院 | Forging method of plate blank for superconducting wire barrier layer niobium sheet |
| CN113523012A (en) * | 2021-07-14 | 2021-10-22 | 山西太钢不锈钢股份有限公司 | Hot processing method of niobium-containing high-alloy austenitic heat-resistant stainless steel bar |
| CN113718110A (en) * | 2021-08-11 | 2021-11-30 | 九江有色金属冶炼有限公司 | Preparation method of high-quality niobium plate for controlling plate structure by accumulated energy |
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