CN107893214A - The technique of impurity and elemental gas defect in a kind of elimination nickel plate target - Google Patents
The technique of impurity and elemental gas defect in a kind of elimination nickel plate target Download PDFInfo
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- CN107893214A CN107893214A CN201711119757.2A CN201711119757A CN107893214A CN 107893214 A CN107893214 A CN 107893214A CN 201711119757 A CN201711119757 A CN 201711119757A CN 107893214 A CN107893214 A CN 107893214A
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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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/06—Refining
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/22—Remelting metals with heating by wave energy or particle radiation
- C22B9/228—Remelting metals with heating by wave energy or particle radiation by particle radiation, e.g. electron beams
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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- Engineering & Computer Science (AREA)
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- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Plasma & Fusion (AREA)
- Physical Vapour Deposition (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to coloured plus metal work field, provide impurity and the purifying technique of elemental gas defect present in a kind of elimination nickel plate target, mainly include stock, prepurging, vacuumize, melting, purification melting, forging, hot rolling, cold rolling and annealing, inspection the step of.The present invention can fully remove the gentle element of volume of the removal of impurity, such as Co, Fe, Cu and C, N, O, by being processed further, purity >=99.996% of nickel plate target can be obtained, and it is internal continuous unanimously without concentrating shrinkage cavity, loose the defects of increasing with stomata, segregation, crystal grain.
Description
Technical field
The invention belongs to technical field of nonferrous metal processing, is related to target, and in particular to one kind eliminates deposits in nickel plate target
Impurity and elemental gas defect purifying technique.
Background technology
The rapid development of information technology, it is desirable to which the integrated level more and more higher of integrated circuit, unit component size is not in circuit
It is disconnected to reduce, component size by grade to micron order, then to nanoscale.By substrate, insulating barrier, medium inside each unit component
The composition such as layer, conductor layer and protective layer.Wherein, dielectric layer, conductor layer even protective layer will use sputter coating process, therefore
Sputtering target material is to prepare one of core material of integrated circuit.Wherein, semiconductor coated film requires that the purity of nickel is very high with target,
Typically in 4N or more than 5N, therefore semiconductor coated film target is expensive.
If the excessive number of field trash in target, during sputter coating, it is easy to particulate is formed on wafer, is caused
Interconnection line short circuit or open circuit, have a strong impact on the performance of sputtered film.At present, still field trash in used target, using by
Limit, most field trashes are formed in melting and casting process, are mainly made up of oxide, in addition to nitride, carbonization
Thing, hydride, sulfide, silicide etc..Therefore, in target melting and casting process, should typically select by reducing material system
The crucible made, ingate, mold etc., and the oxide and other slags of bath surface are thoroughly removed before casting.It is general to use
Melting and casting under vacuum or oxygen-free environment, high-purity nickel target is prepared using electronic torch melting method.
At present, through to electronic beam vacuum smelting mode gained high-purity nickel ingot purity, surface quality and cast inside defect
Analysis and research, i.e., by the observation to nickel ingot casting macro morphology and the chemical analysis of impurity content, it is found that a melting twice can incite somebody to action
Raw material purify to 99.99% (as China applies for a patent 201610812462.2《A kind of system of semiconductor target timber-used high-purity nickel ingot
Standby technique》), but ingot casting still suffers from more macroscopical casting flaw, still can not meet the processing needs of high-purity nickel target.For
This, further melting processing of only trying every possible means, could fully remove the removal of impurity and pernicious gas element, such as Co, Fe, Cu and C, N, O
Deng, then nickel plate target needed for being rolled into, and the inside of nickel plate target is continuously consistent, no concentrating shrinkage cavity, it is loose with stomata, partially
The defects of analysis, crystal grain increase.
The content of the invention
It is an object of the invention to provide a kind of purification for eliminating impurity and elemental gas defect present in nickel ingot target
Technique, impurity and elemental gas are fully eliminated, such as Co, Fe, Cu and C, N, O, by being processed further, finally gives nickel plate
Purity >=99.996% of target, and it is internal continuous unanimously without concentrating shrinkage cavity, loose the defects of increasing with stomata, segregation, crystal grain.
Specifically technical scheme is：
A kind of technique of impurity and elemental gas defect in elimination nickel plate target, it is characterised in that the main stock, clear of including
Stove, vacuumize, melting, purification melting, forging, hot rolling, cold rolling and annealing, the step of examining, be specially：
Stock：Sheet nickel surface is polished, fillet nickel material is cut into, cleans up；
Prepurging：Nickel bar is tied up into rear shove charge, clearing furnace and reactor before shove charge, keeps high-purity environment；
Vacuumize：Body of heater and electron gun are vacuumized, furnace chamber and rifle room vacuum is distinguished ＜ 5 × 10-2With 5 × 10- 3pa；
Melting：Start after vacuumizing and electron gun and preheat, it is 60Kv to set electric high pressure, electric current 5A, electron beam hot spot shape
State is circle, bombards nickel material with the state of circular light spot, gradually increases beam power until electron beam bombards the nickel in region
Material all melts and flowed into water jacketed copper crucible；Adjust electron gun power and keep constant to 600Kw, and start timing, treat copper earthenware
When thering is a certain amount of metal nickel solution to start dummy ingot vertically downward in crucible, the slow speed of mobile control dummy ingot, until all nickel
Material melting is finished, and afterwards, slow downward electron gun performance number is disappeared at high-purity nickel ingot center until electron beam spot, electron gun
Nickel ingot is taken out in blow-on after closing 18h；
Purify melting：The nickel ingot is stripped off the skin, surface clean, repeat melting step described in n times, after annealing, taken
Sample examines to obtain the high-purity nickel ingot target of nickel purity >=99.996%, is transferred to forging step；
Forging：Vacuum flat-die forging cogging is used to form thickness as 50 ± 2mm slabs after the high-purity nickel ingot target annealing
Material, initial forging temperature is 850 DEG C ± 20 DEG C, and final forging temperature is 750 DEG C ± 20 DEG C；
Hot rolling：To plate blank material hot rolling, 850 DEG C ± 20 DEG C of hot-rolled temperature, the plate blank material thickness is rolled down to 15 ± 5mm's
The nickel plate target of different-thickness, puts to normal temperature；
Cold rolling and annealing：Put to the nickel plate target of normal temperature and keep the straight cold rolling of template, roll into 10 ± 5mm nickel plate target
Material, then annealed, annealing temperature is controlled at 730~780 DEG C, is incubated 10min, is put to room temperature, inspection is transferred to after cleaning；
Examine：Nickel plate target after cleaning, the size sawing according to needed for order；During inspection, template is smooth bright and clean, wipes out edge
Crackle, no scuffing or crack defect, qualified storage.
Further, the hot rolling is 855 DEG C.
Further, the annealing temperature controls 750 DEG C.
Further, the n times melting step, N 3,4 or 5 times.
Compared with prior art, technique effect of the invention is that the nickel plate target produced and processed by the present invention can be fully
Remove the gentle element of volume of the removal of impurity, such as Co, Fe, Cu and C, N, O.Purity >=99.996% of nickel plate target.Through examining, nickel plate target
It is continuous unanimously without concentrating shrinkage cavity, loose the defects of increasing with stomata, segregation, crystal grain inside material.
Embodiment
The present embodiment, the work of impurity and elemental gas defect in a kind of elimination nickel plate target of the present invention is described in further detail
Skill, its mainly include stock, prepurging, vacuumize, melting, purification melting, forging, hot rolling, cold rolling and annealing, inspection the step of,
Specially：
Stock：Fillet nickel material will be cut into after sheet nickel surface polishing scale removal and debris, cleaned up；
Prepurging：Nickel bar is tied up into rear shove charge, clearing furnace before shove charge, clears up reactor, is ensured miscellaneous without dropping in vacuum chamber
Thing, avoid polluting, keep high-purity environment；
Vacuumize：Open mechanical pump, lobe pump and diffusion pump respectively to vacuumize body of heater and electron gun, furnace chamber and rifle after 1h
Room vacuum respectively reaches 5 × 10-2With 5 × 10-3Below pa；
Melting：Start after vacuumizing and electron gun and preheat, setting high pressure is 60Kv, electric current 5A, electron beam hot spot form
For circle, it is heated evenly, stably with ensureing that electron beam bombards nickel material with the state of circular light spot all the time in fusion process, gradually
Increase beam power is until the nickel material that electron beam bombards region all melts and flowed into water jacketed copper crucible；Adjust electron gun
Power keeps constant to 600Kw, and starts timing, treats have a certain amount of metal nickel solution to start dummy ingot vertically downward in copper crucible
When, slowly the speed of mobile strict control dummy ingot, until all nickel material meltings finish, afterwards, slowly lowers electron gun performance number
Until electron beam spot is disappeared at high-purity nickel ingot center, electron gun closes blow-on taking-up nickel ingot after 18h；
Purify melting：The nickel ingot is stripped off the skin, surface clean, repeat melting step described in n times, after annealing, taken
Sample examines the high-purity nickel ingot target for finally giving nickel purity >=99.996%, is transferred to forging step；The n times are 3,4 or 5 effects
Fruit is optimal.
Forging：Vacuum flat-die forging cogging is used to form thickness as 50 ± 2mm slabs after the high-purity nickel ingot target annealing
Material, initial forging temperature is 850 DEG C ± 20 DEG C, and final forging temperature is 750 DEG C ± 20 DEG C；
Hot rolling：To plate blank material hot rolling, 850 DEG C ± 20 DEG C of hot-rolled temperature, wherein 855 DEG C of best results, by the plate blank material
Thickness is rolled down to the nickel plate target of 15 ± 5mm different-thickness；
Cold rolling and annealing：Put to the nickel plate target of normal temperature and keep the straight cold rolling of template, form 10 ± 5mm nickel plate target
Material, then annealed, annealing temperature is controlled at 730~780 DEG C, wherein 750 DEG C of best results, are incubated 10min, put to room temperature,
Inspection is transferred to after cleaning；
Examine：Nickel plate target after cleaning, the size sawing according to needed for order；During inspection, template is smooth bright and clean, wipes out edge
Crackle, no scuffing or crack defect, qualified storage.
Compared with the prior art, technique effect of the invention is shown：
1st, the present invention using heat caused by impact of the high-energy electron to electrolytic nickel material of electron beam gun transmitting by its
Fusing, cast ingot casting after being refined in bath.At a high speed, high-energy, high line and stable controllability are held electrolytic nickel material
Continuous, uniformity high energy bombardment.Electronics melting can remove gas content in raw material to greatest extent, avoid a large amount of gases from existing
Ingot solidification forming core at initial stage, the casting flaws such as loose, stomata are formed so as to avoid growing up in later stage continuous cooling process.
2nd, Gases In Metals impurity can be removed under vacuum condition, reduces the solubility of gaseous impurity in a metal.According to
Xi Weici laws, the square root of diatomic gas solubility in a metal and partial pressure is directly proportional under constant temperature.Therefore improve
The vacuum of system, just equivalent to the partial pressure for reducing gas, the solubility of gas in a metal can be also reduced, and more than dissolving
The portion gas impurity of degree will be escaped and removed from metal.In high vacuum conditions, moisture is drastically waved at 100~200 DEG C
Hair, 600~700 DEG C of hydride decomposition effusions, alkali metal and its compound are volatilized at a temperature of 1100~1600 DEG C, melted in nickel material
Point boiling point is volatilized so as to reach impurity less than the impurity element, most of iron, cobalt, copper etc. of matrix nickel in the form of low melting point oxide
Reduce the effect of purification.
3rd, electron gun power is lifted, raises constant temperature, the nitrogen volatilization effusion at 2210 DEG C, than hydrogen, nitrogen to metal parent
The big oxygen with power, then to add carbon deoxidation (C+O=CO ↑) and above-mentioned foreign metal low oxide to be removed, effectively reduction C,
O, N gaseous impurities content.
4th, by multiple melting, rolling, it can effectively remove and be wrapped inside attached entrance melt, internally shape in process of setting
Into gaseous impurity defect, so as to avoid nickel plate target concentrating shrinkage cavity, loose and stomata, segregation, crystal grain increase the defects of occur.
Claims (4)
- A kind of 1. technique of impurity and elemental gas defect in elimination nickel plate target, it is characterised in that the main stock, clear of including Stove, vacuumize, melting, purification melting, forging, hot rolling, cold rolling and annealing, the step of examining, be specially：Stock：Sheet nickel surface is polished, fillet nickel material is cut into, cleans up；Prepurging：Fillet nickel material is tied up into rear shove charge, clearing furnace and reactor before shove charge；Vacuumize：The body of heater and electron gun of vacuum melting furnace are vacuumized, furnace chamber and rifle room vacuum is distinguished ＜ 5 × 10-2With 5 ×10-3pa；Melting：Start after vacuumizing and electron gun and preheat, it is 60Kv to set electric high pressure, electric current 5A, and electron beam hot spot form is Circle, nickel material is bombarded with the state of circular light spot, the nickel material that gradual increase beam power bombards region up to electron beam is complete Melt and flow into water jacketed copper crucible in portion；Adjust electron gun power and keep constant to 600Kw, and start timing, treat in copper crucible When thering is a certain amount of metal nickel solution to start dummy ingot vertically downward, the slow speed of mobile control dummy ingot, until all nickel material melt Refining finishes, and afterwards, slowly lowers electron gun performance number until electron beam spot is disappeared at high-purity nickel ingot center, electron gun is closed Nickel ingot is taken out in blow-on after 18h；Purify melting：The nickel ingot is stripped off the skin, surface clean, repeat melting step described in n times, after annealing, sampling inspection Test to obtain the high-purity nickel ingot target of nickel purity >=99.996%, be transferred to forging step；Forging：Vacuum flat-die forging cogging is used to form thickness as 50 ± 2mm plate blank materials after the high-purity nickel ingot target annealing, Initial forging temperature is 850 DEG C ± 20 DEG C, and final forging temperature is 750 DEG C ± 20 DEG C；Hot rolling：To plate blank material hot rolling, 850 DEG C ± 20 DEG C of hot-rolled temperature, the plate blank material thickness is rolled down to 15 ± 5mm difference The nickel plate target of thickness, puts to normal temperature；Cold rolling and annealing：Put to the nickel plate target of normal temperature and keep the straight cold rolling of template, roll into 10 ± 5mm nickel plate target, Annealed again, annealing temperature is controlled at 730~780 DEG C, is incubated 10min, is put to room temperature, inspection is transferred to after cleaning；Examine：Nickel plate target after cleaning, the size sawing according to needed for order；During inspection, template is smooth bright and clean, wipes out edge and splits Line, no scuffing or crack defect, qualified storage.
- 2. the technique of impurity and elemental gas defect in a kind of elimination nickel plate target as claimed in claim 1, it is characterised in that： The n times melting step, N 3,4 or 5 times.
- 3. the technique of impurity and elemental gas defect in a kind of elimination nickel plate target as claimed in claim 1 or 2, its feature exist In：The hot-rolled temperature is 855 DEG C.
- 4. the technique of impurity and elemental gas defect in a kind of elimination nickel plate target as claimed in claim 1 or 2, its feature exist In：The annealing temperature is 750 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711119757.2A CN107893214A (en) | 2017-10-31 | 2017-10-31 | The technique of impurity and elemental gas defect in a kind of elimination nickel plate target |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592383A (en) * | 2020-06-16 | 2020-08-28 | 昆山国力大功率器件工业技术研究院有限公司 | Method for processing ceramic surface color change trace |
| CN112095019A (en) * | 2020-08-11 | 2020-12-18 | 大连理工大学 | Method for removing inclusions in high-temperature alloy through electron beam overheating dissolution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111592383A (en) * | 2020-06-16 | 2020-08-28 | 昆山国力大功率器件工业技术研究院有限公司 | Method for processing ceramic surface color change trace |
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| CN112095019A (en) * | 2020-08-11 | 2020-12-18 | 大连理工大学 | Method for removing inclusions in high-temperature alloy through electron beam overheating dissolution |
| CN112095019B (en) * | 2020-08-11 | 2021-07-30 | 大连理工大学 | Method for removing inclusions in high-temperature alloy through electron beam overheating dissolution |
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