CN103861982B - A kind of forging method of niobium rotary target material ingot casting - Google Patents
A kind of forging method of niobium rotary target material ingot casting Download PDFInfo
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Abstract
The invention provides the forging method of a kind of niobium rotary target material ingot casting, comprise the following steps: by the first time preheating of niobium ingot casting, niobium ingot casting surface-coated the first ORC after preheat; Niobium ingot casting after being coated with the first ORC is carried out first time forge hot, the niobium ingot casting after first time forge hot is carried out first time heat treatment; Niobium ingot casting after first time heat treatment is carried out second time forge hot, the niobium ingot casting after second time forge hot is carried out second time heat treatment. The present invention mainly adopts the mode of forging that niobium ingot casting is processed so that in the middle part of ingot casting and the columnar zone in heart portion fully crushed, thus improving the degree of irregularity of the casting state tissue of niobium ingot casting; On the other hand, by twice forging, eliminate the existence of the harmful structures such as the niobium ingot casting casting dendrite of state, crystal zone, non-equiax crystal and coarse-grain, make the internal grain tissue of niobium ingot casting fully be refined, finally given internal grain uniform niobium rotary target material niobium base.
Description
Technical field
The present invention relates to target production technical field, particularly relate to the forging method of a kind of niobium rotary target material ingot casting.
Background technology
Target is the material being 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 is clashed 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 sputtering sophisticated technology. According to application, target mainly includes semiconductor applications target, record medium target, display thin film target, advanced touch screen and display, optics target and superconducting target etc.
Magnetron sputtering is one of major technique preparing thin-film material, it utilizes ion source to produce ion, the ion produced is assembled through acceleration in vacuum environment, thus forming the ion beam current of energy at 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 bombarded is the raw material depositing thin film with sputtering method, 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 sets up toroidal magnetic field at target material surface, the equidistant annular surface of between centers is formed etched area, its shortcoming is that thin film deposition thickness evenness is wayward, the utilization rate of target is relatively low, is only 20% ~ 30%. All rotating hollow circular-tube magnetic controlled sputtering target in popularization and application both at home and abroad at present, its advantage is that this hollow circular-tube target can rotate around fixing bar magnet assembly, thus 360 ° of target surfaces can uniformly be etched, and utilization rate is up to 80%.In general, the crystallite dimension of sputtering target material must control below 100 microns, and even the tropism of its crystalline texture also must be under strict control.
Niobium rotary target material, as the important source material preparing niobium and alloy film material thereof, has a wide range of applications in the photoelectric fields such as liquid crystal flat panel display, optical lens, electronic imaging, information storage, solaode and coating film on glass and the corrosive environment such as boats and ships, chemical industry. Niobium rotary target material requires that the whole axial direction homogeneous grain size of product is consistent, and crystallite dimension 50 ~ 100 μm, therefore the production method of niobium target is conducted in-depth research by researcher. Such as: publication number is the preparation method that the Chinese patent of CN102489951A discloses a kind of niobium tubular target materials for sputtering, and the method comprises the following steps: prepare niobium pipe; Steel capsule is adopted inside and outside for niobium pipe wall and two to be closely coated with, welded seal, then carry out hot extrusion, obtain niobium pipe target; Niobium pipe target is carried out pickling and heat treatment, namely obtains niobium tubular target. Said method simply adopts the method for hot extrusion that niobium pipe is processed, thus niobium rotary target material internal grain structural homogenity cannot be ensured.
Summary of the invention
Present invention solves the technical problem that the forging method of the niobium rotary target material ingot casting being in that to provide a kind of internal grain even tissue.
In view of this, the invention provides the forging method of a kind of niobium rotary target material ingot casting, comprise the following steps:
By the first time preheating of niobium ingot casting, niobium ingot casting surface-coated the first ORC after preheat;
Niobium ingot casting after being coated with the first ORC is carried out first time forge hot, the niobium ingot casting after first time forge hot is carried out first time heat treatment;
Niobium ingot casting after first time heat treatment is carried out second time forge hot, the niobium ingot casting after second time forge hot is carried out second time heat treatment.
Preferably, the temperature of preheating of described first time is 150 DEG C ~ 250 DEG C.
Preferably, described first ORC is glass dust, and the thickness of described ORC is 1mm ~ 1.5mm.
Preferably, the niobium ingot casting after being coated with the first ORC is carried out the step of first time forge hot particularly as follows:
The niobium ingot casting first time being coated with the first ORC is heated to 365 DEG C ~ 472 DEG C, first time is incubated 2h ~ 4.5h, niobium ingot casting after insulation carries out first time jumping-up and first time pulling, and the general working rate of described first time jumping-up and first time pulling is 40% ~ 65%.
Preferably, also include with before described first time heat treatment after described first time forge hot:
Niobium ingot casting after first time forge hot is carried out first time pickling.
Preferably, the mixed solution that acid solution is hydrochloric acid, Fluohydric acid. and sulphuric acid of described first time pickling, the time of described pickling is 5min ~ 10min.
Preferably, described first heat treated temperature is 930 DEG C ~ 1300 DEG C, and the described first time heat treated time is 60min ~ 100min.
Preferably, also include with before described second time forge hot after described first time heat treatment:
Niobium ingot casting after first time heat treatment is carried out second time preheating, niobium ingot casting surface-coated the second ORC after second time preheating.
Preferably, also include with before described second time heat treatment after described second time forge hot:
Niobium ingot casting after second time forge hot is carried out second time pickling.
Preferably, the niobium ingot casting after first time heat treatment is carried out second time forge hot step particularly as follows:
By the niobium ingot casting second time heating after first time heat treatment to 365 DEG C ~ 472 DEG C, second time is incubated 2h ~ 4.5h, and the niobium ingot casting after second time insulation carries out second time jumping-up and second time pulling, and the working modulus of described second time jumping-up is 35% ~ 50%.
The invention provides the forging method of a kind of niobium rotary target material ingot casting, first niobium ingot casting is preheated, niobium ingot casting surface-coated ORC after preheat; Then carry out first time warm and hot forging and carry out heat treatment, thus obtaining the niobium ingot casting that crystal grain tentatively refines; Then second time forge hot is carried out, thus thoroughly smashing internal grain tissue, obtaining the niobium ingot casting of grain refinement, finally again carrying out heat treatment, with the internal stress eliminated in forging process and promote forging after tissue recrystallization again, thus obtaining the niobium rotary target material niobium base that crystal grain uniformly refines. In niobium rotary target material ingot casting production process, the present invention mainly adopts the mode of forging so that in the middle part of ingot casting and the columnar zone in heart portion fully crushed, thus improve niobium ingot casting casting state tissue degree of irregularity; On the other hand, by twice forging, eliminate the existence of the harmful structures such as the niobium ingot casting casting dendrite of state, crystal zone, non-equiax crystal and coarse-grain, make the internal grain tissue of niobium ingot casting fully be refined, finally given the niobium rotary target material niobium base that internal grain uniformly refines.
Detailed description of the invention
In order to be further appreciated by the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but it is to be understood that these describe simply as further illustrating the features and advantages of the present invention, rather than limiting to the claimed invention.
The embodiment of the invention discloses the forging method of a kind of niobium rotary target material ingot casting, comprise the following steps:
By the first time preheating of niobium ingot casting, niobium ingot casting surface-coated the first ORC after preheat;
Niobium ingot casting after being coated with the first ORC is carried out first time forge hot, the niobium ingot casting after first time forge hot is carried out first time heat treatment;
Niobium ingot casting after first time heat treatment is carried out second time forge hot, the niobium ingot casting after second time forge hot is carried out second time heat treatment.
According to the present invention, for the processing method of niobium ingot casting, first by niobium ingot casting preheating, niobium ingot casting surface-coated ORC after preheat, to prevent the suction hydrogen oxygen uptake of niobium ingot casting; Then niobium ingot casting is carried out first time forge hot, by niobium ingot casting intra-die historrhexis, carries out heat treatment after first time forge hot, obtain the niobium ingot casting that crystal grain tentatively refines; Carrying out second time forge hot subsequently, by fully broken for niobium inside ingot crystal grain, thus ensureing the uniformity of niobium inside ingot tissue crystal grain, again carrying out heat treatment, thus obtaining the niobium base that crystal grain is uniformly tiny.
First niobium ingot casting is preheated by the present invention, 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, it is most preferred that be 200 DEG C. In order to prevent the suction hydrogen oxygen uptake of niobium ingot casting in hot forging process, by after niobium ingot casting preheating then at niobium ingot casting surface-coated ORC. The thickness of described ORC is preferably 1 ~ 1.5mm, to ensure that ORC can be coated with uniformly on niobium ingot casting surface.
After niobium ingot casting surface-coated ORC, then niobium ingot casting is carried out first time forge hot. According to the present invention, in order to improve the plasticity in niobium ingot casting forging process, it is ensured that the adequacy forging saturating property and die break of niobium ingot casting, the present invention have selected the forging mode of forge hot. Concretely comprising the following steps of described first time forge hot: heat the niobium ingot casting of coating ORC to 365 ~ 472 DEG C, after insulation 2 ~ 4.5h, carries out first time axially jumping-up and the forging of first time axially pulling to niobium ingot casting, and 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. extrusion ingot length direction, prolongs in axial fusion process the direction being to produce coarse-grain, dendrite and crystal zone, and the direction is also the good direction of plasticity. And axial jumping-up is processed and can the coarse-grain of broken casting state, dendrite etc. be organized in the axial direction, making grain refinement, axially jumping-up and the axial niobium ingot casting that pulls out are easily deformed simultaneously, not easy to crack.
After in first time, warm and hot forging completes, in order to avoid the vaporization of the ORC impact on niobium ingot surface quality in follow-up heat treatment process, niobium ingot casting after first time heat treatment is preferably carried out pickling by the present invention, to be removed by the ORC on niobium ingot casting surface. The acid solution of described pickling is preferably the mixed solution of Fluohydric acid., hydrochloric acid and sulphuric acid. Described Fluohydric acid. is commercially available Fluohydric acid., its mass fraction is 35.35wt%, described hydrochloric acid is commercially available hydrochloric acid, its concentration is 37%, described sulphuric acid is commercially available concentrated sulphuric acid, and its concentration is 98%, and the volume ratio of described hydrochloric acid, Fluohydric acid. and sulphuric 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. . In order to enable the glass dust washes clean on 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 the course of processing, niobium ingot casting after forge hot completes in first time, has been carried out heat treatment by the present invention. In forging process, niobium ingot casting can produce hardening, if not carrying out heat treatment can increase the difficulty of second time forge hot, even can cause processing cracking, simultaneously in order to the niobium ingot casting after making first time forging obtains recrystallized structure again, coordinating with follow-up second time forge hot and carry out die break again, the niobium ingot casting after first time forge hot is carried out heat treatment by the present invention. 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, after niobium ingot casting carries out first time heat treatment, then the niobium ingot casting after heat treatment is carried out second time forge hot. As just terminated forging process only with once axial jumping-up and axial pulling, then the degree of grain refinement of niobium ingot casting is not high, do not reach final tissue effect, therefore, the present invention has carried out second time forge hot. The present invention carries out second time forge hot can crush niobium inside ingot grain structure again fully, reaches the effect of crystal grain thinning. Concretely comprising the following steps of described second time forging: by the niobium ingot casting second time heating after first time heat treatment to 365 ~ 472 DEG C, second time insulation 2 ~ 4.5h, niobium ingot casting after second time insulation carries out second time jumping-up and second time pulling, and the working modulus of described second time jumping-up is 35% ~ 50%. For the number of times of forging can also is that 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 been preferably performed twice forging.
In order to prevent niobium ingot casting from inhaling hydrogen oxygen uptake in forging process, preferably, also include before described second time forge hot: the niobium ingot casting after first time heat treatment is carried out second time preheating, niobium ingot casting surface-coated the second ORC after second time preheating. The temperature of described second time preheating is preferably 150 ~ 250 DEG C, more preferably 180 ~ 230 DEG C, it is most preferred that be 200 DEG C.
According to the present invention, after second time warm and hot forging completes, in order to eliminate the residual stress in forging process, the interior tissue making niobium ingot casting is uniformly tiny, then the niobium ingot casting after second time forge hot carries out second time heat treatment.The heat treated temperature of described second time is preferably 930 ~ 1300 DEG C, more preferably 1000 ~ 1200 DEG C; The described second time heat treated time is preferably 60 ~ 100min, more preferably 80 ~ 90min.
The invention provides the forging method of a kind of niobium rotary target material ingot casting, first niobium ingot casting is preheated, niobium ingot casting surface-coated ORC after preheat; Then carry out first time warm and hot forging and carry out heat treatment, thus obtaining the niobium ingot casting that crystal grain tentatively refines; Then second time forge hot is carried out, thus thoroughly smashing internal grain tissue, obtain the niobium ingot casting of grain refinement, finally again carry out heat treatment, to eliminate the internal stress in forging process, thus obtaining the niobium ingot casting after the forging that crystal grain uniformly refines, using the niobium ingot casting that obtains as the niobium base before extrusion process, be conducive to obtaining the niobium target that crystal grain uniformly refines. The present invention mainly adopts the mode of forging so that in the middle part of ingot casting and the columnar zone in heart portion fully crushed, thus improve niobium ingot casting casting state tissue degree of irregularity; On the other hand, by twice forging, eliminate the existence of the harmful structures such as the niobium ingot casting casting dendrite of state, crystal zone, non-equiax crystal and coarse-grain, make the internal grain tissue of niobium ingot casting fully be refined, finally given the niobium rotary target material niobium base that internal grain uniformly refines.
In order to be further appreciated by the present invention, below in conjunction with embodiment, the forging method of niobium ingot casting provided by the invention being described in detail, protection scope of the present invention is not limited by the following examples.
Embodiment 1
1) melting diameter is 190mm, length is 350mm, and chemical composition is the niobium ingot of Nb >=99.95%, electronic torch melting twice;
2) niobium ingot step 1) obtained preheats 200 DEG C, smears glass dust, and ingot heats 400 DEG C, is incubated 3h, niobium ingot carries out axial jumping-up to 200mm, pulls out 200 × 200 × 245mm;
3) by step 2) the niobium ingot that obtains carries out pickling: HCl:HF:H2SO4=5:3:2(volume ratio), pickling time 10min, remove surface impurity and glass dust, perusal visible niobium metal gloss is without assorted speckle;
4) niobium ingot step 3) obtained carries out heat treatment: heat treatment temperature is 1000 DEG C, and temperature retention time is 60min;
5) niobium ingot step 4) obtained is preheated to 200 DEG C, smears 1.5mm glass dust;
6) niobium ingot jumping-up step 5) obtained, to 160mm, forges the side of beating 190 × 190mm, and finally forging is beaten circle and arrived Φ 200mm;
7) the niobium ingot obtained in step 6) is carried out pickling HCl:HF:H2SO4=5:3:2(volume ratio), pickling time 10 minutes, remove surface impurity and glass dust, perusal visible niobium metal gloss is without carrying out heat treatment after assorted speckle, 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, and chemical composition is the niobium ingot of Nb >=99.95%, electronic torch melting 2 times;
2) by step 2) the niobium ingot that obtains preheats 220 DEG C, smears glass dust, and ingot heats 380 DEG C, is incubated 2h. Niobium ingot is carried out axial jumping-up to 380mm, pull out 290 × 290 × 510mm;
3) by step 2) the niobium ingot that obtains carries out pickling: HCl:HF:H2SO4=5:3:2(volume ratio), pickling time 8min, remove surface impurity and glass dust, perusal visible niobium metal gloss is without assorted speckle;
4) niobium ingot step 3) obtained carries out heat treatment: heat treatment temperature is 950 DEG C, and temperature retention time is 80min;
5) niobium ingot step 4) obtained carries out jumping-up to 350mm, forges the side of beating 250 × 250mm, and finally forging is beaten circle and arrived Φ 265mm;
6) niobium ingot step 5) obtained carries out heat treatment, 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, and chemical composition is the niobium ingot of Nb >=99.95%, electronic torch melting 2 times;
2) niobium ingot step 1) obtained preheats 250 DEG C, smears glass dust, and ingot heats 450 DEG C, is incubated 4.5h. Niobium ingot is carried out axial jumping-up to 300mm, pull out 480 × 480 × 390mm;
3) by step 2) the niobium ingot that obtains carries out pickling: HCl:HF:H2SO4=5:3:2(volume ratio), pickling time 10min, remove surface impurity and glass dust, perusal visible niobium metal gloss is without assorted speckle;
4) niobium ingot step 3) obtained carries out heat treatment: heat treatment temperature is 1200 DEG C, and temperature retention time is 100min;
5) niobium ingot step 4) obtained is preheated to 230 DEG C, smears 1mm glass dust;
6) niobium ingot step 5) obtained carries out jumping-up to 270mm, forges the side of beating 290 × 290mm, and finally forging is beaten circle and arrived Φ 300mm;
7) niobium ingot step 6) obtained carries out pickling HCl:HF:H2SO4=5:3:2(volume ratio), pickling time 10 minutes, remove surface impurity and glass dust, perusal visible niobium metal gloss is without carrying out heat treatment after assorted speckle, heat treated temperature is 1200 DEG C, and temperature retention time is 100min, obtains niobium sputtering target niobium base.
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention. It should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to the present invention carries out some improvement and modification, these improve and modify in the protection domain also falling into the claims in the present invention.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention. The multiple amendment of these embodiments be will be apparent from for those skilled in the art, and generic principles defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments. Therefore, the present invention is not intended to be limited to the embodiments shown herein, and is to fit to the widest scope consistent with principles disclosed herein and features of novelty.
Claims (8)
1. the forging method of a niobium rotary target material ingot casting, it is characterised in that comprise the following steps:
By the first time preheating of niobium ingot casting, niobium ingot casting surface-coated the first ORC after preheat;
The niobium ingot casting first time being coated with the first ORC is heated to 365 DEG C～472 DEG C, first time is incubated 2h～4.5h, niobium ingot casting after insulation is carried out first time jumping-up and first time pulling, the general working rate of first time jumping-up and first time pulling is 40%～65%, and the niobium ingot casting after first time forge hot carries out first time heat treatment;
By the niobium ingot casting second time heating after first time heat treatment to 365 DEG C～472 DEG C, second time is incubated 2h～4.5h, niobium ingot casting after second time insulation is carried out second time jumping-up and second time pulling, the working modulus of described second time jumping-up is 35%～50%, and the niobium ingot casting after second time forge hot carries out second time heat treatment.
2. forging method according to claim 1, it is characterised in that the temperature of preheating of described first time is 150 DEG C～250 DEG C.
3. forging method according to claim 1, it is characterised in that described first ORC is glass dust, the thickness of described ORC is 1mm～1.5mm.
4. forging method according to claim 1, it is characterised in that also include with before described first time heat treatment after described first time forge hot:
Niobium ingot casting after first time forge hot is carried out first time pickling.
5. forging method according to claim 4, it is characterised in that the mixed solution that acid solution is hydrochloric acid, Fluohydric acid. and sulphuric acid of described first time pickling, the time of described pickling is 5min～10min.
6. forging method according to claim 1, it is characterised in that heat treated temperature of described first time is 930 DEG C～1300 DEG C, and the described first time heat treated time is 60min～100min.
7. forging method according to claim 1, it is characterised in that also include with before described second time forge hot after described first time heat treatment:
Niobium ingot casting after first time heat treatment is carried out second time preheating, niobium ingot casting surface-coated the second ORC after second time preheating.
8. forging method according to claim 7, it is characterised in that also include with before described second time heat treatment after described second time forge hot:
Niobium ingot casting after second time forge hot is carried out second time pickling.
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| 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 |
| CN112548495B (en) * | 2020-11-26 | 2022-03-01 | 西北有色金属研究院 | Forging method of plate blank for superconducting wire barrier layer niobium sheet |
| CN113523012B (en) * | 2021-07-14 | 2022-05-03 | 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 |
| CN113718110B (en) * | 2021-08-11 | 2023-05-09 | 九江有色金属冶炼有限公司 | Preparation method of high-quality niobium plate adopting accumulated energy to control plate structure |
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| CZ20032246A3 (en) * | 2001-02-20 | 2004-03-17 | H. C. Starck, Inc. | Refractory metal plates of uniform structure and process for producing thereof |
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