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.
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 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.