CN103898459A - Preparation method of high-purity cobalt target - Google Patents
Preparation method of high-purity cobalt target Download PDFInfo
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- CN103898459A CN103898459A CN201410152954.4A CN201410152954A CN103898459A CN 103898459 A CN103898459 A CN 103898459A CN 201410152954 A CN201410152954 A CN 201410152954A CN 103898459 A CN103898459 A CN 103898459A
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Abstract
The invention relates to a preparation method of a high-purity cobalt target, which sequentially comprises the following steps: carrying out radial forging and annealing treatment on a high-purity cobalt ingot with the purity of higher than 99.999%; cutting the treated high-purity cobalt ingot into short pieces, and carrying out longitudinal upsetting and annealing treatment on the short pieces; carrying out repeated calendering and annealing treatment on the treated high-purity cobalt forge piece to obtain a cobalt target billet; and machining the cobalt target billet, and bonding with a copper back panel through an eutectic solder to obtain the high-purity cobalt target. The method obtains the cobalt forge piece with compact inside and uniform microstructure, and overcomes the defect of high rejection rate due to high tendency to cracking in the subsequent calendering process since the cobalt target is hard and fragile. The calendering and annealing treatment can enhance the magnetic permeability of the cobalt target.
Description
Technical field
the present invention relates to a kind of preparation method of high-purity cobalt target.
Background technology
cobalt is the important materials of preparing the components and parts such as magnetic recording media, magnetic recording head, photoelectric device, Magnetic Sensor and unicircuit.Purity is the manufacture that 99.9% ~ 99.99% cobalt has been widely used in magneticsubstance, superalloy, and 99.999% even more highly purified cobalt is used for manufacturing sputtering target material, as manufacturing semi-conductor chip contact layer CoSi
2
material.
sputtering target material is to manufacture the extremely important material of the necessary one of semi-conductor chip, its principle is to adopt physical gas phase deposition technology (PVD), accelerate gas ion with high pressure and bombard target, the atom of target is sputtered out, deposit on silicon chip with the form of film, finally form distribution structure complicated in semi-conductor chip.Sputter coating has the many advantages such as membrane uniformity, controllability, is widely used in semiconductor applications.Along with developing rapidly of semicon industry, increasing to the demand of sputtering target material, sputtering target material has become semicon industry and has developed indispensable material.
grain-size, preparation and the performance of grain orientation to unicircuit metallic film of target have a great impact.Be mainly manifested in: 1. along with the increase of grain-size, film deposition rate is tending towards reducing; 2. in suitable grain size range, plasma impedance when target uses is lower, and film deposition rate is high and film gauge uniformity is good; 3. for improving the performance of target, in controlling target crystalline grains size, also must strictly control the grain orientation of target.
the grain-size of target and grain orientation are mainly adjusted and are controlled by even processing, thermomechanical processing.
semi-conductor uses the general purity requirement of cobalt sputtering target material more than 4N (99.99%).Manufacture method is that high-purity cobalt powder first sinters piece into substantially, obtain high-purity cobalt ingot by vacuum melting furnace again, then cobalt ingot is carried out to viscous deformation and annealing repeatedly, finally carry out recrystallization annealing processing at 400 DEG C ~ 600 DEG C, thereby obtain the cobalt target base with even grained and certain inner texture, target base is by welding and machined with backboard, final finished.
in such manufacture method, high-purity cobalt powder need to first sinter piece into, and then become ingot through vacuum melting, then through moulding distortion and annealing repeatedly, process and could finally obtain the target base that can be used for semi-conductor sputtering target material and manufacture use finally by recrystallization annealing.
whole complex process, cost is also high.High-purity cobalt powder need to be melted, and easily sneaks into the impurity being brought by crucible and reductor etc.It is not very high becoming the purity of cobalt ingot with vacuum melting.The temperature of the anneal of using in subsequent technique is unreasonable, and the cobalt target base forming like this can not get high magnetic spectroscopy susceptibility (Pass Through Flux).And the low cobalt target of magnetic spectroscopy susceptibility, sputtering performance is poor, and target utilization is low, and even sputter cannot continue to carry out.
Summary of the invention
technical problem to be solved by this invention is to provide a kind of preparation method of high-purity cobalt target of high magnetic spectroscopy susceptibility.
for solving above technical problem, the present invention takes following technical scheme:
a preparation method for high-purity cobalt target, comprises the following steps of carrying out successively:
(1), be that more than 99.999% high-purity cobalt ingot carries out radial forging and anneal by purity, wherein, radial forging forging ratio is more than or equal to 2;
(2), will after step (1) is processed, be cut into pipe nipple by high-purity cobalt ingot, described pipe nipple is carried out to the thick and anneal of longitudinal pier, wherein, longitudinal thick short transverse deflection of pier is greater than 60%;
(3), will repeatedly roll with anneal and obtain cobalt palladium base through step (2) high-purity cobalt forging after treatment, wherein, carry out, before described calendering, described high-purity cobalt forging is carried out to thermal pretreatment 50 ~ 70 minutes at 300 DEG C ~ 340 DEG C at every turn; The thickness direction total deformation of calendering is more than or equal to 60%; Described anneal, for being slowly warmed up to 300 ~ 400 DEG C, is incubated 50 ~ 70 minutes, then naturally cools to 15 DEG C ~ 40 DEG C;
(4), described cobalt palladium base is carried out to mechanical workout, then bond together by eutectic solder and copper backboard, obtain described high-purity cobalt target.
preferably, the preparation method of described high-purity cobalt ingot is: adopt electrolytic process to prepare high-purity cobalt; Described high-purity cobalt is smelted into described high-purity cobalt ingot.
preferably, adopt clean electrolytic solution to carry out described electrolysis, the purity of described high-purity cobalt is more than 99.999%.
preferably, be under 0.3 ~ 4Pa in vacuum tightness, adopt vacuum electron beam to carry out described melting.
preferably, in step (3), carry out, before described radial forging, described high-purity cobalt ingot is carried out to thermal pretreatment, the temperature of described thermal pretreatment is 700 DEG C ~ 900 DEG C, and soaking time is 50 ~ 70 minutes.
preferably, in step (3), adopt air hammer to carry out described radial forging to described high-purity cobalt ingot.
in an embodiment, utilize air hammer to carry out impacting of circumferential direction to high-purity cobalt ingot, the cross-sectional area of high-purity cobalt ingot is reduced, highly increase, the ratio of the cross-sectional area of radial forging after than the cross-sectional area and the radial forging that are before radial forging.
particularly, the diameter of described high-purity cobalt ingot is 250 ~ 350mm; The diameter of step (1) high-purity cobalt ingot after treatment is 120 ~ 175mm; The height of the pipe nipple described in step (2) is 45 ~ 55mm; Height after longitudinal pier is thick is 10 ~ 18mm; In step (3), the thickness of cobalt palladium base is 5.5 ~ 6.6mm; The thickness of described high-purity cobalt target is 4.5 ~ 5.5mm.
in step (3), owing to carrying out the temperature of thermal pretreatment and be greater than the recrystallization temperature of cobalt metal before radial forging, so, that in this step, carries out is forged to forge hot, the advantage of forge hot is the as-cast structure that changes ingot metal, and in hot forging process, through recrystallize, thick as-cast structure becomes the new organization of small grains, and reduce the defect of as-cast structure, improve the plasticity of metal.
preferably, in step (3), described anneal, for being slowly warmed up to 500 DEG C ~ 700 DEG C, is incubated 2 ~ 3 hours, then naturally cools to 15 DEG C ~ 40 DEG C.
preferably, in step (4), the longitudinal pier described in carrying out is slightly front carries out thermal pretreatment to described high-purity cobalt ingot, and the temperature of described thermal pretreatment is 700 DEG C ~ 900 DEG C, and soaking time is 50 ~ 70 minutes.
preferably, in step (4), the longitudinal pier described in employing hydraulic forging press carries out described high-purity cobalt ingot is thick.
be in particular, utilize hydraulic forging press to carry out pier to high-purity cobalt ingot thick, the cross-sectional area of cobalt ingot is increased, highly reduce.
preferably, in step (4), described anneal, for being slowly warmed up to 500 DEG C ~ 700 DEG C, is incubated 2 ~ 3 hours, then naturally cools to 15 DEG C ~ 40 DEG C.
calendering in step (5) can change texture direction, and the Z axis of the crystal grain much with hcp structure is approached perpendicular to cobalt target base surface.
preferably, in step (6), described eutectic solder is indium, tin, indium stannum alloy.
due to the enforcement of above technical scheme, the present invention compared with prior art tool has the following advantages:
the present invention obtains the higher cobalt ingot of purity by vacuum electron beam smelting technique, and by radial forging and anneal, the longitudinal thick and anneal of pier, interior solid, the uniform cobalt forging of microtexture are obtained, overcome cobalt target because quality is hard frangible, after easily crack in calender line and cause the problem that condemnation factor is high.Calendering and anneal are to have close-packed hexagonal structure as much as possible (hcp) crystal grain in the cobalt target in order to make to manufacture, and the Z axis in the hcp lattice of cobalt is easy magnetized direction.This direction perpendicular to or approach perpendicular to target material surface, can improve the magnetic spectroscopy susceptibility of cobalt target.Along with the increase of deflection, have increasing hcp crystal grain, its Z-direction perpendicular to or approach perpendicular to target material surface.
Brief description of the drawings
accompanying drawing 1 is process flow sheet of the present invention.
Embodiment
below in conjunction with specific embodiment, the present invention will be further described in detail, but the present invention is not limited to following examples.The implementation condition adopting in embodiment can require to do further adjustment according to the difference of concrete use, and not marked implementation condition is the normal condition in the industry.
embodiment 1
the preparation method of high-purity cobalt target is as follows:
(1), adopt clean electrolytic solution to go out high-purity cobalt by electrolytic process electrolysis, the purity 99.999% of high-purity cobalt.
(2), to adopt vacuum tightness be 0.3Pa, and high-purity cobalt is smelted into high-purity cobalt ingot by vacuum electron beam melting furnace, the diameter of high-purity cobalt ingot is 300mm, purity 99.999%.
(3), need high-purity cobalt ingot to carry out thermal pretreatment before radial forging, the mode of preheating, for high-purity cobalt ingot is heated to 700 DEG C, is incubated 1 hour; Then utilize air hammer to carry out radial forging (being impacting of circumferential direction) to high-purity cobalt ingot, the cross-sectional area of cobalt ingot is reduced, highly increase, the spindle diameter forging is about 150mm; After radial forging, be slowly warmed up to 500 DEG C, be incubated 2 hours, then naturally cool to room temperature.
(4), by after radial forging, pulling forging be cut into the pipe nipple that is highly about 50mm, then carry out thermal pretreatment, thermal pretreatment mode, for being warmed up to 700 DEG C, is incubated 1 hour; Then utilize hydraulic forging press to carry out pier to high-purity cobalt ingot thick, the cross-sectional area of cobalt ingot is increased, highly reduce, the forging height after pier is thick is about 15mm, and the deformation rate of the thick rear short transverse of pier is about 70%; After longitudinal pier is thick, be slowly warmed up to 500 DEG C, be incubated 2 hours, then naturally cool to room temperature.
(5) forging, after thick to longitudinal pier carries out thermal pretreatment, and thermal pretreatment mode, for being warmed up to 300 DEG C, is incubated 1 hour; Then between two rollers of rolling press, be highly the upper and lower surface of the cobalt part of 15mm originally by roller extruding, through calendering repeatedly, finally extend into the nahlock cobalt target base that thickness is about 6mm, the deformation rate of the thickness direction of calendering is about 60%; After calendering, be slowly warmed up to 300 DEG C, be incubated 1 hour, then naturally cool to room temperature.
(6), finally cobalt target base is carried out to car mill and is processed into the cobalt target that thickness is 5mm, then itself and copper backboard are bonded together as scolder with indium.Scan (c-scan) with ultrasonic wave c and detect bonding rate >95%.Record magnetic spectroscopy susceptibility PTF(Pass Through Flux by ASTM standard) 86%.
embodiment 2
the preparation method of high-purity cobalt target is as follows:
(1), adopt clean electrolytic solution to go out high-purity cobalt by electrolytic process electrolysis, the purity 99.999% of high-purity cobalt.
(2), to adopt vacuum tightness be 0.3Pa, and high-purity cobalt is smelted into high-purity cobalt ingot by vacuum electron beam melting furnace, the diameter of high-purity cobalt ingot is 300mm, purity is 99.999%.
(3), need high-purity cobalt ingot to carry out thermal pretreatment before radial forging, the mode of preheating, for high-purity cobalt ingot is heated to 800 DEG C, is incubated 1 hour; Then utilize air hammer to carry out radial forging (being impacting of circumferential direction) to high-purity cobalt ingot, the cross-sectional area of cobalt ingot is reduced, highly increase, the spindle diameter forging is about 150mm; After radial forging, be slowly warmed up to 600 DEG C, be incubated 2 hours, then naturally cool to room temperature.
(4), by after radial forging, pulling forging be cut into the pipe nipple that is highly about 50mm, then carry out thermal pretreatment, thermal pretreatment mode, for being warmed up to 800 DEG C, is incubated 1 hour; Then utilize hydraulic forging press to carry out pier to high-purity cobalt ingot thick, the cross-sectional area of cobalt ingot is increased, highly reduce, the forging height after pier is thick is about 15mm, and the deformation rate of the thick rear short transverse of pier is about 70%; After longitudinal pier is thick, be slowly warmed up to 600 DEG C, be incubated 2 hours, then naturally cool to room temperature.
(5) forging, after thick to longitudinal pier carries out thermal pretreatment, and thermal pretreatment mode, for being warmed up to 350 DEG C, is incubated 1 hour; Then between two rollers of rolling press, be highly the upper and lower surface of the cobalt part of 15mm originally by roller extruding, through calendering repeatedly, finally extend into the nahlock cobalt target base that thickness is about 6mm, the deformation rate of the thickness direction of calendering is about 60%; After calendering, be slowly warmed up to 350 DEG C, be incubated 1 hour, then naturally cool to room temperature.
(6), finally cobalt target base is carried out to car mill and is processed into the cobalt target that thickness is 5mm, then itself and copper backboard are bonded together as scolder with indium.Scan (c-scan) with ultrasonic wave c and detect bonding rate >95%.Record magnetic spectroscopy susceptibility PTF(Pass Through Flux by ASTM standard) 82%.
comparative example 1
(1), being 99.99% to purity, high-purity cobalt ingot carries out thermal pretreatment, the mode of preheating, for cobalt ingot is heated to 700 DEG C, is incubated 1 hour; Utilize air hammer to hit and the upper surface of cobalt ingot is hit to two kinds of modes along circumferential direction cobalt ingot and hocket, each deformation rate of forging is 50%;
(2) the cobalt ingot after forging is slowly warmed up to 500 DEG C, is incubated 2 hours, then naturally cool to room temperature.
(3) before rolling, cobalt ingot is carried out to thermal pretreatment, thermal pretreatment mode, for being warmed up to 420 DEG C, is incubated 1 hour; Then between two rollers of rolling press, by the upper and lower surface of roller extruding cobalt part, through calendering repeatedly, finally extend into nahlock cobalt target base, the deformation rate of the thickness direction of calendering is about 70%; After calendering, be slowly warmed up to 450 DEG C, be incubated 1 hour.
(4), finally cobalt target base is carried out to car mill and is processed into cobalt target, then bond together with backboard.Scan (c-scan) with ultrasonic wave c and detect bonding rate >95%.Record magnetic spectroscopy susceptibility PTF (Pass Through Flux) 68% by ASTM standard.
above the present invention is described in detail; its object is to allow the personage who is familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; the equivalence that all spirit according to the present invention are done changes or modifies, and all should be encompassed in protection scope of the present invention.
Claims (10)
1. a preparation method for high-purity cobalt target, is characterized in that: comprise the following steps of carrying out successively:
(1), be that more than 99.999% high-purity cobalt ingot carries out radial forging and anneal by purity, wherein, radial forging forging ratio is more than or equal to 2;
(2), will after step (1) is processed, be cut into pipe nipple by high-purity cobalt ingot, described pipe nipple is carried out to the thick and anneal of longitudinal pier, wherein, longitudinal thick short transverse deflection of pier is greater than 60%;
(3), will repeatedly roll with anneal and obtain cobalt palladium base through step (2) high-purity cobalt ingot after treatment, wherein, carry out, before described calendering, described high-purity cobalt ingot is carried out to thermal pretreatment 50 ~ 70 minutes at 300 DEG C ~ 340 DEG C at every turn; The thickness direction deflection of calendering is more than or equal to 60%; Described anneal, for being slowly warmed up to 300 ~ 400 DEG C, is incubated 50 ~ 70 minutes, then naturally cools to 15 DEG C ~ 40 DEG C;
(4), described cobalt palladium base is carried out to mechanical workout, then bond together by eutectic solder and copper backboard, obtain described high-purity cobalt target.
2. the preparation method of high-purity cobalt target according to claim 1, is characterized in that: the preparation method of described high-purity cobalt ingot is: adopt electrolytic process to prepare high-purity cobalt; Described high-purity cobalt melting is cast into described high-purity cobalt ingot.
3. the preparation method of high-purity cobalt target according to claim 2, is characterized in that: be under 0.3 ~ 4Pa in vacuum tightness, adopt vacuum electron beam to carry out described melting.
4. the preparation method of high-purity cobalt target according to claim 1, it is characterized in that: in step (3), carry out, before described radial forging, described high-purity cobalt ingot is carried out to thermal pretreatment, the temperature of described thermal pretreatment is 700 DEG C ~ 900 DEG C, and soaking time is 50 ~ 70 minutes.
5. the preparation method of high-purity cobalt target according to claim 1, is characterized in that: in step (3), adopt air hammer to carry out described radial forging to described high-purity cobalt ingot.
6. the preparation method of high-purity cobalt target according to claim 1, is characterized in that: in step (3), described anneal, for being slowly warmed up to 500 DEG C ~ 700 DEG C, is incubated 2 ~ 3 hours, then naturally cools to 15 DEG C ~ 40 DEG C.
7. the preparation method of high-purity cobalt target according to claim 1, it is characterized in that: in step (4), longitudinal pier described in carrying out is slightly front carries out thermal pretreatment to described high-purity cobalt ingot, and the temperature of described thermal pretreatment is 700 DEG C ~ 900 DEG C, and soaking time is 50 ~ 70 minutes.
8. the preparation method of high-purity cobalt target according to claim 1, is characterized in that: in step (4), the longitudinal pier described in employing hydraulic forging press carries out described high-purity cobalt ingot is thick.
9. the preparation method of high-purity cobalt target according to claim 1, is characterized in that: in step (4), described anneal, for being slowly warmed up to 500 DEG C ~ 700 DEG C, is incubated 2 ~ 3 hours, then naturally cools to 15 DEG C ~ 40 DEG C.
10. the preparation method of high-purity cobalt target according to claim 1, is characterized in that: in step (6), described eutectic solder is indium, tin, indium stannum alloy.
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| CN111118459A (en) * | 2019-12-30 | 2020-05-08 | 有研亿金新材料有限公司 | Preparation method of high-performance ferromagnetic target material |
| CN111155060A (en) * | 2018-11-07 | 2020-05-15 | 宁波江丰电子材料股份有限公司 | Method for manufacturing cobalt target blank |
| CN111604651A (en) * | 2020-06-28 | 2020-09-01 | 沈阳有色金属加工有限公司 | Preparation method of large-size high-purity copper rotary target material |
| CN112779508A (en) * | 2020-12-28 | 2021-05-11 | 宁波江丰电子材料股份有限公司 | Preparation method of high-purity vanadium target blank and high-purity vanadium target prepared by using same |
| CN118272678A (en) * | 2024-03-26 | 2024-07-02 | 重庆材料研究院有限公司 | Preparation method of cobalt wire for self-energized neutron sensing element |
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| CN118272678A (en) * | 2024-03-26 | 2024-07-02 | 重庆材料研究院有限公司 | Preparation method of cobalt wire for self-energized neutron sensing element |
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