CN105177357A - Production method of pure nickel N6 used for lithium battery rivets and having higher qualified product ratio - Google Patents
Production method of pure nickel N6 used for lithium battery rivets and having higher qualified product ratio Download PDFInfo
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- CN105177357A CN105177357A CN201410255451.XA CN201410255451A CN105177357A CN 105177357 A CN105177357 A CN 105177357A CN 201410255451 A CN201410255451 A CN 201410255451A CN 105177357 A CN105177357 A CN 105177357A
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Abstract
The invention relates to a production method of pure nickel N6 used for lithium battery rivets and having higher finished product ratio. The production method includes the following steps: 1) vacuum smelting; 2) electroslag remelting; 3) forging cogging; 4) hot rolling molding; 5) coarse wire drawing; 6) blank pickling and whitening; 7) grinding and trimming; 8) annealing treatment; 9) pickling testing; 10) fine broaching; and 11) heat treatment. Reasons why the pure nickel N6 generates unhealthy phenomena during rivet pressing are studied, production optimization is carried out in the production process, the purity of the product is ensured, and various pure nickel N6 unhealthy conditions generated during rivet pressing are significantly reduced. By adopting a vacuum induction melting furnace and by optimizing the production process, non-metallic inclusions in steel is reduced from the interior and the exterior and induced cracks and other harms are relieved.
Description
Technical field
The present invention relates to pure nickel N6 and manufacture craft thereof, specifically lithium cell rivet pure nickel N6 and production method thereof.
Background technology
In recent years, along with the develop rapidly of China Electronics's information industry, the demand of lithium cell rivet is increasing, because purity is the nickel of 99%, iron mold can not be there is in 20 years, its superior plasticity and corrosion resisting property can bear the pressure of reaction generation and the corrosion of electrolytic solution in battery, and do not occur to leak and receive favor greatly, its consumption also continues to increase thereupon.
The utilization ratio of raw material, in order to cost-saving, improves in processor, selects the mode of low-loss cold-heading compacting to process.In the course of processing, occurred a large amount of bad phenomenon, there is crack defect in wire rod end face.Because nickel has certain drag to various reductibility chemical substance, and is irreplaceable to the drag of caustic alkali.Compared with nickel-base alloy, pure nickel has higher conduction and heat conductivility, and Curie temperature is also higher simultaneously, has good Magnetostriction.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of lithium cell rivet pure nickel N6 and production method thereof, by carrying out Optimizing manufacture in process of production, ensure that the purity of product, considerably reduces the various unfavorable conditions that pure nickel N6 occurs when pressed rivet.
For solving the problems of the technologies described above, lithium cell rivet pure nickel N6 provided by the invention, the weight percent content of it each composition comprised is respectively: nickel: >=99.5%, manganese :≤0.05%, magnesium :≤0.1%, silicon :≤0.1%, sulphur :≤0.005%, carbon :≤0.1%, phosphorus :≤0.002%.
The production method of above-mentioned pure nickel N6, comprises successively: vacuum melting → esr → forge cogging → hot-roll forming → crin drawing → sour openpore material → polishing deburring → anneal → pickling test → cold drawn → thermal treatment, and above steps is as follows respectively:
1) vacuum melting: by raw material Jinchuan Ni plate and Ultra-low carbon furnace charge after baking, load in vacuum induction melting furnace and carry out melting, high-power high speed melt is added after melting 70%, when entering refining period after refining temperature more than 1550 DEG C (preferably 1600 DEG C) to be achieved after fine melt, refining keeps at least 30 minutes, and the refining later stage turns rough vacuum (10
3-10
-1pa), tapping in high-power stirring 1-3 minute, waters injecting electrode;
2) esr: by the preferred 1:1 of 0.9:1 to 1.1:1() mass ratio fluorite and titanium dioxide are prepared into striking agent, adopt CaF2, Al2O3 and CaO to make remelting electroslag system, wherein, the mass percent of three is: CaF
2: 65%-75%, Al
2o
3: 15%-25%, CaO: surplus; Shove charge, striking slag making, smelting, feeding, cooling, make steel ingot base; When adding slag, spoon does not allow to contact with crystallizer, electrode bar or slag charge on crystallizer disorderly smash by slag spoon simultaneously, striking electric current is 500-1500A, normally smelt again after slag fine melt, control electric current 2500-3000A, voltage 38-41V, make electrode melting, until crystallizer is filled, smelting finishes carries out feeding, the de-ingot air cooling of remelted ingot cooling;
Described vacuum metling operation and esr operation, the ZGHL0.25-250-1 type vacuum induction melting furnace used improves purity and the uniform texture of steel alloy effectively, improve the surface of steel ingot, inner quality, improve the performance of steel alloy, reduce further the generation of nonmetallic inclusionsin steel.
3) cogging is forged: (1) preheating: steel ingot base is heated to 850 DEG C by room temperature, preheating 30-50 minute;
(2) heat up: be warmed up to 1050-1150 DEG C and turn over ingot blank, insulation 40-50 minute;
(3) be incubated: when reaching forging temperature, initial forging temperature >=1100 DEG C, final forging temperature >=950 DEG C.
(4) forging: adopt the second light industry bureau one weight, two uniform methodologys make steel ingot.
Described forging forges to start to touch with less deflection, improve rear bang of taking the circumstances into consideration etc. plasticity, touch again when closing on final forging temperature, require that distortion is even, avoid repeatedly clashing at same position, forge in process and want duty to stand up, diligent charging, it is wide that each inlet amount should be less than brill, be greater than draught, avoid producing hammering and folding, failure surface, affects the quality of cold heading steel.
4) hot-roll forming: material loads the temperature of annealing furnace :≤600 DEG C; Heating-up time >=120 minutes; Heating temperature: 1100-1150 DEG C; Soaking time: >=30 minutes, begins to roll temperature: >=1100 DEG C; Finishing temperature >=950 DEG C.
Above-mentioned hot-rolled process, enters stokehold and assembles production spare part and adjust, and can avoid producing folding in the operation of rolling or scratching, destroy product surface, form the crackle of cracking.
5) crin drawing: before operation, first carries out joining mould, carries out drawing process by deformation requirements glomerocryst mould.
Described crin drawing procedure, according to dimensional requirement, need select the mould of suitable pass, and it is as follows to join mold technique standard:
Unit (mm) " * " represents annealing (annealing temperature is see " well vacuum electric furnace thermal treatment (annealing) table look-up ")
￠12.0—￠11.0—￠10.0*—￠8.0—￠7.0—￠6.0—￠5.0*
Well vacuum electric furnace thermal treatment (annealing) table look-up
| Classification | State | Specification mm | Heating temperature DEG C | Soaking time | The type of cooling |
| Nickel-base alloy | Work in-process | ≥￠8 | 800-850 | >=40 minutes | Air cooling |
6) sour openpore material: with sulfuric acid immersion, salt acid rinse to white, pickling temperature 30-70 DEG C, pickling time 20-35 minute.
Blank pickle solution proportioning:
| Pickle solution proportioning | Concentration % | Temperature DEG C | Time |
| HCL:HNO3:H2O=1:1: surplus | 15 | 30-50 | 10-20 |
| Pickle solution proportioning | Concentration % | Temperature DEG C | Time |
| H2SO4:HNO3:NaCl:H2O=4:1:1: surplus | 30 | 50-70 | 10-15 |
Described pickling process, concentration is with the Weight computation of complex acid, and the blank after pickling must embathe and high pressure water flushing wash clean, conveniently finds out surface crack.
7) polishing deburring: check material surface situation, if any surface imperfection (as burr, foreskin, crackle), carry out reconditioning process with portable emery wheel.
8) anneal: be placed on by crin in pit type annealing furnace and carry out anneal, temperature, at 800 DEG C-850 DEG C, is incubated 1-2 hour.
9) pickling test: with sulfuric acid immersion, salt acid rinse to white, pickling temperature 50-80 DEG C, pickling time 8-15 minute.Check material surface situation, carry out light pruning with portable emery wheel, require that the surface imperfection degree of depth is no more than 0.5mm.
10) finish draw: (1) joins mould: according to dimensional requirement, the mould of suitable pass need be selected, it is as follows to join mold technique standard:
Unit (mm) " * " represents annealing (annealing temperature is see " well vacuum electric furnace process (annealing) table look-up ")
￠4.0—￠3.0—￠2.5—￠2.0*-￠1.48
￠4.0—￠3.0—￠2.5—￠1.8*—￠1.18
(2) finish draw: often draw next specification all to need to carry out pickling test, reconditioning process.
11) thermal treatment: be placed in well formula argon shield bright annealing oven by the silk material after cold drawn and heat-treat, thermal treatment temp is at 800 DEG C-850 DEG C, and insulation is air cooling after 1-2 hour, discharging.
Above-mentioned annealing thermal treatment and thermal treatment, can improve or eliminate steel casting, forge, the various tissues disappearance that causes in the process such as rolling and unrelieved stress, and crystal grain thinning, prevent stress concentration, thus reduce the cracking probability of pure nickel wire in pressing process, larger deflection can be born, there is larger unit elongation, relative reduction in area, preferably plasticity and higher toughness and intensity.
The present invention from feeding intake with regard to the generation of attentional manipulation nonmetallic impurity, first ZGHL0.25-250-1 type vacuum induction melting furnace is used effectively to improve purity and the uniform texture of steel alloy, improve the surface of steel ingot, inner quality, improve the performance of steel alloy, reduce the content of nonmetallic inclusionsin steel and the gas content of H, O; Secondly deoxidation, crystal grain thinning process, expand the deflection of steel, unit elongation, relative reduction in area, preferably plasticity and higher toughness and intensity; Then steel ingot enters that stove forges, assembles and adjust before rolling to production spare part, avoids producing folding in process or scratching, destroys product surface, form the crackle of cracking.Finally by the pickling carried out blank repeatedly, reconditioning, annealing, drawing, accomplish surperficial zero-fault as far as possible.
Embodiment
Battery rivet pure nickel N6, its chemical composition is (wt.% represents): nickel: 99.99%, carbon: 0.01%.
The production method of above embodiment comprises the following steps:
1, vacuum melting:
(1), raw material prepares: described furnace charge is Jinchuan Ni plate and Ultra-low carbon material, for subsequent use after baking;
(2), feed: load after baking for subsequent use by raw material Jinchuan Ni plate and Ultra-low carbon furnace charge in vacuum induction melting furnace;
(3), refining: low power material, adds high-power high speed melt after melting 70%, and when entering refining period after refining temperature 1600 degree to be achieved after fine melt, refining keeps at least 30 minutes;
(4), pour into a mould: the refining later stage turns rough vacuum (10
3-10
-1pa), high-power stirring tapping in a minute, waters injecting electrode.Steel teeming ladle used should clean, and do not have cold steel, residue, bucket wall stopper rod can not have the grey black, oil smoke etc. that burn incompletely.
2, esr:
(1), the allotment of striking agent and remelting electroslag system: in the ratio of 1:1, fluorite and titanium dioxide are prepared into striking agent, CaF2, Al2O3 and CaO press 7:2:1 and make remelting electroslag system;
(2), shove charge: chassis, striking agent, crystallizer and electrode are installed, necessary first water flowing before dress crystallizer, and check with or without drainage, pad powder on trying to get to the heart of a matter and must be tight between crystallizer, pad powder inner ring will circle as far as possible, water tank face wants dry, clean, puts striking agent, to ensure its electroconductibility;
(3), striking slag making: reduce electrode and electrode is contacted with striking agent, complete striking work, striking agent is melted, add remelting electroslag system;
(4), smelt: when adding slag, spoon does not allow to contact with crystallizer, electrode bar or slag charge on crystallizer disorderly smash by slag spoon simultaneously, striking electric current is 500-1500A, normally smelt again after slag fine melt, control electric current 2500-3000A, voltage 38-41V, make electrode melting, until crystallizer is filled;
(5), feeding cooling: smelting finishes carries out feeding, feeding electric current diminishes gradually, until current value becomes 0, and feeding time 3-5 minute, electroslag face more than 3cm is left in electrode rising could have a power failure, de-ingot air cooling after remelted ingot cools 30 minutes in a crystallizer.
3, cogging is forged:
(1), preheating: steel ingot base is heated to 850 DEG C by room temperature, answers slow heat, preheating 30-50 minute;
(2), heat up: steel nail base rapid heating is warmed up to 1050-1150 DEG C, and duty turns over ingot blank, makes its equalizing temperature, insulation 40-50 minute;
(3), be incubated: reach when forging temperature and be incubated, be incubated and forge for 20 minutes, initial forging temperature is 1100 DEG C, and final forging temperature is 950 DEG C.
(4), forging: forging adopts the second light industry bureau one weight, and two uniform methodologys make steel ingot.Forge the slag, oxide skin, rubbish etc. that start in front and process, to clear up surface in time, first touch with less deflection, improve rear bang of taking the circumstances into consideration etc. plasticity, touch again when closing on final forging temperature, require that distortion evenly, avoids repeatedly clashing at same position, forge in process and want duty to stand up, diligent charging, it is wide that each inlet amount should be less than brill, is greater than draught, avoids producing hammering and folding, failure surface, affects the quality of cold heading steel.
4, hot-roll forming:
(1), material loads the temperature of annealing furnace :≤600 DEG C;
(2), heating-up time >=120 minutes;
(3), Heating temperature: 1100-1150 DEG C;
(4), soaking time: >=30 minutes;
(5), begin to roll temperature: >=1100 DEG C;
(6), finishing temperature >=950 DEG C.
Enter stokehold to assemble production spare part and adjust, import and export guide and guard in the same horizontal line, and must keep optimum distance with roll.Can not high-speed rolling during rolling, can avoid producing folding in the operation of rolling or scratching, destroy product surface, form the crackle of cracking.
5, crin drawing: (1), wire drawing skidding processing requirement: before operation, first puts into the lubricant (see table-1) prepared and lubricates, fully stir, coating uniform by parcel.Parcel after lubrication should evenly be spread out, carries out Exposure to Sunlight and dries or dry.Lubricating box should keep clean dry, removes foul and lump in box.
Lubricant formulation ratio
| Starting material title | Technical requirements | Quantity (kg) |
| Graphite Powder 99 | 200-300# | 50 |
| Machine oil | 20# | 50 |
| Soap | 5 | |
| Lime | 10 | |
| Water | 500 |
Table-1
(2), join mold technique requirement: according to dimensional requirement, need select the mould of suitable pass, it is as follows to join mold technique standard:
Unit (mm) " * " represents annealing (annealing temperature is see " well vacuum electric furnace thermal treatment (annealing) table look-up ")
￠12.0—￠11.0—￠10.0*—￠8.0—￠7.0—￠6.0—￠5.0*
Well vacuum electric furnace thermal treatment (annealing) table look-up
| Classification | State | Specification mm | Heating temperature DEG C | Soaking time | The type of cooling |
| Nickel-base alloy | Work in-process | ≥￠8 | 800-850 | >=40 minutes | Air cooling |
6, sour openpore material: after checking material mark, pickling tub submergence is put into by after loose for material bundle, pickling concentration is with the Weight computation of complex acid, with sulfuric acid immersion, salt acid rinse to white, pickling temperature 30-70 DEG C, pickling time 20-35 minute, the blank after pickling must embathe with high pressure water flushing wash clean, dry, and conveniently finds out surface crack.
Blank pickle solution proportioning:
| Pickle solution proportioning | Concentration % | Temperature DEG C | Time |
| HCL:HNO3:H2O=1:1: surplus | 15 | 30-50 | 10-20 |
| Pickle solution proportioning | Concentration % | Temperature DEG C | Time |
| H2SO4:HNO3:NaCl:H2O=4:1:1: surplus | 30 | 50-70 | 10-15 |
7, polishing deburring: check material surface situation, if any surface imperfection (as burr, foreskin, crackle), carry out reconditioning process with portable emery wheel, notes being with protection tool.
8, anneal: silk material enters in stove, stove, exit operates, in line in case silk material occurs buckling phenomenon or contact with furnace wall occurring abrading.Confirmation silk material clean surface, unlubricated dose of residual just can placing it in well annealing furnace carry out anneal, and temperature, at 800 DEG C-850 DEG C, is incubated 1-2 hour.
9, pickling test: with sulfuric acid immersion, salt acid rinse to white, pickling temperature 50-80 DEG C, pickling time 8-15 minute.Check material surface situation, carry out light pruning with portable emery wheel, require that the surface imperfection degree of depth is no more than 0.5mm.
| Pickle solution proportioning | Concentration % | Temperature DEG C | Time |
| HCL:HNO3:H2O=1:1: surplus | 15 | 30-50 | 3-15 |
| Pickle solution proportioning | Concentration % | Temperature DEG C | Time |
| H2SO4:HNO3:NaCl:H2O=4:1:1: surplus | 30 | 50-70 | 5-10 |
10, finish draw: (1), wire drawing skidding processing requirement: before operation, first puts into the lubricant (see table-1) prepared and lubricates, fully stir, coating uniform by parcel.Parcel after lubrication should evenly be spread out, carries out Exposure to Sunlight and dries or dry.
Join mold technique requirement: according to dimensional requirement, need select the mould of suitable pass, it is as follows to join mold technique standard:
Unit (mm) " * " represents annealing (annealing temperature is see " well vacuum electric furnace process (annealing) table look-up ")
￠4.0—￠3.0—￠2.5—￠2.0*-￠1.48
￠4.0—￠3.0—￠2.5—￠1.8*—￠1.18
(2), finish draw: often draw next specification all to need to carry out pickling test, reconditioning process.Should tie up after the drawing of silk material is complete, handle with care, in order to avoid damage, scratch.
11, thermal treatment: be placed in well formula argon shield bright annealing oven by the silk material after cold drawn and heat-treat, thermal treatment temp is at 800 DEG C-850 DEG C, and insulation is air cooling after 1-2 hour, discharging.
The battery rivet pure nickel N6 that the present invention produces, we cannot accomplish odds and ends matter in process of production, so from raw material feed intake select purity be 99.99% Jinchuan Ni plate and Ultra-low carbon material, ZGHL0.25-250-1 type vacuum induction melting furnace is used effectively to improve purity and the uniform texture of steel alloy, improve the surface of steel ingot, inner quality, improve the performance of steel alloy, reduce the content of the elementary composition non-metallic inclusion of Al, O, Si, Ca, C etc. in steel and the gas content of H, O; Enter stokehold to clean production spare part, assemble and adjust, avoid forging as far as possible, produce folding in the operation of rolling or scratch, destroy product surface; Use well formula argon shield bright annealing oven to carry out deoxidation, crystal grain thinning, reduce or eliminate stress, expand the deflection of steel, unit elongation, relative reduction in area, preferably plasticity and higher toughness and intensity; The crackle forming cracking, by carrying out pickling repeatedly, reconditioning, annealing, drawing to blank, accomplishes surperficial zero-fault, the strong lumber recovery that ensure that pure nickel wire.Pure nickel N6 wire rod is by the effective control in production process, and inner and surperficial non-metallic inclusion significantly declines, and shown in the actual processing of client, its crackle production rate is less than 3.5%, belongs to high one-tenth section product.
Claims (1)
1. a production method of pure nickel N6, wherein, the mass percent of the composition in described pure nickel N6 is:
Nickel: >=99.5%, manganese :≤0.05%, magnesium :≤0.1%, silicon :≤0.1%, sulphur :≤0.005%, carbon :≤0.1%, phosphorus :≤0.002%;
The production method of described pure nickel N6, comprises the following steps:
1) vacuum melting: Ni plate and Ultra-low carbon furnace charge are loaded in vacuum induction melting furnace and carries out melting, when entering refining period after refining temperature 1600 DEG C to be achieved after fine melt, refining keeps at least 30 minutes, and the refining later stage turns rough vacuum, stir tapping in 1-3 minute, water injecting electrode;
2) esr: fluorite and titanium dioxide are prepared into striking agent by the mass ratio of 1:1, CaF2, Al2O3 and CaO are made remelting electroslag system, wherein, the mass percent of three is: CaF
2: 65%-75%, Al
2o
3: 15%-25%, CaO: surplus; Shove charge, striking slag making, smelting, feeding, cooling, make steel ingot base;
3) hammer cogging: steel ingot base is heated to 850 DEG C by room temperature, preheating 30-50 minute; Be warmed up to 1000-1150 DEG C, insulation 40-50 minute; Reach forging temperature, initial forging temperature >=1100 DEG C, final forging temperature >=950 DEG C;
4) hot-roll forming: material loads temperature≤600 DEG C of annealing furnace; Heating-up time >=120 minutes; Heating temperature 1000-1150 DEG C; Soaking time >=30 minute, begin to roll temperature >=1180 DEG C; Finishing temperature >=950 DEG C;
5) crin drawing: before operation, first carries out joining mould, carries out drawing process by deformation requirements;
6) sour openpore material: with sulfuric acid immersion, salt acid rinse to white, pickling temperature 50-80 DEG C, pickling time 20-30min;
7) polishing deburring: check material surface situation, and effects on surface defect carries out reconditioning process;
8) anneal: anneal temperature at 580 DEG C-600 DEG C, insulation 1-2 hour, below air cooling to 150 DEG C, discharging;
9) pickling test: with sulfuric acid immersion, salt acid rinse to white, pickling temperature 50-80 DEG C, pickling time 20-30min; Check material surface situation, pedestrian's work of going forward side by side reconditioning, requires that the surface imperfection degree of depth is no more than 0.5mm;
10) finish draw;
11) thermal treatment: thermal treatment temp is at 580 DEG C-600 DEG C, and insulation is after 1-2 hour below air cooling to 150 DEG C, discharging.
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|---|---|---|---|
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410255451.XA CN105177357A (en) | 2014-06-11 | 2014-06-11 | Production method of pure nickel N6 used for lithium battery rivets and having higher qualified product ratio |
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| CN105177357A true CN105177357A (en) | 2015-12-23 |
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ID=54899775
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108823431A (en) * | 2018-06-04 | 2018-11-16 | 沈阳屹辰科技有限公司 | A kind of preparation method of high-purity nickel wire |
| CN113293387A (en) * | 2021-05-28 | 2021-08-24 | 金川集团股份有限公司 | Drawing and pickling process for removing oxide skin of nickel/nickel alloy wire |
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|---|---|---|---|---|
| CN101748314A (en) * | 2008-11-28 | 2010-06-23 | 江苏龙鑫特殊钢实业总公司 | Nickel-based alloy of nuclear power steam generator |
| CN102732751A (en) * | 2012-06-18 | 2012-10-17 | 江苏新华合金电器有限公司 | Anti-vibration alloy material for nuclear power station steam generator and preparation process thereof |
| CN103103381A (en) * | 2011-11-14 | 2013-05-15 | 王云华 | Production method of elastic alloy material |
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2014
- 2014-06-11 CN CN201410255451.XA patent/CN105177357A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101748314A (en) * | 2008-11-28 | 2010-06-23 | 江苏龙鑫特殊钢实业总公司 | Nickel-based alloy of nuclear power steam generator |
| CN103103381A (en) * | 2011-11-14 | 2013-05-15 | 王云华 | Production method of elastic alloy material |
| CN102732751A (en) * | 2012-06-18 | 2012-10-17 | 江苏新华合金电器有限公司 | Anti-vibration alloy material for nuclear power station steam generator and preparation process thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108823431A (en) * | 2018-06-04 | 2018-11-16 | 沈阳屹辰科技有限公司 | A kind of preparation method of high-purity nickel wire |
| CN113293387A (en) * | 2021-05-28 | 2021-08-24 | 金川集团股份有限公司 | Drawing and pickling process for removing oxide skin of nickel/nickel alloy wire |
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Application publication date: 20151223 |