CN114888292A - Preparation method of high-strength superfine tungsten alloy wire for cutting - Google Patents
Preparation method of high-strength superfine tungsten alloy wire for cutting Download PDFInfo
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- CN114888292A CN114888292A CN202210508823.XA CN202210508823A CN114888292A CN 114888292 A CN114888292 A CN 114888292A CN 202210508823 A CN202210508823 A CN 202210508823A CN 114888292 A CN114888292 A CN 114888292A
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- 229910001080 W alloy Inorganic materials 0.000 title claims abstract description 87
- 238000005520 cutting process Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 70
- 238000010438 heat treatment Methods 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 22
- 238000000137 annealing Methods 0.000 claims abstract description 18
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 13
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 11
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005498 polishing Methods 0.000 claims abstract description 11
- 238000002844 melting Methods 0.000 claims abstract description 10
- 230000008018 melting Effects 0.000 claims abstract description 10
- 229910052702 rhenium Inorganic materials 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 239000012266 salt solution Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 28
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 21
- 238000004321 preservation Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 17
- 230000009467 reduction Effects 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 14
- 229910052721 tungsten Inorganic materials 0.000 claims description 12
- 239000010937 tungsten Substances 0.000 claims description 12
- 238000005242 forging Methods 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 230000007547 defect Effects 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 238000000462 isostatic pressing Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 229910003460 diamond Inorganic materials 0.000 abstract description 21
- 239000010432 diamond Substances 0.000 abstract description 21
- 239000011159 matrix material Substances 0.000 abstract description 13
- 238000005491 wire drawing Methods 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 5
- FAYUQEZUGGXARF-UHFFFAOYSA-N lanthanum tungsten Chemical compound [La].[W] FAYUQEZUGGXARF-UHFFFAOYSA-N 0.000 description 21
- 229910000691 Re alloy Inorganic materials 0.000 description 19
- 229910000858 La alloy Inorganic materials 0.000 description 18
- 230000006835 compression Effects 0.000 description 16
- 238000007906 compression Methods 0.000 description 16
- DECCZIUVGMLHKQ-UHFFFAOYSA-N rhenium tungsten Chemical compound [W].[Re] DECCZIUVGMLHKQ-UHFFFAOYSA-N 0.000 description 16
- 238000005516 engineering process Methods 0.000 description 12
- 229910000831 Steel Inorganic materials 0.000 description 10
- 239000010959 steel Substances 0.000 description 10
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 9
- 238000011049 filling Methods 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 7
- HRLYFPKUYKFYJE-UHFFFAOYSA-N tetraoxorhenate(2-) Chemical compound [O-][Re]([O-])(=O)=O HRLYFPKUYKFYJE-UHFFFAOYSA-N 0.000 description 7
- 238000005303 weighing Methods 0.000 description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 5
- 229910052750 molybdenum Inorganic materials 0.000 description 5
- 239000011733 molybdenum Substances 0.000 description 5
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of a high-strength superfine tungsten alloy wire for cutting, which comprises the following steps: lanthanum or rhenium is added to pure tungsten powder or acid-washed tungsten powder in the form of its salt solution, then in H 2 Roasting and reducing under the atmosphere to obtain tungsten alloy powder; pressing tungsten alloy powder into a tungsten alloy round bar billet, and then performing presintering; performing vertical melting, cogging, rotary swaging and thick and thin wire drawing on the pre-sintered tungsten alloy round bar billet to obtain a tungsten alloy thin wire with the diameter of 10-60 um; and then carrying out continuous annealing heat treatment on the tungsten alloy filaments with the diameters of 10-60 um, and finally carrying out electrolytic polishing to obtain the high-strength superfine tungsten alloy filaments which can be applied to the diamond wire saw matrix filaments for cutting the crystal materials, wherein the diameters of the high-strength superfine tungsten alloy filaments are 10-60 um, and the room-temperature tensile strength is not less than 5000 MPa.
Description
Technical Field
The invention belongs to the technical field of tungsten material manufacturing, and particularly relates to a preparation method of a high-strength superfine tungsten alloy wire for cutting.
Background
In the technical field of crystal material processing, a method for cutting monocrystalline silicon is a diamond wire saw and a cutting technology. The diamond wire saw consists of a matrix steel wire and a diamond wear-resistant layer coated on the surface of the matrix steel wire, wherein the diameter of the matrix steel wire is 150-450 um, and the thickness of a diamond particle coating is 5-20 um. The mechanism of the diamond wire saw cutting technology is that the diamond wear-resistant coating and the monocrystalline silicon of a workpiece are ground mutually, the cutting of the monocrystalline silicon rod is realized, the thickness of the silicon wafer is 2mm, the cutting efficiency is high, no harmful substance is generated, and no pollution is caused to the environment. However, the wire diameter of the diamond wire saw is 150-500 μm, the loss of the cutting edge of the cut crystal is large, and especially, a single crystal silicon rod with the diameter not less than 2 inches needs to be cut by multiple cutters, the loss of the cutting edge is more serious, and the production cost is high. The diamond wire saw is mainly determined by the performance of the diamond wire saw matrix steel wire, namely when the strength of the steel wire is 5000-6000 MPa, the diameter of the steel wire is 150-450 um. Therefore, how to obtain the high-strength superfine diamond wire saw matrix wire is the key for reducing the blade loss.
Compared with the traditional diamond wire saw matrix steel wire, the conventional tungsten and tungsten alloy wire has the advantages of high melting point, good wear resistance and the like, the diameter of the tungsten wire can reach 20-100 mu m, the room-temperature tensile strength is 3000-4000 MPa, and the technical requirements on the performance of the diamond wire saw matrix wire for cutting the crystal material can not be met.
Disclosure of Invention
The invention aims to provide a preparation method of a high-strength superfine tungsten alloy wire for cutting, which adopts rare earth modification and doping technology and drawing technology, and can obtain a room-temperature high-strength superfine tungsten wire meeting the requirements of a diamond wire saw matrix after tungsten powder is doped with rare earth elements and a thick and thin wire drawing process is improved.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a high-strength superfine tungsten alloy wire for cutting comprises the following steps:
1) preparing materials: the high-strength superfine tungsten alloy wire comprises the following components in percentage by mass: 0.05-2% of lanthanum or 0-1% of rhenium, and the balance of tungsten; the tungsten adopts pure tungsten powder or acid-washing tungsten powder as a raw material, and the particle size is 1-3 um; the rare earth elements lanthanum and rhenium are doping elements;
2) doping: adding lanthanum and rhenium into pure tungsten powder or acid-washing tungsten powder in the form of salt solution; the method specifically comprises the following steps: weighing lanthanum nitrate and ammonium rhenate according to a proportion, putting the lanthanum nitrate and the ammonium rhenate into deionized water, uniformly stirring, completely dissolving the lanthanum nitrate and the ammonium rhenate at a constant temperature of 80-150 ℃, and then injecting the solution into a doping mixer to mix with pure tungsten powder or acid-washed tungsten powder;
3) reduction: mixing the mixture obtained in 2) in H 2 Roasting and reducing in the atmosphere to obtain tungsten alloy powder; after reduction treatment, the rare earth elements lanthanum and rhenium are uniformly attached to the surface of pure tungsten powder or acid-washed tungsten powder;
4) pressing a blank bar: preparing tungsten alloy round bar billet from the tungsten alloy powder obtained in the step 3) in an isostatic pressing mode;
5) pre-burning: pre-sintering a tungsten alloy round bar billet; the pre-sintering can improve the strength of the green body and avoid mechanical damage or fracture in the subsequent vertical melting process;
6) vertical melting: loading the pre-sintered tungsten alloy round bar billet into a vertical melting machine in H 2 Sintering the tungsten alloy round bar with the relative density not lower than 95% after heavy current in the atmosphere, wherein the diameter is 17.4-20 mm;
7) cogging: cogging a tungsten alloy round bar with the diameter of 17.4-20 mm to obtain a tungsten alloy rod with the diameter of 8.0-9.0 mm;
8) rotary swaging: performing rotary swaging on the tungsten alloy rod with the diameter of 8.0-9.0 mm to obtain the tungsten alloy rod with the diameter of 3.0-4.0 mm;
9) drawing the thick wire: drawing a tungsten alloy rod with the diameter of 3.0-4.0 mm to obtain a tungsten alloy thick wire with the diameter of 0.1-0.2 mm;
10) drawing the filaments: drawing a tungsten alloy thick wire with the diameter of 0.1-0.2 mm to obtain a tungsten alloy thin wire with the diameter of 10-60 mu m;
11) annealing treatment: carrying out continuous annealing heat treatment on tungsten alloy filaments with the diameters of 10-60 um by using a hydrogen tube type annealing furnace to eliminate internal stress;
12) electrolytic polishing: and the tungsten alloy wire is cleaned by continuous electrolytic polishing, so that the surface defects of the wire material are eliminated.
The high-strength superfine tungsten alloy wire which has high tensile strength at room temperature and can be applied to the diamond wire saw matrix wire for cutting crystal materials can be obtained by the method.
Furthermore, the diameter of the high-strength superfine tungsten alloy wire prepared by the preparation method is 10-60 um, and the tensile strength at room temperature is more than or equal to 5000 MPa.
Further, the purity of the pure tungsten powder in the step 1) is 99.99%, and the granularity is 1-3 um; the potassium content of the acid-washing tungsten powder is 10-100 ppm, and the granularity is 1-3 um.
Further, the roasting reduction temperature in the step 3) is 500-950 ℃, the heat preservation time is 5-7 h, and the tungsten alloy powder is obtained after being discharged from the furnace and passing through a 120-mesh sieve, wherein the particle size is 1-3 um.
Further, the pre-sintering in 5) is carried out in H 2 And (3) carrying out heat preservation for 1-2 h at 1000-1300 ℃ in the atmosphere.
Further, the medium and large current in the step 6) is 2500-3000A, and the heat preservation time is 20-30 min.
Further, in the cogging process of 7), the pass compression rate is 10-15%, the heating temperature is 1500-1600 ℃, and the temperature is kept for 20-30 min.
Further, in the 8) rotary calcining process, the pass compressibility is 10-15%, the heating temperature is 1300-1500 ℃, and the heat preservation time is 10-30 s.
Further, in the drawing process of the thick wire of 9), the pass compressibility is 15-35%, the heating temperature is 650-1000 ℃, and the drawing speed is 5-30 m/min.
Further, in the 10) filament drawing process, the pass compression rate is 15-25%, the heating temperature is 650-1000 ℃, and the drawing speed is 20-100 m/min.
Further, the annealing temperature of the 11) continuous annealing heat treatment is 1100-1300 ℃, the take-up speed is 10-15 m/min, and the hydrogen flow rate is 3L/min.
Further, the electrolytic voltage of the continuous electrolytic polishing in the step 12) is 10-50V, the concentration of the electrolytic alkali liquor is 10-15 wt%, and the take-up speed is 40-70 m/min.
Compared with the prior art, the invention has the beneficial effects that:
1. the technology of doping rare earth elements (lanthanum and rhenium) by using tungsten powder (pure tungsten powder or acid-washing tungsten powder) is utilized to replace the traditional blue tungsten rare earth element doping technology. The traditional blue tungsten doping rare earth element technology is that APT is firstly added in H 2 Reducing the alloy into blue tungsten under the atmosphere at 500-950 ℃, doping a salt solution of rare earth elements into blue tungsten powder, carrying out acid pickling to obtain rough-particle acid-pickled tungsten powder, and finally carrying out H treatment on the rough-particle acid-pickled tungsten powder 2 And carrying out secondary reduction at 500-950 ℃ in the atmosphere to obtain coarse-grained rare earth element-doped tungsten powder with the powder granularity of 10-20 mu m. The technology of doping rare earth elements in tungsten powder is to directly dope the salt solution of rare earth elements in tungsten powder in H 2 Reducing the tungsten powder into fine-particle and uniform rare earth element-doped tungsten powder at the temperature of 500-950 ℃ in the atmosphere. Compared with the traditional rare earth element doping technology, the tungsten powder rare earth element doping technology has three advantages: 1) only one-time reduction is carried out, the process flow is shortened, and the cost is reduced; 2) the tungsten powder pickling process is removed, no harmful substance is generated, and the pollution to the environment is avoided; 3) the rare earth element-doped tungsten powder has fine granularity of about 1-3 um and better uniformity.
2. And (3) improving and optimizing three key process parameters of pass compression ratio, heating temperature and drawing speed in the processes of drawing the thick wire in the step 9) and drawing the thin wire in the step 10), and obtaining the high-strength superfine tungsten alloy wire. Compared with the traditional drawing process, after the compression ratio is increased by 5-10%, the microscopic tungsten grains of the core part and the outer surface layer of the wire material after large deformation amount can be effectively controlled to have no obvious difference, and the grain size of the cross section is smaller, so that the room-temperature tensile strength of the superfine tungsten wire is improved; after the heating temperature is reduced by 10-20% and the drawing speed is increased by 50-100%, the recrystallization growth of fibrous tungsten grains can be effectively overcome, the problem of work hardening caused by large-deformation processing is also weakened, and the defects of cracking, wire breakage and the like of the superfine tungsten wire in the drawing process and the final product are avoided.
3. According to the invention, by adopting a tungsten powder rare earth element doping technology and a drawing process to improve and optimize, the diameter of the prepared high-strength superfine tungsten wire is only 10-60 um, the room-temperature tensile strength is not less than 5000MPa, the surface of the wire is smooth, and the defects of burrs, cracking and the like are avoided, so that the high-strength superfine tungsten wire can replace a matrix steel wire of a traditional diamond wire saw, and the blade loss of cutting of a single crystal silicon rod is greatly reduced.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is an SEM image of tungsten alloy powder obtained by the technique of doping lanthanum element with tungsten powder according to the present invention;
FIG. 3 is an SEM image of tungsten alloy powder obtained by the technology of doping rhenium element with tungsten powder;
FIG. 4 is an SED diagram of a high strength ultra-fine tungsten wire prepared in example 1 of the present invention;
FIG. 5 is the SED diagram of the high strength ultra-fine tungsten wire prepared in example 2 of the present invention.
Detailed Description
The technical solutions and effects of the present invention will be further described with reference to the drawings and specific embodiments, but the scope of the present invention is not limited thereto.
As shown in fig. 1, a method for preparing a high-strength ultra-fine tungsten alloy wire for cutting comprises the following steps:
1) preparing materials: selecting pure tungsten powder or acid-washing tungsten powder (such as potassium content is 10-100 ppm) as a raw material, wherein the granularity is 1-3 um, and the purity is 99.99%; the prepared high-strength superfine tungsten alloy wire comprises the following components in percentage by mass: 0.05-2% of lanthanum or 0-1% of rhenium, and the balance of tungsten;
2) doping: weighing a certain amount of lanthanum nitrate or ammonium rhenate according to a proportion, adding the lanthanum nitrate or ammonium rhenate into deionized water, uniformly stirring, heating at a constant temperature of 80-150 ℃, stopping heating after the materials are completely dissolved, and filling the mixed solution into a doping mixer at a rotating speed of 20-30 r/min for 2-4 h to obtain rare earth element doped tungsten powder;
3) reduction: loading rare earth element doped tungsten powder into a molybdenum boat, roasting the molybdenum boat in a reduction furnace at the roasting temperature of 500-950 ℃ for 5-7H, wherein the weight of each boat of the tungsten powder is 200-300 g, and H 2 The flow rate is 30-50L/mim, and the tungsten alloy powder is obtained by sieving through a 120-mesh wire mesh after discharge;
4) pressing a blank bar: filling tungsten alloy powder into a rubber sleeve, and forming by adopting an isostatic pressing mode, wherein the pressing pressure is 150-160 MPa, and the pressure maintaining time is 120-180 s, so as to form a tungsten alloy round bar blank strip;
5) pre-burning: putting the tungsten alloy round bar billet which is formed by pressing into a pre-burning furnace in H 2 Sintering at the high temperature of 1000-1300 ℃ in the atmosphere, and keeping the temperature for 1-2 h to obtain tungsten alloy pre-sintering billet bars;
6) vertical melting: putting the preburning billet into a vertical melting machine in H 2 Under the atmosphere, the current is 2500-3000A, the heat preservation time is 20-30 min, and a tungsten alloy round bar with the relative density of not less than 95% is obtained, and the diameter is 17.4-20 mm;
7) cogging: forging and cogging a tungsten alloy round bar with the diameter of 17.4-20 mm by using a 203-shaped rotary hammer machine, and performing rotary forging for 8-12 times, wherein the compression rate of each time is 10-15%, the heating temperature is 1500-1600 ℃, and the heat preservation time is 20-30 min to obtain a rod with the diameter of 8.0-9.0 mm;
8) rotary swaging: continuously forging the tungsten alloy rod with the diameter of 8.0-9.0 mm by using a rotary hammer machine, performing rotary forging for 8-15 times, wherein the compression ratio of each time is 10-15%, the heating temperature is 1300-1500 ℃, and the heat preservation time is 10-30 s, so as to obtain the rod with the diameter of 3.0-4.0 mm;
9) drawing the thick wire: carrying out hot drawing on a rod with the diameter of 3.0-4.0 mm for 20-35 times by using a wire drawing machine, wherein the compression rate of each pass is 15-35%, the heating temperature is 650-1100 ℃, and the drawing speed is 5-30 m/min, so as to obtain tungsten alloy thick wires with the diameter of 0.1-0.2 mm;
10) drawing the filaments: carrying out hot drawing on the tungsten alloy thick wire with the diameter of 0.1-0.2 mm for 5-10 times, wherein the compression rate of each pass is 15-25%, the heating temperature is 650-1100 ℃, and the drawing speed is 20-100 m/min, so as to obtain the tungsten alloy thin wire with the diameter of 10-60 um;
11) annealing treatment: carrying out continuous annealing heat treatment on tungsten alloy wires with the diameter of 10-60 um by using a tubular annealing furnace, wherein the annealing temperature is 1100-1300 ℃, the take-up speed is 10-15 m/min, and the hydrogen flow is 3L/min;
12) electrolytic polishing: and (3) cleaning the tungsten alloy wire by adopting continuous electrolytic polishing, wherein the electrolytic voltage is 10-50V, the concentration of the electrolytic alkali liquor is 10-15 wt%, and the take-up speed is 40-70 m/min.
Example 1
This embodiment is described with reference to a high-strength ultra-fine W-La alloy wire with a wire diameter of 38 um.
(1) Weighing 500g of lanthanum nitrate, adding the lanthanum nitrate into 1L of deionized water, uniformly stirring, heating at a constant temperature of 150 ℃, and stopping heating after the lanthanum nitrate is completely dissolved. Weighing 49.5Kg of pure tungsten powder, filling the pure tungsten powder into a doping mixer, injecting the completely dissolved lanthanum nitrate solution into the doping mixer, and mixing at the rotating speed of 30r/min for 4h to obtain the tungsten-lanthanum doping powder.
Loading tungsten lanthanum doped powder into molybdenum boats, roasting the molybdenum boats in a reduction furnace at the roasting temperature of 500-950 ℃, wherein the first temperature zone is 500 ℃, the second temperature zone is 750 ℃, the third temperature zone is 830 ℃, the fourth temperature zone is 950 ℃, the heat preservation time is 6.5H, and H is 2 The flow rate is 50L/mim, and the tungsten lanthanum alloy powder is obtained by sieving with a 120-mesh wire mesh after being discharged from the furnace. As shown in fig. 2, it was found that the fine lanthanum oxide powder was uniformly distributed around the large tungsten powder particles, and the uniformity of lanthanum oxide distribution and the adhesion to the tungsten powder were good.
(2) And (3) filling the tungsten-lanthanum alloy powder into rubber sleeves, wherein the filling amount of each tungsten-lanthanum alloy powder is 1.2Kg, and forming by adopting cold isostatic pressing, wherein the pressing pressure is 160MPa, and the pressure maintaining time is 180s to form tungsten-lanthanum alloy round bar billets. Pre-burning tungsten lanthanum alloy round bar billet by using a muffle furnace, namely H 2 Sintering at 1250 ℃ in the atmosphere for 1h to obtain the tungsten lanthanum alloy pre-sintering billet. And then loading the pre-sintered tungsten lanthanum alloy billet into a vertical melting machine, wherein the hydrogen flow is 3L/h, the current is 3000A, the heat preservation time is 20min, removing impurity elements in the tungsten lanthanum billet and realizing densification, and the relative density of the tungsten lanthanum alloy rod is 96%, the diameter is 18mm, and the length is 600 mm.
(3) Cogging the tungsten lanthanum alloy rod by using a 203-shaped rotary hammer machine, and carrying out rotary forging for 10 times, wherein the compression rate of each time is 14%, the heating temperature is 1500 ℃, and the temperature is kept for 20min, so that the tungsten alloy rod with the diameter of 8.2mm is obtained. And (3) continuously forging the tungsten-lanthanum alloy thick rod with the diameter of 8.2mm by adopting a rotary hammer machine, carrying out rotary forging for 10 times, wherein the compression rate of each time is 14%, the heating temperature is 1300 ℃, and the heat preservation time is 15s, so as to obtain the tungsten-lanthanum alloy rod with the diameter of 3.5 mm.
(4) And (3) carrying out hot drawing on the tungsten alloy thin rod with the diameter of 3.5mm for 30 times by using a wire drawing machine, wherein the compression ratio of each pass is 30%, the heating temperature is 700 ℃, and the drawing speed is 25m/min, so that the tungsten lanthanum alloy thick wire with the diameter of 0.11mm is obtained. And (3) carrying out hot drawing on the tungsten lanthanum alloy thick wire with the diameter of 0.11mm for 7 times by using a wire drawing machine, wherein the compression rate of each pass is 20%, the heating temperature is 650 ℃, and the drawing speed is 80m/min, so that the tungsten lanthanum alloy thin wire with the diameter of 38um is obtained. And annealing the drawn tungsten lanthanum alloy wire at the annealing temperature of 1200 ℃, the take-up speed of 10m/min and the hydrogen flow rate of 3L/min. And finally, continuously carrying out electrolytic polishing and cleaning on the tungsten lanthanum alloy wire, wherein the electrolytic voltage is 15V, the concentration of the electrolytic alkali liquor is 10wt%, and the take-up speed is 50 m/min.
As shown in FIG. 4, the high-strength ultra-fine tungsten lanthanum wire obtained in the present example was tested to have a wire diameter of 38 μm, a room-temperature tensile strength of 6230MPa, an elongation of 1.8%, and a smooth surface without defects such as burrs and cracks. Compared with the traditional diamond wire saw matrix steel wire, the tungsten lanthanum alloy wire has the characteristics of smaller wire diameter, higher strength, better wear resistance and longer service life, and can be well applied to the preparation of diamond wire saws.
Example 2
This embodiment is described with a high strength ultra-fine W-Re alloy wire with a wire diameter of 35 um.
(1) Weighing 360g of ammonium rhenate, adding the ammonium rhenate into 1L of deionized water, uniformly stirring, heating at a constant temperature of 150 ℃, and stopping heating after the materials are completely dissolved. Weighing 49.75Kg of pure tungsten powder, filling the pure tungsten powder into a doping mixer, and injecting the completely dissolved mixed solution into the doping mixer for mixing at the rotating speed of 30r/min for 4h to obtain the rare earth element doped tungsten powder.
Loading the rare earth element doped tungsten powder into a molybdenum boat, wherein the weight of each boat of the tungsten powder is 250g, and roasting in a reduction furnace at the roasting temperature of500-950 ℃, wherein the temperature of the first temperature zone is 500 ℃, the temperature of the second temperature zone is 750 ℃, the temperature of the third temperature zone is 830 ℃, the temperature of the fourth temperature zone is 950 ℃, the heat preservation time is 7H, H 2 The flow rate is 40L/mim, the tungsten-rhenium alloy powder is obtained by sieving with a 120-mesh wire mesh after discharge, as shown in fig. 3, it can be seen from an electron microscope picture that fine rhenium powder is uniformly distributed around large tungsten powder particles, and the uniformity of the distribution of rhenium powder and the adhesion of rhenium powder to tungsten powder are good.
(2) And (3) filling the tungsten-rhenium alloy powder into a rubber sleeve, wherein the filling amount of each tungsten-rhenium alloy powder is 1.2Kg, and forming by adopting cold isostatic pressing, wherein the pressing pressure is 160MPa, and the pressure maintaining time is 200s to form a tungsten-rhenium alloy round bar blank. Pre-burning the W-Re alloy rod blank in a muffle furnace to obtain H 2 Sintering at 1250 ℃ in the atmosphere for 1h to obtain the tungsten-rhenium alloy pre-sintering billet. And then loading the tungsten-rhenium alloy blank strip subjected to pre-sintering into a vertical melting machine, wherein the hydrogen flow is 3L/h, the current is 3000A, the heat preservation time is 20min, removing impurity elements in the blank strip and realizing densification, and the tungsten-rhenium alloy rod has the relative compactness of 95%, the diameter of 17mm and the length of 620 mm.
(3) And (3) cogging the tungsten-rhenium alloy rod by adopting a 203-shaped rotary hammer machine, carrying out rotary forging for 10 times, wherein the compression rate of each time is 14%, the heating temperature is 1550 ℃, and carrying out heat preservation for 30min to obtain the tungsten alloy rod with the diameter of 7.8 mm. And (3) continuously forging the tungsten-rhenium alloy thick rod with the diameter of 7.8mm by adopting a rotary hammer machine, carrying out rotary forging for 9 times, wherein the compression ratio of each time is 14%, the heating temperature is 1350 ℃, and the heat preservation time is 10s to obtain the tungsten-rhenium alloy rod with the diameter of 3.2 mm.
(4) And (3) carrying out 28 times of hot drawing on the tungsten-rhenium alloy rod with the diameter of 3.2mm by using a wire drawing machine, wherein the compression ratio of each pass is 28%, the heating temperature is 650 ℃, and the drawing speed is 20m/min, so that the tungsten alloy thick wire with the diameter of 0.13mm is obtained. And (3) carrying out hot drawing on the tungsten-rhenium alloy thick wire with the diameter of 0.13mm for 5 times by using a wire drawing machine, wherein the compression ratio of each pass is 16%, the heating temperature is 600 ℃, and the drawing speed is 70m/min, so that the tungsten-rhenium alloy thin wire with the diameter of 35um is obtained. And annealing the drawn tungsten-rhenium alloy wire at 1150 ℃, the take-up speed of 12m/min and the hydrogen flow of 3L/min. And finally, continuously carrying out electrolytic polishing and cleaning on the tungsten-rhenium alloy wire, wherein the electrolytic voltage is 15V, the concentration of the electrolytic alkali liquor is 10wt%, and the take-up speed is 60 m/min.
As shown in FIG. 5, the high-strength ultra-fine W-Re alloy wire obtained in the example has a wire diameter of 35um, a room-temperature tensile strength of 5730MPa and an elongation of 2.5%, has a smooth surface, has no defects such as burrs and cracks, and can meet the use requirements of diamond wire saw substrates. Compared with the traditional diamond wire saw matrix steel wire, the tungsten-rhenium alloy wire has the characteristics of smaller wire diameter, higher strength, better wear resistance and longer service life, and can be well applied to the preparation of diamond wire saws.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The preparation method of the high-strength superfine tungsten alloy wire for cutting is characterized by comprising the following steps of:
1) preparing materials: the high-strength superfine tungsten alloy wire comprises the following components in percentage by mass: 0.05-2% of lanthanum or 0-1% of rhenium, and the balance of tungsten; the tungsten adopts pure tungsten powder or acid-washing tungsten powder as a raw material, and rare earth elements lanthanum and rhenium are doping elements;
2) doping: adding lanthanum or rhenium into pure tungsten powder or acid-washing tungsten powder in the form of salt solution thereof;
3) reduction: mixing the mixture obtained in 2) in H 2 Roasting and reducing under the atmosphere to obtain tungsten alloy powder;
4) pressing a blank bar: preparing tungsten alloy round bar billet from the tungsten alloy powder obtained in the step 3) in an isostatic pressing mode;
5) pre-burning: pre-sintering a tungsten alloy round bar billet;
6) vertical melting: loading the pre-sintered tungsten alloy round bar billet into a vertical melting machine in H 2 Sintering the tungsten alloy round bar with the relative density not lower than 95% after heavy current in the atmosphere, wherein the diameter is 17.4-20 mm;
7) cogging: cogging a tungsten alloy round bar with the diameter of 17.4-20 mm to obtain a tungsten alloy rod with the diameter of 8.0-9.0 mm;
8) rotary swaging: performing rotary swaging on the tungsten alloy rod with the diameter of 8.0-9.0 mm to obtain the tungsten alloy rod with the diameter of 3.0-4.0 mm;
9) drawing the thick wire: drawing a tungsten alloy rod with the diameter of 3.0-4.0 mm to obtain a tungsten alloy thick wire with the diameter of 0.1-0.2 mm;
10) drawing the filaments: drawing a tungsten alloy thick wire with the diameter of 0.1-0.2 mm to obtain a tungsten alloy thin wire with the diameter of 10-60 mu m;
11) annealing treatment: carrying out continuous annealing heat treatment on tungsten alloy filaments with the diameters of 10-60 um by using a hydrogen tube type annealing furnace to eliminate internal stress;
12) electrolytic polishing: and the tungsten alloy wire is cleaned by continuous electrolytic polishing, so that the surface defects of the wire material are eliminated.
2. The method for preparing the high-strength superfine tungsten alloy wire for cutting as claimed in claim 1, wherein the diameter of the high-strength superfine tungsten alloy wire prepared by the preparation method is 10-60 um, and the tensile strength at room temperature is not less than 5000 MPa.
3. The preparation method of the high-strength superfine tungsten alloy wire for cutting according to claim 1, wherein the roasting reduction temperature in 3) is 500-950 ℃, the heat preservation time is 5-7 h, and the tungsten alloy wire is taken out of a furnace and then sieved by a 120-mesh sieve to obtain tungsten alloy powder with the particle size of 1-3 um.
4. The method for preparing high-strength ultra-fine tungsten alloy wire for cutting as claimed in claim 1, wherein the pre-sintering in 5) is performed in H 2 And (3) carrying out heat preservation for 1-2 h at 1000-1300 ℃ in the atmosphere.
5. The method for preparing the high-strength superfine tungsten alloy wire for cutting according to claim 1, wherein in the 7) cogging process, the pass reduction rate is 10-15%, the heating temperature is 1500-1600 ℃, and the temperature is kept for 20-30 min.
6. The preparation method of the high-strength superfine tungsten alloy wire for cutting according to claim 1, wherein in the 8) rotary forging process, the pass reduction rate is 10-15%, the heating temperature is 1300-1500 ℃, and the heat preservation time is 10-30 s.
7. The method for preparing the high-strength superfine tungsten alloy wire for cutting according to claim 1, wherein in the drawing process of the 9) thick wire, the pass reduction rate is 15-35%, the heating temperature is 650-1000 ℃, and the drawing speed is 5-30 m/min.
8. The method for preparing the high-strength superfine tungsten alloy wire for cutting according to claim 1, wherein in the drawing process of the 10) filament, the pass reduction rate is 15-25%, the heating temperature is 650-1000 ℃, and the drawing speed is 20-100 m/min.
9. The preparation method of the high-strength superfine tungsten alloy wire for cutting as claimed in claim 1, wherein the annealing temperature of the 11) continuous annealing heat treatment is 1100-1300 ℃, the take-up speed is 10-15 m/min, and the hydrogen flow rate is 3L/min.
10. The method for preparing the high-strength ultrafine tungsten alloy wire for cutting according to claim 1, wherein the electrolytic voltage of the continuous electrolytic polishing in the step 12) is 10-50V, the concentration of the electrolytic alkali solution is 10-15 wt%, and the wire take-up speed is 40-70 m/min.
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