CN110257745A - A kind of white tungsten wire and preparation method thereof - Google Patents

A kind of white tungsten wire and preparation method thereof Download PDF

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Publication number
CN110257745A
CN110257745A CN201910680942.1A CN201910680942A CN110257745A CN 110257745 A CN110257745 A CN 110257745A CN 201910680942 A CN201910680942 A CN 201910680942A CN 110257745 A CN110257745 A CN 110257745A
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tungsten wire
wire
silk
independently
temperature
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CN110257745B (en
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徐福生
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Liaoning dongdaihe New District Xingyuan Technology Co.,Ltd.
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Langfang Huaxing Tungsten Molybdenum Industry Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C1/00Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
    • B21C1/02Drawing metal wire or like flexible metallic material by drawing machines or apparatus in which the drawing action is effected by drums
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C51/00Measuring, gauging, indicating, counting, or marking devices specially adapted for use in the production or manipulation of material in accordance with subclasses B21B - B21F
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/52Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
    • C21D9/525Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length for wire, for rods
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00Electrolytic etching or polishing
    • C25F3/16Polishing
    • C25F3/22Polishing of heavy metals
    • C25F3/26Polishing of heavy metals of refractory metals

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Metal Extraction Processes (AREA)
  • Heat Treatment Of Strip Materials And Filament Materials (AREA)

Abstract

The present invention provides a kind of preparation methods of tungsten wire, belong to copying machines technical field.Preparation method of the invention, comprising the following steps: (1) tungsten wire precursor is successively put silk, annealing, attachment aquadag, heating, wire drawing and receives silk, obtains black tungsten wire;Repeat attachment aquadag, heating and drawing process n times;Wherein 4≤N≤12;The annealing opportunity be the N-4 times wire drawing after, before N-3 attachment aquadag;(2) the black tungsten wire that the step (1) obtains successively is subjected to continuous electrolysis and stress homogenizes, obtaining specification is the white tungsten wire of 28~420mg/200mm.By the parameter in optimum organization rate-determining steps (1), (2), obtained white tungsten wire for copying machines heating lamp core pulling coiling, without bar sizing when, tungsten wire deformation rate drops to 1% hereinafter, solving the defect of bar sizing simultaneously.20% or more production cost is reduced for heating lamp manufacturing enterprise.

Description

A kind of white tungsten wire and preparation method thereof
Technical field
The present invention relates to copying machines technical fields more particularly to a kind of white tungsten wire and preparation method thereof.
Background technique
Requirement due to copying machines manufacturer to heating lamp is very high, and in addition to photoelectricity index, vibration strength is the key that heating lamp Quality index, in the entire lifetime of heating lamp, the wire broken rate of heating lamp under the normal transport and use condition of copying machines It will be below a ten thousandth.Under this high request, even if the tungsten wire for selecting vibration strength best using existing bar method for shaping Material can not reach.The reason is that bar sizing can make filament generate brittle point, vibration strength is influenced.And be formed without bar then can be with for use Solve this problem.But no bar can be such that filament deforms when being formed, and to solve filament problem on deformation must just make tungsten wire production process The stress of the different directions of middle generation reaches consistent.In order to realize the purpose, the method that existing tungsten wire manufacturing enterprise generally uses Be: select top quality raw material the pulling process of black tungsten wire take select different annealing point even increase annealing times, It improves the methods of annealing temperature, extension annealing time and eliminates as much as the stress generated in pulling process;In white silk production process In some using electrolytic method, some using annealing in hydrogen atmosphere method, when using electrolytic method, by changing electrolyte prescription, dense The parameters such as degree, temperature, electric current, speed, electrolyte flow rate reduce polarization as far as possible.Though tungsten wire manufacturing enterprise is existing all to use these Method, but optimal combination is not all reached, qualification rate when tungsten wire produced being caused to be used for core pulling coiling, be formed without bar is most Height only 85%.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of white tungsten wires and preparation method thereof, using preparation of the invention The white tungsten wire that method obtains for copying machines heating lamp core pulling coiling, without bar sizing when, tungsten wire deformation rate drop to 1% with Under, while solving the defect of bar sizing.20% or more production cost is reduced for heating lamp manufacturing enterprise.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of white tungsten wire, comprising the following steps:
(1) tungsten wire precursor is successively put silk, annealing, attachment aquadag, heating, wire drawing and receives silk, obtains black tungsten wire;
Repeat attachment aquadag, heating and drawing process n times;
Wherein 4≤N≤12;
The annealing opportunity be the N-4 times wire drawing after, before N-3 attachment aquadag;
The tungsten wire precursor includes the Φ 0.39-0.60A for meeting W91 the or W61 trade mark specified in GB/T23272-2009 Grade material;
As N=4, the parameter in step (1) includes: to put a counter pull for 4.7~6.7g/mg, annealing temperature 1200 ~1300 DEG C, annealing time is 10~14s, and four schungite cream Baume degrees independently are 5.0, and four times heating temperature independently is 900~1000 DEG C, the temperature of four wire drawing dies independently is 350~370 DEG C, and four wire drawing compression ratios independently are 20~ 22%, drawing speed is 8~12m/min, and receipts silk torque is 1.1~1.3Nm;The specification of the black tungsten wire be 185~ 460mg/200mm, tensile strength are 2000~2150N/mm2, other inspections meet national standard qualification index;
(2) the black tungsten wire that the step (1) obtains successively is subjected to continuous electrolysis and stress homogenizes, obtain white tungsten wire, institute The specification for stating white tungsten wire is 165~420mg/200mm, and tensile strength is 2080~2230N/mm2
Preferably, as N=5 or 6, the parameter in the step (1) includes: to put a counter pull for 5.0~7.0g/mg, Annealing temperature is 1200~1300 DEG C, and annealing time is 8~11s, and five times or six times aquadag Baume degrees independently are 5.0, Five times or six heating temperatures independently are 800~900 DEG C, and the temperature of five times or six times wire drawing dies independently is 350~370 DEG C, five times or six times wire drawing compression ratios independently are 18~21%, and drawing speed is 13~17m/min, and receiving silk torque is 0.8 ~1.0Nm;The specification of the black tungsten wire is 125~180mg/200mm, and tensile strength is 2120~2200N/mm2, Qi Taxiang Inspection meets national standard qualification index;
The black tungsten wire successively carries out continuous electrolysis and stress homogenizes, and obtains white tungsten wire;The specification of the white tungsten wire is 105 ~165mg/200mm, tensile strength are 2230~2310N/mm2
Preferably, as N=7 or 8, the parameter of the step (1) includes;Putting a counter pull is 6.0~8.0g/mg, is moved back Fiery temperature is 1250~1350 DEG C, and annealing time is 6.0~7.5s;Seven times or eight schungite cream Baume degrees independently 5.0, seven times Or eight heating temperatures independently are 750~850 DEG C, the temperature of seven times or eight times wire drawing dies independently is 350~370 DEG C, Seven times or eight times wire drawing compression ratios independently are 17~20%, and drawing speed is 18~22m/min, receive silk torque be 0.4~ 0.6N·m;The specification of the black tungsten wire is 95~125mg/200mm, and tensile strength is 2190~2270N/mm2, other inspections It tests and meets national standard qualification index;
The black tungsten wire successively carries out continuous electrolysis and stress homogenizes, and obtains white tungsten wire;The specification of the white tungsten wire is 80 ~105mg/200mm, tensile strength are 2230~2380N/mm2
Preferably, when N=9,10,11 or 12, when four times after repetition attachment aquadag, heating, wire drawing, the step (1) parameter include: put a counter pull be 6.0~8.0g/mg, annealing temperature be 1250~1350 DEG C, annealing time be 4~ 5.5s, latter four times aquadag Baume degrees independently are 3.5, and rear four heating temperatures independently are 600~620 DEG C, and rear four The temperature of secondary wire drawing die independently is 380~420 DEG C, and latter four times wire drawing compression ratios independently are 17~19%, wire drawing speed Degree is 23~30m/min, and receipts silk torque is 0.25~0.35Nm;The specification of the black tungsten wire is 38~95mg/200mm, is resisted Tensile strength is 2270~2500N/mm2, other inspections meet national standard qualification index;
The black tungsten wire successively carries out continuous electrolysis and stress homogenizes, and obtains white tungsten wire;The specification of the white tungsten wire is 28 ~80mg/200mm, tensile strength are 2380~2570N/mm2
Preferably, the continuous electrolysis includes four electrolytic processes.
Preferably, it is NaOH and H that the once electrolytic procedure parameter, which includes: electrolyte,2O is mixed by weight 11:100, Electrolyte temperature is 20~35 DEG C, and electrolyte flow rate is 17~23L/min, and electric current is 9~11A, and receipts silk speed is 14~17m/ Min, putting a counter pull is 3.7~4.3g/mg;
Re-electrolysis procedure parameter includes: that electrolyte is NaOH and H2O is mixed by weight 11:100, and electrolyte temperature is 20~35 DEG C, 17~23L/min of electrolyte flow rate, electric current is 10~17A, and receipts silk speed is 14~17m/min, puts a counter pull For 3.7~4.3g/mg;
It is NaOH and H that electrolytic process parameter, which includes: electrolyte, three times2O is mixed by weight 7:100, and electrolyte temperature is 20~35 DEG C, electrolyte flow rate is 17~23L/min, and electric current is 10~17A, and receipts silk speed is 9~17m/min, puts a reverse drawing Power is 3.7~4.3g/mg;
Four electrolytic process parameters include: that electrolyte is NaOH and H2O is mixed by weight 7:100, and electrolyte temperature is 20~35 DEG C, electrolyte flow rate is 17~23L/min, and electric current is 25~30A, and receipts silk speed is 6~17m/min, puts a reverse drawing Power is 3.7~4.3g/mg.
Preferably, the homogenized wet hydrogen annealing temperature of the stress be 1200~1300 DEG C, dry hydrogen annealing temperature be 1400~ 1500 DEG C, putting a counter pull is 2.7~3.3g/mg, and receipts silk speed is 2~12m/min.
The present invention also provides the white tungsten wire being prepared described in above-mentioned technical proposal, the tensile strength of the white tungsten wire is 2000~2600N/mm2
Silk, annealing, attachment aquadag, heating, wire drawing are successively put the present invention provides (1) tungsten wire precursor and receives silk, are obtained To black tungsten wire;Repeat attachment aquadag, heating and drawing process n times;Wherein 4≤N≤12;The annealing opportunity is the N-4 times After wire drawing, before N-3 attachment aquadag;The tungsten wire precursor includes meeting W91 or W61 specified in GB/T23272-2009 0.39-0.60A grades of materials of Φ of the trade mark;The specification that black tungsten wire is obtained after n times wire drawing is 38~460mg/200mm, tension Intensity is 2000~2600N/mm2, other inspections meet national standard qualification index;(2) the black tungsten wire for obtaining the step (1) It successively carries out continuous electrolysis and stress homogenizes, obtain white tungsten wire, the specification of the white tungsten wire is 28~420mg/200mm, tension Intensity is 2000~2600N/mm2.The present invention passes through the specification of strict control tungsten wire precursor, the counter pull for putting silk, aquadag wave U.S. degree, heating temperature, wire-drawing temperature, wire drawing compression ratio, drawing speed, torque, the annealing temperature, annealing time for receiving silk, obtain The black tungsten wire haveing excellent performance;Processing is homogenized in conjunction with electrolysis and stress, so that the stress of tungsten wire becomes smaller, is obtained satisfactory white Tungsten wire.The white tungsten wire tensile strength that the present invention obtains is 2000~2600N/mm2;The core pulling for copying machines heating lamp around When making, being formed without bar, tungsten wire deformation rate drops to 1% hereinafter, solving the defect of bar sizing simultaneously.For heating lamp manufacturing enterprise drop Low 20% or more production cost.
Detailed description of the invention
Fig. 1 is wire-drawing frame schematic diagram;
Fig. 2 is continuous electrolysis schematic device;
Fig. 3 is TO furnace high temperature stress homogenizer schematic diagram.
Specific embodiment
The present invention provides a kind of preparation methods of white tungsten wire, comprising the following steps:
(1) tungsten wire precursor is successively put silk, annealing, attachment aquadag, heating, wire drawing and receives silk, obtains black tungsten wire;
Repeat attachment aquadag, heating and drawing process n times;
Wherein 4≤N≤12;
The annealing opportunity be the N-4 times wire drawing after, before N-3 attachment aquadag;
The tungsten wire precursor includes the Φ 0.39-0.60A for meeting W91 the or W61 trade mark specified in GB/T23272-2009 Grade material;
As N=4, the parameter in step (1) includes: to put a counter pull for 4.7~6.7g/mg, annealing temperature 1200 ~1300 DEG C, annealing time is 10~14s, and four schungite cream Baume degrees independently are 5.0, and four times heating temperature independently is 900~1000 DEG C, the temperature of four wire drawing dies independently is 350~370 DEG C, and four wire drawing compression ratios independently are 20~ 22%, drawing speed is 8~12m/min, and receipts silk torque is 1.1~1.3Nm;The specification of the black tungsten wire be 185~ 460mg/200mm, tensile strength are 2000~2150N/mm2, other inspections meet national standard qualification index;
(2) the black tungsten wire that the step (1) obtains successively is subjected to continuous electrolysis and stress homogenizes, obtain white tungsten wire, institute The specification for stating white tungsten wire is 165~420mg, and tensile strength is 2080~2230N/mm2
Tungsten wire precursor is successively put silk, annealing, attachment aquadag, heating, wire drawing and receives silk by the present invention, obtains black tungsten Silk;Repeat attachment aquadag, heating and drawing process n times.In the present invention, 4≤N≤12.In the present invention, when the annealing Machine be the N-4 times wire drawing after, before N-3 attachment aquadag.
In the present invention, as N=4, the annealing opportunity is that tungsten wire precursor is directly annealed after putting silk;Tungsten after annealing Silk precursor repeats attachment aquadag-heating-drawing process 4 times, receives silk and obtains black tungsten wire.
In the present invention, the counter pull for putting silk be 4.7~6.7g/mg, preferably 5.0~6.5g/mg, more preferably 5.5~6.0g/mg.In the present invention, a counter pull of putting keeps tungsten wire precursor to enter the stability of wire-drawing die, to subtract The generation of small irregular stress.
In the present invention, the annealing temperature is 1200~1300 DEG C, preferably 1220~280 DEG C, more preferably 1240 ~1260 DEG C;The annealing time is 10~14s, preferably 11~13s, more preferably 11.5~12.5s.In the present invention, The annealing can eliminate black tungsten wire internal stress, it is ensured that final white tungsten wire quality.
In the present invention, 4 schungite cream Baume degrees independently are 5.0.In the present invention, the aquadag plays lubrication and makees With, it is ensured that tungsten wire precursor can pass through wire-drawing die under the effect of lesser deformation force.
In the present invention, 4 heating temperatures independently are 900~1000 DEG C, preferably 920~980 DEG C, more preferably 940~960 DEG C.In the present invention, the heating can dry the aquadag adhered on tungsten wire precursor, and reach tungsten wire precursor To 600 DEG C of plastic deformation temperatures or more, the quality of black tungsten wire is improved.
In the present invention, the temperature of 4 wire drawing dies independently is 350~370 DEG C, preferably 355~365 DEG C, more preferably It is 358~362 DEG C;4 wire drawing compression ratios independently are 20~22%, preferably 20.5~21.5%, more preferably 20.8~ 21.2%;Drawing speed is 8~12m/min, preferably 9~11m/min, more preferably 9.5~10.5m/min.In the present invention In, wire drawing can draw and attenuate tungsten wire precursor, obtain the satisfactory black tungsten wire of each index.
In the present invention, the receipts silk torque be 1.1~1.3Nm, preferably 1.15~1.25Nm, more preferably 1.18~1.22Nm.In the present invention, the receipts silk can ensure that black tungsten wire has certain tension, and can be avoided curly wire And silk pressing.In the present invention, as N=4, the black tungsten wire specification that the step (1) obtains is 185~460mg/200mm, tension Intensity is 2000~2150N/mm2, other inspections meet national standard qualification index.
In the present invention, as N=5, the annealing opportunity is that tungsten wire precursor is put silk, once adheres to aquadag, is primary After heating, a wire drawing;It anneals;After tungsten wire precursor after annealing repeats attachment aquadag-heating-drawing process 4 times, receive Silk obtains black tungsten wire: as N=6, the annealing opportunity is that tungsten wire precursor is put silk, repeats attachment aquadag-heating-wire drawing After journey 2 times;It anneals;Tungsten wire precursor after annealing repeats attachment aquadag-heating-drawing process 4 times, and receipts silk obtains black Tungsten wire.In the present invention, as N=5 or 6, in addition to annealing opportunity is different, the other parameters range of choice in step (1) is identical. Specifically: the counter pull for putting silk is preferably 5.0~7.0g/mg, more preferably 5.5~6.5g/mg, most preferably 5.8~ 6.2g/mg。
In the present invention, annealing temperature is preferably 1200~1300 DEG C, and more preferably 1220~1280 DEG C, most preferably 1240~1260 DEG C;Annealing time is preferably 8~11s, more preferably 8.5~10.5s, most preferably 9.0~10.0s.
In the present invention, 5 times or 6 times aquadag Baume degrees are independently preferably 5.0.
In the present invention, independently preferably 800~900 DEG C of 5 times or 6 times heating temperatures, more preferably 820~880 DEG C, most preferably 840~860 DEG C.
In the present invention, independently preferably 350~370 DEG C of 5 times or 6 times wire drawing die temperature, more preferably 355~ 365 DEG C, most preferably 358~362 DEG C;5 times or 6 wire drawing compression ratios are independently preferably 18~21%, more preferably 18.5 ~20.5%, most preferably 19~20%;Drawing speed is preferably 13~17m/min, more preferably 14~16m/min, optimal It is selected as 14.5~15.5m/min.
In the present invention, the torque for receiving silk is preferably 0.8~1.0Nm, more preferably 0.85~0.98Nm, most Preferably 0.9~0.95Nm.In the present invention, as N=5 or 6, the specification for the black tungsten wire that the step (1) obtains is 125 ~180mg/200mm, tensile strength are 2120~2200N/mm2, other inspections meet national standard qualification index.
In the present invention, as N=7, the annealing opportunity is that tungsten wire precursor is put silk, repeats to adhere to aquadag-heating- After drawing process 3 times;It anneals;Tungsten wire precursor after annealing repeats attachment aquadag-heating-drawing process 4 times, receives silk and obtains To black tungsten wire.As N=8, the annealing opportunity is that tungsten wire precursor is put silk, repeats to adhere to aquadag-heating-drawing process 4 After secondary;It anneals;Tungsten wire precursor after annealing repeats attachment aquadag-heating-drawing process 4 times, receives silk and obtains black tungsten wire. In the present invention, as N=7 or 8, in addition to annealing opportunity is different, the other parameters range of choice in step (1) is identical.Specifically Are as follows: a counter pull of putting is preferably 6.0~8.0g/mg, more preferably 6.5~7.5g/mg, most preferably 6.8~7.2g/ mg。
In the present invention, the annealing temperature is preferably 1250~1350 DEG C, and more preferably 1270~1330 DEG C, most preferably It is 1290~1310 DEG C;The annealing time is preferably 6~7.5s, more preferably 6.2~7.3s, most preferably 6.5~7.0s.
In the present invention, 7 times or 8 times aquadag Baume degrees are independently preferably 5.0.
In the present invention, independently preferably 750~850 DEG C of 7 times or 8 times heating temperatures, more preferably 770~830 DEG C, most preferably 790~820 DEG C.
In the present invention, independently preferably 350~370 DEG C of 7 times or 8 times wire drawing die temperature, more preferably 355~ 365 DEG C, most preferably 358~362 DEG C;7 times or 8 times wire drawing compression ratios are independently preferably 17~20%, more preferably 18 ~19%, most preferably 18.4~18.8%;Drawing speed is preferably 18~22m/min, more preferably 19~21m/min, most Preferably 19.5~20.5m/min.
In the present invention, the receipts silk torque is preferably 0.4~0.6Nm, and more preferably 0.45~0.55Nm is optimal It is selected as 0.48~0.52Nm.In the present invention, as N=7 or 8, the specification of the black tungsten wire that the step (1) obtains is 95~ 125mg/200mm, tensile strength are 2190~2270N/mm2, other inspections meet national standard qualification index.
In an embodiment of the present invention, the wire-drawing frame of use can only carry out 8 wire drawings, so as 4≤N≤8, one 8 wire drawings can be completed in a wire-drawing frame.As 9≤N≤12, need two wire-drawing frames that could complete wire drawing.In this hair In bright, preferably carry out putting silk in the first wire-drawing frame, repeat to adhere to aquadag-heating-wire drawing N-4 times, receive silk and obtain black tungsten wire; 4 wire drawings are carried out in the second wire-drawing frame;The black tungsten wire obtained after N-4 wire drawing is vertical once putting silk in the second wire-drawing frame It anneals, then repeats attachment aquadag-heating-drawing process 4 times, received silk and obtain black tungsten wire.
In the present invention, when N=9,10,11,12, attachment aquadag-heating-wire drawing is repeated in the first wire-drawing frame Process is respectively 5 times, 6 times, 7 times and 8 times.Attachment aquadag-heating-drawing process 5 times or 6 times are repeated in the first wire-drawing frame When, the parameter of the step (1) is identical as the parameter selection of step (1) when N=5 or 6;It is repeatedly attached in the first wire-drawing frame Aquadag-heating-wire drawing 7 times or at 8 times, the parameter of the step (1), the parameter selection model with step (1) when N=7 or 8 It encloses identical.
In the present invention, when N=9,10,11 or 12, attachment aquadag-heating-wire drawing is repeated in the second wire-drawing frame After process at 4 times, the parameter area selection in the step (1) is identical;Specifically: it is described put a counter pull be preferably 6.0~ 8.0g/mg, more preferably 6.5~7.5g/mg, most preferably 6.8~7.2g/mg.
In the present invention, the annealing temperature is preferably 1250~1350 DEG C, and more preferably 1280~1330 DEG C, most preferably It is 1290~1320 DEG C;The annealing time is preferably 4.0~5.5s, more preferably 4.2~5.2s, most preferably 4.5~ 5.0s。
In the present invention, latter 4 times aquadag Baume degrees are independently preferably 3.5.
In the present invention, independently preferably 600~620 DEG C of rear 4 heating temperatures, more preferably 605~615 DEG C, Most preferably 608~613 DEG C.
In the present invention, independently preferably 380~420 DEG C of latter 4 times wire drawing die temperature, more preferably 390~410 DEG C, most preferably 395~405 DEG C;Afterwards 4 wire drawing compression ratios independently be preferably 17~19%, more preferably 17.4~ 18.6%, most preferably 17.5~18.5%;The drawing speed is preferably 23~30m/min, more preferably 25~28m/ Min, most preferably 26~27m/min.
In the present invention, the receipts silk torque is preferably 0.25~0.35Nm, more preferably 0.27~0.33Nm, most Preferably 0.29~0.31Nm.
In the present invention, latter N-8 times aquadag Baume degrees is independently preferably 3.5.
In the present invention, independently preferably 600~620 DEG C of latter N-8 times heating temperature, more preferably 605~615 DEG C, most preferably 608~613 DEG C.
In the present invention, independently preferably 380~420 DEG C of the temperature of rear N-8 wire drawing die, more preferably 390~410 DEG C, most preferably 395~405 DEG C;The N-8 wire drawing compression ratio is independently preferably 16~19% afterwards, more preferably 16.5~18.5%, most preferably 17~18%;The drawing speed is preferably 32~45m/min, more preferably 35~43m/ Min, most preferably 38~40m/min.
In the present invention, the torque for receiving silk is preferably 0.1~0.2Nm, more preferably 0.12~0.18Nm, most Preferably 0.14~0.16Nm.In the present invention, when N=9,10,11 or 12, black tungsten wire that the step (1) obtains Specification is 38~95mg/200mm, and tensile strength is 2270~2500N/mm2, other inspections meet national standard qualification index.
In the present invention, the tungsten wire precursor includes the Φ for meeting W91 the or W61 trade mark specified in GB/T23272-2009 0.39-0.60A grades of materials.
In the present invention, the tensile strength of the black tungsten wire is preferably 2000~2600N/mm2.The present invention is to step (1) Number of repetition there is no special restriction, as long as the wire drawing of tungsten wire precursor, at the black tungsten wire of desired size, and tensile strength is 2000 ~2600N/mm2?.
Tungsten wire precursor is preferably prepared by black tungsten wire using wire-drawing frame in an embodiment of the present invention.In the present invention, The wire-drawing frame is as shown in Figure 1.In Fig. 1: 1 puts silk device for tungsten wire: containing putting guide frame, counter pull device;2 be tungsten wire precursor, 3 It is aquadag slot for eight guide wheel group of tower, 4,5 be heating furnace, and 6 be electric heating mould bases, the mould that can put eight wire drawing dies simultaneously Tool, 7 be eight passage pulling wheel of tower, and 8 is receive silk, bus cable device, and 9 be combustion gas annealing furnace.In the present invention, the tungsten wire precursor Silk device 1 is put by tungsten wire and puts silk, is poured out through eight guide wheel 3 of tower, adheres to aquadag into aquadag slot 4, heating furnace 5 will adhere to stone The tungsten wire precursor heating of black cream, while the aquadag being attached on tungsten wire precursor being dried;Tungsten wire precursor after heating, into electricity The mold 6 heated on mould bases carries out wire drawing;Tungsten wire precursor after wire drawing leads eight guide wheel 3 of tower through eight passage pulling wheel 7 of tower In, again through on aquadag slot 4, heating furnace 5, electric heating mould bases mold 6 and tower pulling wheel 7 enter eight guide wheel 3 of tower in, Number of repetition is determined as needed;After obtaining the black tungsten wire of target size, is received silk, bus cable device 8 and collected black tungsten wire;Combustion gas is moved back Stove 9 be it is moveable, those skilled in the art according to annealing opportunity, combustion gas annealing furnace 9 is put into specified position.
After obtaining black tungsten wire, the black tungsten wire is successively carried out continuous electrolysis to the present invention and stress homogenizes, and obtains white tungsten wire.
In the present invention, the continuous electrolysis preferably includes four electrolytic processes.In the present invention, the electrolytic process is excellent Choosing includes that black tungsten wire is put to silk, electrolysis, neutralization, cleaning, dehydration, drying and receives silk, obtains white tungsten wire.
In the present invention, the electrolyte of the once electrolytic process is preferably NaOH and H2O is mixed by weight 11:100. In the present invention, the electrolyte temperature of once electrolytic process is preferably 20~35 DEG C, more preferably 23~33 DEG C, most preferably 25 ~30 DEG C.In the present invention, the electrolyte flow rate of the once electrolytic process is preferably 17~23L/min, more preferably 18~ 22L/min, most preferably 19~21L/min.In the present invention, the electric current of the once electrolytic process is preferably 9~11A, more Preferably 9.5~10.5A, most preferably 9.8~10.2A.In the present invention, the receipts silk speed of the once electrolytic process is preferred For 14~17m/min, more preferably 14.5~16.5m/min, most preferably 15~16m/min.In the present invention, described primary A counter pull of putting for electrolytic process is preferably 3.7~4.3g/mg, more preferably 3.8~4.2g/mg, most preferably 3.9~ 4.1g/mg。
In the present invention, the electrolyte of the re-electrolysis process is preferably NaOH and H2O is by weight 11:100.At this In invention, the electrolyte temperature of the re-electrolysis process is preferably 20~35 DEG C, more preferably 23~33 DEG C, most preferably 25 ~30 DEG C.In the present invention, the electrolyte flow rate of the re-electrolysis process is preferably 17~23L/min, more preferably 18~ 22L/min, most preferably 19~21L/min.In the present invention, the electric current of the re-electrolysis process is preferably 10~17A, more Preferably 12~16A, most preferably 14~15A.In the present invention, the receipts silk speed of the re-electrolysis process be preferably 14~ 17m/min, more preferably 15.5~16.5m/min, override are 15.8~16.2m/min.In the present invention, the secondary electricity A counter pull of putting for solution preocess is preferably 3.7~4.3g/mg, more preferably 3.8~4.2g/mg, most preferably 3.9~4.1g/ mg。
In the present invention, the electrolyte of the electrolytic process three times is preferably NaOH and H2O is mixed by weight 7:100. In the present invention, the electrolyte temperature of the electrolytic process three times is preferably 20~35 DEG C, and more preferably 23~32 DEG C, most preferably It is 25~30 DEG C.In the present invention, the electrolyte flow rate of the electrolytic process three times is preferably 17~23L/min, more preferably 18~22L/min, most preferably 19~21L/min.In the present invention, the electric current of the electrolytic process three times be preferably 10~ 17A, more preferably 12~16A, most preferably 13~15A.In the present invention, the receipts silk speed of the electrolytic process three times is preferred For 9~17m/min, more preferably 11~15m/min, most preferably 12~14m/min.In the present invention, described to put silk three times Counter pull be preferably 3.7~4.3g/mg, more preferably 3.8~4.2g/mg, most preferably 3.9~4.1g/mg.
In the present invention, the electrolyte of four electrolytic processes is preferably NaOH and H2O is mixed by weight 7:100. In the present invention, the electrolyte temperature of four electrolytic processes is preferably 20~35 DEG C, and more preferably 23~33 DEG C, most preferably It is 25~30 DEG C.In the present invention, the electrolyte flow rate of four electrolytic processes is preferably 17~23L/min, more preferably 18~22L/min, most preferably 19~21L/min.In the present invention, the electric current of four electrolytic processes be preferably 25~ 30A, more preferably 26~29A, most preferably 27~28A.In the present invention, the receipts silk speed of four electrolytic processes is preferred For 6~17m/min, more preferably 8~15m/min, more preferable 10~12m/min.In the present invention, four electrolytic processes A counter pull of putting be preferably 3.7~4.3g/mg, more preferably 3.8~4.2g/mg, most preferably 3.9~4.1g/mg.
The present invention restriction not special to neutralization, cleaning, dehydration and the drying in the electrolytic process, using this field Operation known to technical staff, specifically, the black tungsten wire after four electrolysis is in oxalic acid: in water=3L:100L solution into Row neutralizes, and is cleaned using city tap-water, is dehydrated using the dehydrated alcohol of purity >=95%, is dried at 300~400 DEG C.
The device that the present invention uses continuous electrolysis does not have special restriction, using well known to those skilled in the art continuous Electrolysis unit.In embodiments of the present invention, the continuous electrolysis apparatus structure of use is as shown in Figure 2.In Fig. 2: 1 puts for tungsten wire Silk mechanism, counter pull regulating mechanism, 2 be 10~20 groups of electrolytic cells, and 3 be electrolyte separating tube, and 4 be neutralization chamber, and 5 clean for water purification Slot, 6 be dehydration slot, and 7 be drying unit, and 8 receive silk, wire-arranging mechanism for adjustable speed, and 9 be black tungsten wire.In the present invention, the black tungsten Silk puts silk through tungsten wire thread supplying machine structure, counter pull adjustment structure 1;Into in electrolytic cell 2, it is electrolysed;Subsequently into neutralization chamber 4 into Row neutralizes, and subsequently enters water purification rinse bath 5 and is cleaned;Dehydration slot 6 is subsequently entered to be dehydrated;Subsequently enter drying unit 7 Drying receives silk, the receipts silk of cable structure 8 through adjustable speed, obtains being electrolysed white tungsten wire.
In the present invention, electrolysis can remove the impurity such as graphitic lubricant, the oxide of black tungsten filament, while can change The roughness of kind tungsten filament keeps tungsten wire clean bright.In the present invention, the tensile strength of the tungsten wire after electrolysis is preferably 2000 ~2600N/mm2
It obtains after being electrolysed white tungsten wire, the present invention will be electrolysed white tungsten wire progress stress and homogenize, and obtain white tungsten wire.In the present invention In, the stress homogenize preferably include to be electrolysed white tungsten wire put silk, wet hydrogen annealing, dry hydrogen annealing and receive silk.In the present invention, The wet hydrogen annealing temperature is preferably 1200~1300 DEG C, more preferably 1220~1280 DEG C, most preferably 1240~1260 DEG C. In the present invention, the wet hydrogen annealing can remove the impurity of tungsten filament, reduce stress.In the present invention, the dry hydrogen moves back Fiery temperature is preferably 1400~1500 DEG C, more preferably 1420~1480 DEG C, most preferably 1440~1460 DEG C.In the present invention In, it is the protection of 99.999 dry hydrogens that the dry hydrogen, which is annealed into the white tungsten wire of electrolysis by purity, and non-contact 360 ° of electricity add in circle molybdenum tube Heat reduces tungsten wire stress.In the present invention, a counter pull of putting is preferably 2.7~3.3g/mg, more preferably 2.8~ 3.2g/mg, most preferably 2.9~3.1g/mg.In the present invention, the speed for receiving silk is preferably 2~12m/min, more preferably For 4~10m/min, most preferably 6~8m/min.In the present invention, the time of the wet hydrogen annealing and dry hydrogen return of goods annealing is equal It is determined by receipts silk speed.
Preferably stress is carried out using TO furnace high temperature stress homogenizer in an embodiment of the present invention to homogenize.In the present invention In, the TO furnace high temperature stress homogenizer structure is as shown in Figure 3.In Fig. 3: 1 is tungsten wire actinobacillus device, counter pull adjusts dress It sets, 2 is are electrolysed white tungsten wire, and 3 be wet hydrogen annealing furnace, and 4 be dry hydrogen annealing furnace, and 5 fill to receive silk speed guide wheel, 6 for receipts silk, winding displacement It sets.In the present invention, the white tungsten wire of electrolysis puts silk through tungsten wire actinobacillus device, reverse drawing apparatus for adjusting force 1;Into wet hydrogen annealing furnace 3 anneal;Dry hydrogen annealing furnace 4 is subsequently entered to anneal;It is received silk speed guide wheel 5 and receives silk, the white tungsten that annealing is obtained Silk, which is packed into, receives silk, bus cable device 6.
In the present invention, the stress homogenizes the stress that can eliminate tungsten wire different directions, reduces tungsten wire in application Disqualification rate.
The present invention also provides the white tungsten wires that preparation method described in above-mentioned technical proposal obtains.In the present invention, described white The tensile strength of tungsten wire is 2000~2600N/mm2;For copying machines heating lamp core pulling coiling, without bar sizing when, white tungsten wire Deformation rate drops to 1% hereinafter, solving the defect of bar sizing simultaneously.20% or more production is reduced for heating lamp manufacturing enterprise Cost.
White tungsten wire provided by the invention and preparation method thereof is described in detail below with reference to embodiment, but cannot They are interpreted as limiting the scope of the present invention.
Embodiment 1
The diameter of tungsten wire precursor is 0.50mm
A kind of preparation method of white tungsten wire, comprising the following steps:
(1) tungsten wire precursor is successively put silk, annealing, attachment aquadag, heating, wire drawing and receives silk, obtains black tungsten wire;It repeats Adhere to aquadag-heating-drawing process 4 times;
The annealing opportunity is that tungsten wire precursor is directly annealed after putting silk, after annealing;Attachment aquadag-is repeated to add It heat-wire drawing four times, is received silk and obtains black tungsten wire;
Parameter in step (1) includes: to put a counter pull for 5.5g/mg, annealing temperature is 1250 DEG C, and annealing time is 12.8s, four schungite cream Baume degrees independently are 5.0, and four heating temperatures independently are 950 DEG C, and four times wire drawing die temperature is only It is on the spot 360 DEG C, four wire drawing compression ratios independently are 20~22%, drawing speed 12m/min, and receipts silk torque is 1.1N m;Obtaining specification is the black tungsten wire of 295 ± 3mg/200mm, tested for tensile strength 2043N/mm2, examine for other and meet national standard conjunction Lattice index.
(2) the black tungsten wire that the step (1) obtains successively is subjected to continuous electrolysis and stress homogenizes, obtain tungsten wire;
The continuous electrolysis include four electrolytic processes: the once electrolytic procedure parameter include: electrolyte be NaOH and H2O 11:100 in mass ratio mixing, electrolyte temperature are 25 DEG C, electrolyte flow rate 20L/min, electric current 10A, receive silk speed For 17m/min, putting a counter pull is 4g/mg;
Re-electrolysis procedure parameter includes: that electrolyte is NaOH and H2O 11:100 in mass ratio mixing, electrolyte temperature are 25 DEG C, electrolyte flow rate 20L/min, electric current 12A, receipts silk speed is 17m/min, and putting a counter pull is 4g/mg;
It is NaOH and H that electrolytic process parameter, which includes: electrolyte, three times2O 7:100 in mass ratio mixing, electrolyte temperature are 25 DEG C, electrolyte flow rate 20L/min, electric current 15A, receipts silk speed is 17m/min, and putting a counter pull is 4g/mg;
Four electrolytic process parameters include: that electrolyte is NaOH and H2O 7:100 in mass ratio mixing, electrolyte temperature are 25 DEG C, electrolyte flow rate 20L/min, electric current 30A, receipts silk speed is 8m/min, and putting a counter pull is 4g/mg;It is advised Lattice are that 270 ± 2mg/200mm is electrolysed white tungsten wire.Tested for tensile strength is 2270N/mm2
The homogenized wet hydrogen annealing temperature of stress is 1250 DEG C, and wet hydrogen annealing time is 7.5s, and dry hydrogen annealing temperature is 1400 DEG C, dry hydrogen annealing time is 7.5s, and putting a counter pull is 3.0g/mg, and receipts silk speed is 4m/min.
Using the Appendix B method in GB/T23272-2009, the tensile strength of the white tungsten wire of gained is measured, as a result are as follows: white tungsten The tensile strength of silk is 2195N/mm2.Other inspections meet national standard qualification index.
Embodiment 2
The diameter of tungsten wire precursor is 0.39mm
A kind of preparation method of white tungsten wire, comprising the following steps:
(1) tungsten wire precursor is successively put silk, annealing, attachment aquadag, heating, wire drawing and receives silk, obtains black tungsten wire;It repeats Adhere to aquadag-heating-drawing process 6 times;The black tungsten wire that specification is 125 ± 1.5mg/200mm is obtained, measurement gained tungsten wire Tensile strength is 2230N/mm2, other inspections meet national standard qualification index.The annealing opportunity is tungsten wire precursor through putting silk Afterwards, it after repeating attachment aquadag-heating-drawing process 2 times, anneals, after annealing, repeats to adhere to aquadag-heating-wire drawing It 4 times, receives silk and obtains black tungsten wire;
Parameter in step (1) includes: to put a counter pull as 6g/mg, and 6 schungite cream Baume degrees independently are 5.0,6 times Heating temperature independently is 850 DEG C, and 6 wire drawing die temperature independently are 360 DEG C, and 6 wire drawing compression ratios independently are 18~ 21%, drawing speed 17m/min, receipts silk torque are 0.8Nm;Annealing temperature is 1280 DEG C, annealing time 8.6s.
(2) the black tungsten wire that the step (1) obtains successively is subjected to continuous electrolysis and stress homogenizes, obtain white tungsten wire;
The continuous electrolysis include four electrolytic processes: the once electrolytic procedure parameter include: electrolyte be NaOH and H2O 11:100 in mass ratio mixing, electrolyte temperature are 25 DEG C, electrolyte flow rate 20L/min, electric current 9A, receive silk speed For 17m/min, putting a counter pull is 4g/mg;
Re-electrolysis procedure parameter includes: that electrolyte is NaOH and H2O 11:100 in mass ratio mixing, electrolyte temperature are 25 DEG C, electrolyte flow rate 20L/min, electric current 10A, receipts silk speed is 17m/min, and putting a counter pull is 4g/mg;
It is NaOH and H that electrolytic process parameter, which includes: electrolyte, three times2O 7:100 in mass ratio mixing, electrolyte temperature are 25 DEG C, electrolyte flow rate 20L/min, electric current 10A, receipts silk speed is 17m/min, and putting a counter pull is 4g/mg;
Four electrolytic process parameters include: that electrolyte is NaOH and H2O 7:100 in mass ratio mixing, electrolyte temperature are 25 DEG C, electrolyte flow rate 20L/min, electric current 25A, receipts silk speed is 17m/min, and putting a counter pull is 4g/mg.It is advised Lattice are the white tungsten wire of electrolysis of 115 ± 1mg/200mm;Tested for tensile strength is 2340N/mm2
The homogenized wet hydrogen annealing temperature of stress is 1200 DEG C, and wet hydrogen annealing time is 3.75s, and dry hydrogen annealing temperature is 1450 DEG C, dry hydrogen annealing time is 3.75s, and putting a counter pull is 3g/mg, and receipts silk speed is 8m/min.
Using the Appendix B method in GB/T23272-2009, the tensile strength of the white tungsten wire of gained is measured, as a result are as follows: white tungsten The tensile strength of silk is 2230N/mm2;Other inspections meet national standard qualification index.
Embodiment 3
The diameter of tungsten wire precursor is 0.39mm
A kind of preparation method of white tungsten wire, comprising the following steps:
(1) tungsten wire precursor is successively put silk, annealing, attachment aquadag, heating, wire drawing and receives silk, obtains black tungsten wire;It repeats Adhere to aquadag-heating-drawing process 10 times;Obtaining specification is the black tungsten wire of 63 ± 1.0mg/200mm, the black tungsten wire of measurement gained Tensile strength is 2410N/mm2, other inspections meet national standard qualification index.
Since wire drawing number has been more than 8 times, so needing to carry out wire drawing in two wire-drawing frames;In the first wire-drawing frame Six wire drawings of middle progress, obtaining specification is the black tungsten wire of 157 ± 2mg/200mm, and the tensile strength of measurement gained tungsten wire is 2570N/ mm2, other inspections meet national standard qualification index;Four wire drawings after being carried out in the second wire-drawing frame again;The annealing opportunity To anneal immediately after putting silk in the second wire-drawing frame, attachment aquadag-heating-wire drawing 4 times is then repeated, silk is received and obtains To black tungsten wire;
Parameter in step (1) include: the first wire-drawing frame put a counter pull be 7g/mg, the six of the first wire-drawing frame Schungite cream Baume degrees independently is 5.0, and six heating temperatures independently are 850 DEG C, and six wire drawing die temperature are independently It is 360 DEG C, six wire drawing compression ratios independently are 18~21%, drawing speed 17m/min, and receipts silk torque is 0.8Nm;It moves back Fiery temperature is 1300 DEG C, annealing time 4.1s, and four schungite cream Baume degrees of the second wire-drawing frame independently are 3.5, four times Heating temperature independently is 600 DEG C, and four wire drawing die temperature independently are 400 DEG C, and four wire drawing compression ratios independently are 17~ 19%, drawing speed 27m/min, receipts silk torque are 0.3Nm;
(2) the black tungsten wire that the step (1) obtains successively is subjected to continuous electrolysis and stress homogenizes, obtain tungsten wire;
The continuous electrolysis include four electrolytic processes: the once electrolytic procedure parameter include: electrolyte be NaOH and H2O 11:100 in mass ratio mixing, electrolyte temperature are 25 DEG C, electrolyte flow rate 20L/min, electric current 9A, receive silk speed For 17m/min, putting a counter pull is 4g/mg;
Re-electrolysis procedure parameter includes: that electrolyte is NaOH and H2O 11:100 in mass ratio mixing, electrolyte temperature are 25 DEG C, electrolyte flow rate 20L/min, electric current 10A, receipts silk speed is 17m/min, and putting a counter pull is 4g/mg;
It is NaOH and H that electrolytic process parameter, which includes: electrolyte, three times2O 7:100 in mass ratio mixing, electrolyte temperature are 25 DEG C, electrolyte flow rate 20L/min, electric current 10A, receipts silk speed is 17m/min, and putting a counter pull is 4g/mg;
Four electrolytic process parameters include: that electrolyte is NaOH and H2O 7:100 in mass ratio mixing, electrolyte temperature are 25 DEG C, electrolyte flow rate 20L/min, electric current 25A, receipts silk speed is 17m/min, and putting a counter pull is 4g/mg;It is advised Lattice are that 55 ± 0.5mg/200mm is electrolysed white tungsten wire;Tested for tensile strength is 2530N/mm2
The homogenized wet hydrogen annealing temperature of stress is 1200 DEG C, and wet hydrogen annealing time is 2.5s, and dry hydrogen annealing temperature is 1450 DEG C, dry hydrogen annealing time is 2.5s, and putting a counter pull is 3g/mg, and receipts silk speed is 12m/min.
Using the Appendix B method in GB/T23272-2009, the tensile strength of the white tungsten wire of measurement gained, result is white tungsten wire Tensile strength be 2380N/mm2
From embodiment it can be seen that the present invention is by the parameter in strict control step (1), and combines continuous electrolysis and answer Power homogenizes parameter, so that the tensile strength of white tungsten wire is 2000~2600N/mm2, the core pulling for copying machines heating lamp around When making, being formed without bar, tungsten wire deformation rate drops to 1% hereinafter, reducing by 20% or more production cost for heating lamp manufacturing enterprise.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (9)

1. a kind of preparation method of white tungsten wire, comprising the following steps:
(1) tungsten wire precursor is successively put silk, annealing, attachment aquadag, heating, wire drawing and receives silk, obtains black tungsten wire;
Repeat attachment aquadag, heating and drawing process n times;
Wherein 4≤N≤12;
The annealing opportunity be the N-4 times wire drawing after, before N-3 attachment aquadag;
The tungsten wire precursor includes the 0.39-0.60A grades of materials of Φ for meeting W91 the or W61 trade mark specified in GB/T23272-2009 Material;
(2) the black tungsten wire that the step (1) obtains successively is subjected to continuous electrolysis and stress homogenizes, obtain white tungsten wire;It is described white The specification of tungsten wire is 28~420mg/200mm.
2. preparation method according to claim 1, which is characterized in that as N=4, the parameter in step (1) includes: to put Silk counter pull is 4.7~6.7g/mg, and annealing temperature is 1200~1300 DEG C, and annealing time is 10~14s, four schungite cream waves U.S. degree independently is 5.0, and four heating temperatures independently are 900~1000 DEG C, and the temperature of four wire drawing dies independently is 350~ 370 DEG C, four wire drawing compression ratios independently are 20~22%, and drawing speed is 8~12m/min, receive silk torque be 1.1~ 1.3N·m;The specification of the black tungsten wire is 185~460mg/200mm, and tensile strength is 2000~2150N/mm2, other inspections It tests and meets national standard qualification index;
The black tungsten wire successively carries out continuous electrolysis and stress homogenizes, and obtains white tungsten wire;The specification of the white tungsten wire be 165~ 420mg/200mm, tensile strength are 2080~2230N/mm2
3. preparation method according to claim 1, which is characterized in that the parameter as N=5 or 6, in the step (1) Include: put a counter pull be 5.0~7.0g/mg, annealing temperature be 1200~1300 DEG C, annealing time be 8~11s, five times or Six aquadag Baume degrees independently are 5.0, and five times or six heating temperatures independently are 800~900 DEG C, five times or six times The wire drawing compression ratio that the temperature of wire drawing die independently is 350~370 DEG C, five times or six times independently is 18~21%, wire drawing speed Degree is 13~17m/min, and receipts silk torque is 0.8~1.0Nm;The specification of the black tungsten wire is 125~180mg/200mm, is resisted Tensile strength is 2120~2200N/mm2, other inspections meet national standard qualification index;
The black tungsten wire successively carries out continuous electrolysis and stress homogenizes, and obtains white tungsten wire;The specification of the white tungsten wire be 105~ 165mg/200mm, tensile strength are 2230~2310N/mm2
4. preparation method according to claim 1, which is characterized in that as N=7 or 8, the parameter packet of the step (1) It includes;Putting a counter pull is 6.0~8.0g/mg, and annealing temperature is 1250~1350 DEG C, and annealing time is 6.0~7.5s;Seven times or Eight schungite cream Baume degrees independently 5.0, seven times or eight times heating temperatures independently are 750~850 DEG C, seven times or eight times drawings The wire drawing compression ratio that the temperature of silk mould independently is 350~370 DEG C, seven times or eight times independently is 17~20%, drawing speed For 18~22m/min, receipts silk torque is 0.4~0.6Nm;The specification of the black tungsten wire is 95~125mg/200mm, and tension is strong Degree is 2190~2270N/mm2, other inspections meet national standard qualification index;
The black tungsten wire successively carries out continuous electrolysis and stress homogenizes, and obtains white tungsten wire;The specification of the white tungsten wire be 80~ 105mg/200mm, tensile strength are 2230~2380N/mm2
5. preparation method according to claim 1, which is characterized in that when N=9,10,11 or 12, repeat to adhere to graphite When four times after cream, heating, wire drawing, the parameter of the step (1) includes: to put a counter pull for 6.0~8.0g/mg, annealing temperature It is 1250~1350 DEG C, annealing time is 4~5.5s, and latter four times aquadag Baume degrees independently are 3.5, rear four heating Temperature independently is 600~620 DEG C, and the temperature of rear four wire drawing dies independently is 380~420 DEG C, latter four times wire drawing pressures Than independently being 17~19%, drawing speed is 23~30m/min for contracting, and receipts silk torque is 0.25~0.35Nm;The black tungsten The specification of silk is 38~95mg/200mm, and tensile strength is 2270~2500N/mm2, examine for other and meet national standard qualification and refer to Mark;
The black tungsten wire successively carries out continuous electrolysis and stress homogenizes, and obtains white tungsten wire;The specification of the white tungsten wire be 28~ 80mg/200mm, tensile strength are 2380~2570N/mm2
6. described in any item preparation methods according to claim 1~5, which is characterized in that the continuous electrolysis includes four electricity Solution preocess.
7. preparation method according to claim 6, which is characterized in that the once electrolytic procedure parameter includes: electrolyte For NaOH and H2O is mixed by weight 11:100, and electrolyte temperature is 20~35 DEG C, and electrolyte flow rate is 17~23L/min, electricity Stream is 9~11A, and receipts silk speed is 14~17m/min, and putting a counter pull is 3.7~4.3g/mg;
Re-electrolysis procedure parameter includes: that electrolyte is NaOH and H2O by weight 11:100 mix, electrolyte temperature be 20~ 35 DEG C, 17~23L/min of electrolyte flow rate, electric current is 10~17A, and receipts silk speed is 14~17m/min, and putting a counter pull is 3.7~4.3g/mg;
It is NaOH and H that electrolytic process parameter, which includes: electrolyte, three times2O is mixed by weight 7:100, and electrolyte temperature is 20~35 DEG C, electrolyte flow rate is 17~23L/min, and electric current is 10~17A, and receipts silk speed is 9~17m/min, and putting a counter pull is 3.7 ~4.3g/mg;
Four electrolytic process parameters include: that electrolyte is NaOH and H2O is mixed by weight 7:100, and electrolyte temperature is 20~35 DEG C, electrolyte flow rate is 17~23L/min, and electric current is 25~30A, and receipts silk speed is 6~17m/min, and putting a counter pull is 3.7 ~4.3g/mg.
8. preparation method according to claim 1 or claim 7, which is characterized in that the homogenized wet hydrogen annealing temperature of stress is 1200~1300 DEG C, dry hydrogen annealing temperature is 1400~1500 DEG C, and putting a counter pull is 2.7~3.3g/mg, and receiving silk speed is 2 ~12m/min.
9. the white tungsten wire that any one of claim 1~8 preparation method obtains, which is characterized in that the tension of the white tungsten wire Intensity is 2000~2600N/mm2
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116984404A (en) * 2023-07-28 2023-11-03 浙江创特新材科技有限公司 Movable multi-section thin tungsten wire heating module and high-strength thin tungsten wire drawing equipment
CN117960814A (en) * 2024-03-28 2024-05-03 赣州市光华有色金属有限公司 Drawing process for cutting bus fine tungsten wire

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5954416A (en) * 1982-09-24 1984-03-29 Toshiba Corp Manufacture of tungsten wire
JP3569182B2 (en) * 1999-11-24 2004-09-22 株式会社東芝 Tungsten material for secondary processing
JP3769008B2 (en) * 2005-09-07 2006-04-19 株式会社東芝 Tungsten material for secondary processing
CN101547757A (en) * 2007-03-15 2009-09-30 联合材料公司 Diamond dice and method for producing wire using diamond dice
CN101868306A (en) * 2007-11-21 2010-10-20 株式会社东芝 The manufacture method of tungsten filament
CN102755784A (en) * 2011-04-27 2012-10-31 江苏大维管线有限公司 Stainless microfilament used for filtering, and production method thereof
JP5086503B2 (en) * 2001-02-02 2012-11-28 株式会社東芝 Method for manufacturing thorium tungsten wire
CN104438390A (en) * 2014-11-26 2015-03-25 北京矿冶研究总院 Double-wire drawing method of rare earth tungsten electrode material
CN107685079A (en) * 2017-07-26 2018-02-13 东北大学 Pure titanium or titanium alloy ultrafine wire preparation technology
CN109402719A (en) * 2018-12-14 2019-03-01 西安瑞福莱钨钼有限公司 A kind of preparation method of tungsten narrowband foil
CN109622641A (en) * 2018-12-19 2019-04-16 苏州全佳金属制品有限公司 A kind of efficient stainless steel wire drawing technique

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5954416A (en) * 1982-09-24 1984-03-29 Toshiba Corp Manufacture of tungsten wire
JP3569182B2 (en) * 1999-11-24 2004-09-22 株式会社東芝 Tungsten material for secondary processing
JP5086503B2 (en) * 2001-02-02 2012-11-28 株式会社東芝 Method for manufacturing thorium tungsten wire
JP3769008B2 (en) * 2005-09-07 2006-04-19 株式会社東芝 Tungsten material for secondary processing
CN101547757A (en) * 2007-03-15 2009-09-30 联合材料公司 Diamond dice and method for producing wire using diamond dice
CN101868306A (en) * 2007-11-21 2010-10-20 株式会社东芝 The manufacture method of tungsten filament
CN102755784A (en) * 2011-04-27 2012-10-31 江苏大维管线有限公司 Stainless microfilament used for filtering, and production method thereof
CN104438390A (en) * 2014-11-26 2015-03-25 北京矿冶研究总院 Double-wire drawing method of rare earth tungsten electrode material
CN107685079A (en) * 2017-07-26 2018-02-13 东北大学 Pure titanium or titanium alloy ultrafine wire preparation technology
CN109402719A (en) * 2018-12-14 2019-03-01 西安瑞福莱钨钼有限公司 A kind of preparation method of tungsten narrowband foil
CN109622641A (en) * 2018-12-19 2019-04-16 苏州全佳金属制品有限公司 A kind of efficient stainless steel wire drawing technique

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116984404A (en) * 2023-07-28 2023-11-03 浙江创特新材科技有限公司 Movable multi-section thin tungsten wire heating module and high-strength thin tungsten wire drawing equipment
CN116984404B (en) * 2023-07-28 2024-04-26 浙江创特新材科技有限公司 Movable multi-section thin tungsten wire heating module and high-strength thin tungsten wire drawing equipment
CN117960814A (en) * 2024-03-28 2024-05-03 赣州市光华有色金属有限公司 Drawing process for cutting bus fine tungsten wire
CN117960814B (en) * 2024-03-28 2024-06-11 赣州市光华有色金属有限公司 Drawing process for cutting bus fine tungsten wire

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