CN105274428A - Production method for alloy filament with zero defect on surface - Google Patents

Production method for alloy filament with zero defect on surface Download PDF

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Publication number
CN105274428A
CN105274428A CN201410255380.3A CN201410255380A CN105274428A CN 105274428 A CN105274428 A CN 105274428A CN 201410255380 A CN201410255380 A CN 201410255380A CN 105274428 A CN105274428 A CN 105274428A
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temperature
wire rod
annealing
pickling
time
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荆正伟
钟静
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Danyang Kaixin Alloy Material Co Ltd
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Danyang Kaixin Alloy Material Co Ltd
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Abstract

The invention discloses a 4J42 alloy filament for a discharge tube electrode and a production method for the alloy filament. The production method comprises the following steps: pouring a 4J42 raw material into a vacuum furnace for making steel and forming an ingot; performing forging cogging and hot rolling to form a wire rod; performing acid washing processing on the wire rod subjected to hot rolling; polishing and trimming after acid washing, and performing first drawing; performing annealing processing on a semi-finished product subjected to first drawing; performing acid washing and grinding on the semi-finished product subjected to annealing processing; performing secondary drawing after no crack is determined to exist; performing hot-processing annealing on the wire rod subjected to secondary drawing; detecting the case of the wire rod surface again, performing crude-filament finish drawing, performing hot processing after each time of the wire rod being drawn and entering a next specification, and stopping untie the wire rod reaches the finished-product dimension. According to the technical scheme, based on the real demands on the discharge tube electrode, various factors influencing 4J42 plasticity and rolling yield during production are researched and found, and the defects that 4J42 is bad in plasticity, low in rolling yield and the like in the subsequent processing process are solved by improving the 4J42 production technology.

Description

A kind of production method of surperficial zero-fault B alloy wire
Technical field
The present invention relates to the manufacture method of 4J42 B alloy wire, be specifically related to a kind of production method of discharge tube electrode 4J42 B alloy wire of surperficial zero-fault.
Background technology
4J42 alloy belongs to the expansion alloy in Precise Alloy, and nickel content is about 42%, and all the other are mainly iron, and (under normal temperature, average coefficient of expansion is 1.6X10 to have stable low-expansion coefficient -6/ DEG C), have a wide range of applications in aerospace, precision instrument, electron trade, its main application is for producing discharge tube electrode.Discharge tube is used for protecting communication system, traffic signal system, computer data system and the external cable of various electronics, the safe operation of electronic machine.Also do not have other material can replace this traditional vacuum seal material at present.Although the 4J42 market requirement is huge, the quality product fluctuation of most domestic producer is comparatively large, makes it in following process, occur the defects such as plasticity is poor, lumber recovery is low, thus causes the high-end market of domestic discharge tube to be captured by external producer for a long time.Production process as the 4J42 B alloy wire of raw material is an important process link, can impact to a great extent to the quality of the finished product.But the systematic study that there is no at present the special 4J42 B alloy wire production technique for the effective electrode cap of tele-release, this directly affects science and the reasonableness of this product processes.Present system have studied the every factor affecting 4J42 plasticity and lumber recovery in process of production, by the improvement to 4J42 production process, solve it in following process, occur the defects such as plasticity is poor, lumber recovery is low, reduce the production loss of discharge tube, improve the advantage of China in discharge tube market.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of production method of electrode 4J42 B alloy wire, improve or eliminate steel cast, forge, the folding or scuffing of the generation that causes in the process such as rolling, avoid destroying product surface and eliminating unrelieved stress, improve plasticity difference and the cracking probability of finished silk material in process of manufacture, and realize surperficial zero-fault.
For solving the problems of the technologies described above, the invention provides a kind of discharge tube electrode 4J42 B alloy wire, the mass percent of it each chemical composition comprised is: nickel: 40-45%, manganese :≤0.8%, silicon :≤0.3%, phosphorus :≤0.02%, carbon :≤0.05%, sulphur :≤0.02%, cobalt :≤1.0%, iron: surplus.
The production method of above-mentioned discharge tube electrode 4J42 B alloy wire, comprises the steps:
Vacuum melting → esr → forge cogging → hot-roll forming → sour game of shuttlecocks mill → first time drawing → anneal → pickling test → second time drawing → anneal → disk peeling → finish draw → thermal treatment, wherein:
1) vacuum melting: by Ni plate, Co sheet, Si, Mn, Ultra-low carbon technical pure Fe 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 1580 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), high-power stirring tapping in 5 minutes, waters injecting electrode;
2) esr: be that the fluorite of 1:1 to 1:1.2 and titanium dioxide prepare striking agent, by CaF with mass ratio 2, Al 2o 3be in harmonious proportion with CaO and make remelting electroslag system, wherein, the mass percent of three is: CaF 2: 70%-75%, Al 2o 3: 20%-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 of use improves purity and the uniform texture of steel alloy effectively, improves the surface of steel ingot, inner quality, improves the performance of steel alloy.
3) hammer cogging: (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, rear bang of taking the circumstances into consideration is improved 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, avoid producing hammering and folding, failure surface.
4) dish is rolled into: material loads the temperature of annealing furnace :≤600 DEG C; Heating-up time >=120 minutes; Heating temperature: 1000-1150 DEG C; Soaking time: >=30 minutes, begins to roll temperature: >=1180 DEG C; Finishing temperature >=950 DEG C;
Described hot rolling very easily produces scuffing defect, tiny crack, the defect such as folding, easily cause occurring the phenomenons such as stress accumulation, fracture of wire when following process, so blank enters stokehold reply, production spare part is assembled and adjusted, import and export guide and guard must be in the same horizontal line, and keep optimum distance with roll, to avoid the generation of above phenomenon.
5) sour game of shuttlecocks mill: with sulfuric acid immersion, salt acid rinse to white, pickling temperature 50-80 DEG C, pickling time 20-30min; Check material surface situation, and effects on surface defect carries out reconditioning process;
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.Check material surface situation after pickling, if any surface imperfection (as burr, foreskin, crackle), carry out reconditioning process with portable emery wheel.
6) first time drawing: before operation, first carry out joining mould, carry out drawing process by deformation requirements glomerocryst mould;
Described 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
7) anneal: work in-process are placed in pit type annealing furnace and carry out anneal, temperature, at 800 DEG C-850 DEG C, is incubated 1-2 hour;
8) 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, carry out artificial reconditioning with portable emery wheel, require that the surface imperfection degree of depth is no more than 0.5mm;
9) second time drawing: second time continuous drawing is carried out to the dish circle after reconditioning;
10) anneal: work in-process are placed in pit type annealing furnace and carry out anneal, temperature, at 800 DEG C-850 DEG C, is incubated 1-2 hour;
11) disk peeling: to the work in-process employing dish circle peeling after anneal to eliminate its surface oxide layer;
12) 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;
13) 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, goes out finished product.
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 4J42 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 adopts above technical scheme, have the following advantages and positively effect: the deficiency that the production for former discharge tube electrode 4J42 B alloy wire exists, vacuum induction melting furnace is adopted 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; By deoxidation, crystal grain thinning process, expand the deflection of steel, unit elongation, relative reduction in area, preferably plasticity and higher toughness and intensity; Steel ingot enters that stove forges, assemble production spare part and adjust before rolling, avoids producing folding in process or scratching, destroys product surface, form the crackle of cracking.The round peeling of 4J42 work in-process dish is improved to the surface quality of alloy, simultaneously pickling repeatedly, reconditioning, annealing, drawing, accomplish surperficial zero-fault as far as possible.
Embodiment
A production method for discharge tube electrode 4J42 B alloy wire, concrete steps are as follows:
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 DEG C to be achieved after fine melt, refining keeps at least 30 minutes;
(4), cast: the refining later stage turns rough vacuum (103-10-1Pa), and 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 should clear up surface before starting and in process 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, 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.
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, sour game of shuttlecocks mill: 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.Check material surface situation, if any surface imperfection (as burr, foreskin, crackle), carry out reconditioning process with portable emery wheel, note being with protection tool.
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
6, first time drawing: before operation, first carry out joining mould, operates by the following method:
(1), wire drawing skidding processing requirement: before operation, first parcel is put into the lubricant (see table-1) prepared and lubricate, fully stir, coating uniform.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
7, 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;
8) 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, carry out artificial reconditioning 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
9) second time drawing: second time continuous drawing is carried out to the dish circle after reconditioning;
10) anneal: again work in-process are placed in pit type annealing furnace and carry out anneal, temperature, at 800 DEG C-850 DEG C, is incubated 1-2 hour;
11) disk peeling: to the work in-process employing dish circle peeling after anneal to eliminate its surface oxide layer;
12) 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.
13) 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, goes out finished product.
The technical superiority of the production method of the discharge tube electrode 4J42 B alloy wire that the present invention produces is mainly manifested in following several respects:
(1) purity and the surface quality of 4J42 material is improved
Adopt vacuum induction melting furnace 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; 4J42P blank enters that stove forges, assemble production spare part and adjust before rolling, avoids producing folding in process or scratching, destroys product surface, form the crackle of cracking; Carry out coiling round peeling after second time Drawing-anneal, carrying out filament finish draw, improve the homogeneity of the specification of product, improve length and the quality of a material.
(2) improve mechanical property and the weave construction of silk material, improve the processing characteristics of product
Rational control annealing thermal treatment and thermal treatment, improve or eliminate steel cast, forge, the various tissues that cause in the process such as rolling lack and unrelieved stress, and crystal grain thinning, and pass through deoxidation, crystal grain thinning process.Expand the deflection of steel, prevent stress concentration, thus reduce the cracking probability of 4J42 in pressing process, larger deflection can be born, there is larger unit elongation, relative reduction in area, preferably plasticity and higher toughness and intensity.

Claims (1)

1. a production method for 4J42 B alloy wire, is characterized in that: the mass percent of each chemical composition that described B alloy wire comprises is:
Nickel: 40-45%, manganese :≤0.8%, silicon :≤0.3%, carbon :≤0.05%, cobalt :≤1.0%, iron: surplus;
The production method of above-mentioned B alloy wire, comprises the following steps:
1) vacuum melting: by Ni plate, Co sheet, Si, Mn, Fe after baking, load in vacuum induction melting furnace and carry out melting, when after refining temperature more than 1580 DEG C to be achieved after fine melt, refining at least 30 minutes, the refining later stage turns rough vacuum, stirs tapping in 5 minutes, waters injecting electrode;
2) esr: prepare striking agent, by CaF in the ratio of 1:1 to 1:1.2 with fluorite and titanium dioxide 2, Al 2o 3be in harmonious proportion with CaO and make remelting electroslag system, wherein, the mass percent of three is: CaF 2: 70%-75%, Al 2o 3: 20%-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) dish is rolled into: material loads the temperature of annealing furnace :≤600 DEG C; Heating-up time >=120 minutes; Heating temperature: 1000-1150 DEG C; Soaking time: >=30 minutes, begins to roll temperature: >=1180 DEG C; Finishing temperature >=950 DEG C;
5) sour game of shuttlecocks mill: with sulfuric acid immersion, salt acid rinse to white, pickling temperature 50-80 DEG C, pickling time 20-30min; Check material surface situation, and effects on surface defect carries out reconditioning process;
6) first time drawing: before operation, first carry out joining mould, carry out drawing process by deformation requirements glomerocryst mould;
7) anneal: annealing temperature, at 800 DEG C-850 DEG C, is incubated 1-2 hour;
8) 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, carry out artificial reconditioning, require that the surface imperfection degree of depth is no more than 0.5mm;
9) second time drawing: second time continuous drawing is carried out to the dish circle after reconditioning;
10) anneal: anneal temperature, at 800 DEG C-850 DEG C, is incubated 1-2 hour;
11) disk peeling: to the work in-process employing dish circle peeling after anneal, to eliminate its surface oxide layer;
12) finish draw;
13) thermal treatment: thermal treatment temp is at 800 DEG C-850 DEG C, and insulation is air cooling after 1-2 hour, goes out finished product.
CN201410255380.3A 2014-06-11 2014-06-11 Production method for alloy filament with zero defect on surface Pending CN105274428A (en)

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Publication number Priority date Publication date Assignee Title
CN107030127A (en) * 2017-05-27 2017-08-11 京仪股份有限公司 A kind of copper bar drawing process
CN110280619A (en) * 2019-05-21 2019-09-27 江苏图南合金股份有限公司 A kind of high temperature alloy bar silk material preparation method
CN112044965A (en) * 2020-08-21 2020-12-08 南通市华星钢丝制品有限公司 Method for rapidly preparing 5G communication wire material based on drawing process
CN114855070A (en) * 2021-02-03 2022-08-05 上海梅山钢铁股份有限公司 Cold-rolled electroplated tin steel plate with surface black and gray grade of 1 grade and manufacturing method thereof
CN113732101A (en) * 2021-08-31 2021-12-03 东风商用车有限公司 Fine wire for high-temperature alloy GH4080A cold heading and preparation method thereof
CN113732101B (en) * 2021-08-31 2023-09-19 东风商用车有限公司 Fine wire for high-temperature alloy GH4080A cold heading and preparation method thereof

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