CN1054563C - Production method of lanthanum-tungsten electrode - Google Patents
Production method of lanthanum-tungsten electrode Download PDFInfo
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- CN1054563C CN1054563C CN97100727A CN97100727A CN1054563C CN 1054563 C CN1054563 C CN 1054563C CN 97100727 A CN97100727 A CN 97100727A CN 97100727 A CN97100727 A CN 97100727A CN 1054563 C CN1054563 C CN 1054563C
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- lanthanum
- tungsten
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- composite powder
- coated composite
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Abstract
The present invention relates to a manufacture method of lanthanum-tungsten electrodes, particularly to a manufacture method of lanthanum-tungsten electrodes, which is mainly used for welding, cutting, spraying, smelting metals, etc. in the technical fields of TIG (tungsten-inert gas protection welding) and PLASMA. The present invention is characterized in that lanthanum acetate and slurry material which is made by solid raw material comprising APT, WO3 and W powder and water are uniformly mixed to prepare lanthanum tungsten coated powder; the decomposition process of lanthanum salt in the lanthanum tungsten coated powder is carried out in hydrogen atmosphere. The method of the present invention makes the lanthanum salt sufficiently decomposed, obviously improves the conductive performance of square material in the process of incipient fusion, and makes the decomposition process and the reduction process of the lanthanum salt simultaneously carried out in the same device. The method simplifies technology, effectively decreases man-hour and saves energy resources.
Description
The manufacture method of lanthanum-tungsten electrode relates to a kind of TIG of being mainly used in (gas tungsten arc welding) and PLASMA (plasma) technical field, carries out a kind of manufacture method of tungsten electrode of the welding, cutting, spraying, melting etc. of metal.
Tungsten electrode material is one of critical material in TIG and the PLASMA technology.The tungsten electrode in industrial use has numerous species.Thorium tungsten electrode in the widely used tungsten electrode has shown preferable performance.But because thorium wherein can produce the radiological hazard of accumulative total property and environment is produced radioactive pollution human body, people develop the cerium tungsten electrode for this reason, attempt to be substituted with radioactive thorium tungsten electrode at TIG and PLASMA technical field.Practical application effect shows that the cerium tungsten electrode has successfully replaced thorium tungsten electrode at aspects such as little electric current argon arc weldings.But exchanging aspect polarity, glow discharge spot lamp, the cathode emission material, still the end replaces the thorium electrode fully, defective such as exist the starting the arc repeatedly, poor reliability, burn out rate is big, the life-span is low.Along with development of high-tech, fields such as mechano-electronic, oil, chemical industry, Aero-Space, boats and ships, atomic energy, the requirement of the kind of the metal parent material that is cut, shape, thickness etc. becomes increasingly complex, and is more and more harsher to the performance requirement of tungsten electrode.Need develop the better electrode of performance to satisfy the demand.Result of study shows that performance, particularly lanthanum-tungsten electrode that interpolation rare-earth elements La, Y can improve tungsten electrode effectively have the advantages that the life-span is long, arc starting performance is good, have broad application prospects.Make the method for lanthanum-tungsten electrode at present, mainly be to adopt solid material is evenly mixed with lanthanum nitrate,, oven dry (roasting) concentrated by heating, operation such as sieve are prepared lanthanum tungsten coated composite powder, reduce then, die mould, incipient fusion, base and finished product processing makes lanthanum-tungsten electrode.Owing to be to adopt nitrate to prepare the method for coated composite powder, in preparation process, can produce a large amount of NO and pollute, and, cause technology difficulty big because the decomposition temperature height of nitrate needs long roasting that it is decomposed fully.But also might produce because nitrate decomposes not exclusively the phenomenon that the poor electric conductivity of the base bar that causes, processing performance worsen.The applicant in September, 1989 in the patent No. is 89107270.5 patent application, disclosed and adopted cerous acetate to prepare the method for cerium tungsten electrode, this method is avoided in the cerium tungsten electrode manufacture process effectively, the NO that produces during the preparation coated composite powder
xThe problem of contaminated environment, operating condition inclement condition, but aspect processing characteristics, also have deficiency.
The objective of the invention is in order to overcome above shortcomings in the prior art, provide that a kind of technology difficulty is little, pollution-free, the manufacture method of a kind of new lanthanum-tungsten electrode of good processability.
The objective of the invention is to be achieved through the following technical solutions.
The manufacture method of lanthanum-tungsten electrode comprises it is characterized in that preparation, reduction, die mould, incipient fusion, base and the finished product process of lanthanum tungsten coated composite powder: a: adopt lanthanum acetate and comprise APT, WO
3Add water finish mix slurry with the solid material of W powder and mix, preparation lanthanum tungsten coated composite powder; B. the decomposable process of lanthanum salt is to carry out in hydrogen atmosphere in the lanthanum tungsten coated composite powder, one time reduction temperature is controlled at 600～700 ℃, and the time is 2-3 hour, and the secondary reduction temperature is controlled at 800-970 ℃, recovery time 3-5 hour, the control hydrogen flowing quantity was 1.39 * 10 in the process
-4～5.56 * 10
-4m
3/ S.
Process of the present invention adopts and adds lanthanum acetate and comprise APT, WO
3With the solid material of W powder, the method for synthetic lanthanum tungsten coated composite powder prepares lanthanum-tungsten electrode, has replaced the method that adopts lanthanum nitrate to prepare lanthanum tungsten coated composite powder in original technology, has eliminated because of nitrate decomposes and has produced NO
xThe pollution of gas.Because lanthanum acetate and the difference of lanthanum nitrate on decomposition temperature cause the difference on the technological effect.Adopt lanthanum acetate to prepare lanthanum tungsten coated composite powder and greatly reduce decomposition temperature, simplified technical process effectively, and the decomposition of lanthanum salt is carried out in method employing of the present invention in hydrogen atmosphere, avoided the instability volatilization of lanthanide in oxidizing atmosphere, and it is more abundant that lanthanum salt is decomposed, and obviously improved the electric conductivity of square stock in the incipient fusion process.Uninterruptedly finishing two technical process continuously with decomposition that makes lanthanum salt and reduction process realization in identical device, simplified technology greatly, reduced man-hour, saved the energy, is a kind of manufacture method of more satisfactory lanthanum-tungsten electrode.
Description of drawings
Accompanying drawing is the flow chart of the manufacture method of lanthanum-tungsten electrode of the present invention.
Below in conjunction with example method of the present invention is described in detail as follows.
The manufacture method of lanthanum-tungsten electrode comprises it is characterized in that preparation, reduction, die mould, incipient fusion, base and the finished product process of lanthanum tungsten coated composite powder: a. adopts lanthanum acetate and comprises APT, WO
3Add water finish mix slurry roller with the solid material of W powder and close evenly, prepare lanthanum tungsten coated composite powder; B. the decomposable process of lanthanum salt is to carry out in hydrogen atmosphere in the lanthanum tungsten coated composite powder, one time reduction temperature is controlled at 600～700 ℃, and the time is 2-3 hour, and the secondary reduction temperature is controlled at 800-970 ℃, recovery time 3-5 hour, the control hydrogen flowing quantity was 1.39 * 10 in the process
-4～5.56 * 10
-4m
3/ S.
1. experimental raw
APT, WO
3, the W powder: purity is all greater than 99.5% (by weight);
Fe
2O
3: content is less than 0.0025%;
MO: content is less than 0.01%;
As: content is less than 0.0025%;
Al
2O
3: content is less than 0.005%;
P: content is less than 0.01%;
Oxidation residua vestige raw meal particle size APT:25～26 μ m;
WO
3：8～9μm；
W powder: 2～2.5 μ m;
2. the preparation of lanthanum tungsten coated composite powder
Press admittedly raw materials used: H
2O=1: fully stir the 1 ratio back of sizing mixing, and by made tungsten electrode trade mark requirement proportional quantities, adds lanthanum acetate equably again, after continuing to mix, delivers reduction after operations such as, drying concentrated by steam heated are sieved.
3. reduction
Behind the lanthanum tungsten coated composite powder dress boat that makes, in reduction furnace, heat up and decompose and first and second reduction, when one time reduction temperature was 600～700 ℃, the recovery time was 2～3 hours.The secondary reduction temperature is: 800～970 ℃, the time is 3-5 hour.Said process all carries out under hydrogen atmosphere, control throughput: 1.39 * 10
-4～5.56 * 10
-4m
3/ S.
4. die mould
Lanthanum tungsten cladding powder after the reduction is closed batch 2-5 hour, carry out physico-chemical analysis then, when particle mean size, LaO content and the uniformity for the treatment of lanthanum tungsten cladding powder all meets technological requirement, add alcohol, glycerine lubrication agent mix after 1 hour sieve, compacting, pre-burning, compacting, pre-sinter process condition be:
Filling amount: the 650-700g/ root, compacting pre-burning pressure: 60～80MPa, sintering temperature: 1050～1400 ℃, sintering time: 40～60 minutes.
5. incipient fusion
Adopt conventional incipient fusion sintering process, process conditions are as follows:
The incipient fusion temperature: 2600～3000 ℃, temperature retention time: 20 minutes, temperature fall time: 2 minutes, cool time: 3 minutes.
6. finished product processing
Square billet behind the incipient fusion with qualified material base, is put into the heating furnace that has hydrogen shield after the assay was approved, and the technological requirement temperature of pressing sample is incubated 20 minutes, swages on request, is machined to required different size finished product then.
Example 1.
Get APT powder 1000 gram, add 1000 gram water, stir, add lanthanum acetate 60 grams, after continuing to stir, with steam heated concentrate, after the drying, sieving obtains lanthanum tungsten coated composite powder.With the lanthanum tungsten coated composite powder dress boat that makes, put into the reduction furnace that is connected with hydrogen, heat up and once reduce, temperature is 600 ℃, the recovery time is 2 hours.Continue to be warming up to 800 ℃ again and carry out secondary reduction, the recovery time was controlled at 3.5 hours, and hydrogen flowing quantity is 1.39 * 10 in the process
-4m
3/ s.Then lanthanum tungsten coated composite powder add alcohol, glycerine lubrication agent mix after 1 hour sieve, compacting, pre-burning, compacting, pre-sinter process condition be: filling amount: 650-700g/ root, compacting pre-burning pressure: 60～80MPa, sintering temperature: 1050～1400 ℃, sintering time: 40～60 minutes.Adopt conventional incipient fusion sintering process then, process conditions are as follows: the incipient fusion temperature: 2600～3000 ℃, and temperature retention time: 20 minutes, temperature fall time: 2 minutes, cool time: 3 minutes.Carry out finished product processing at last, the square billet behind the incipient fusion with qualified material base, is put into the heating furnace that has hydrogen shield after the assay was approved, and the technological requirement temperature of pressing sample is incubated 20 minutes, swages on request, is machined to required different size finished product then.
Example 2.
Get W powder 700 gram, add 700 gram water, stir, add lanthanum acetate 55 grams, after continuing to stir, with Steam Heating concentrate, after the drying, sieving obtains lanthanum tungsten coated composite powder.With the lanthanum tungsten coated composite powder dress boat that makes, put into the reduction furnace that is connected with hydrogen, heat up and once reduce, temperature is 650 ℃, 2 hours recovery times.Continue to be warming up to 900 ℃ again and carry out secondary reduction, the recovery time was controlled at 4 hours, and hydrogen flowing quantity is 1.39 * 10 in the process
-4m
3/ s.Other condition is with example 1.
Example 3.
Get WO
3Powder 850 gram adds 850 gram water, stirs, and adds lanthanum acid lanthanum 58 grams, after continuing to stir, by Steam Heating concentrate, after the drying, sieving obtains lanthanum tungsten coated composite powder.With the lanthanum tungsten coated composite powder that makes dress boat, put into the reduction furnace that is connected with hydrogen, heat up and once reduce, temperature is 670 ℃, during reduction 2.5 hours.Continue to be warming up to 970 ℃ and carry out secondary reduction, the recovery time was controlled at 5 hours, and hydrogen flowing quantity is 1.39 * 10 in the process
-4m
3/ s.Other condition is with example 1.
The resulting sample of above-mentioned experiment all meets the requirement of GB4191 and ISO6848-84 standard.
Method of the present invention is compared with the method that adopts lanthanum nitrate to prepare lanthanum tungsten coated composite powder, and common ground is the prolongation along with the recovery time, and the particle mean size of its lanthanum tungsten coated composite powder is grown up.And lanthanum nitrate is subjected to the influence of recovery time more responsive, and particle mean size increases wide ranges.Method of the present invention, lanthanum tungsten coated composite powder are subjected to the granularity fluctuation range that the recovery time influences then less, and particle size range reaches unanimity substantially in the regular hour.These two kinds of diverse ways all are finally with La
2O
3Form be coated in the tungsten base, play a part crystal grain thinning, but because their difference on the decomposition temperature separately must cause the difference on the result.Method of the present invention, under specific process conditions, the fluctuation of powder size scope is less, and meets compacting, pre-sinter process requirement, can simplify technology effectively, helps eliminating NO
xHarmful gas pollution is a kind of preparation method of comparatively desirable lanthanum-tungsten electrode.
Claims (1)
1. the manufacture method of lanthanum-tungsten electrode comprises it is characterized in that preparation, reduction, die mould, incipient fusion, base and the finished product process of lanthanum tungsten coated composite powder:
A. adopt lanthanum acetate and comprise APT, WO
3Add water finish mix slurry with the solid material of W powder and mix, preparation lanthanum tungsten coated composite powder;
B. the decomposable process of lanthanum salt is to carry out synchronously with reduction process in hydrogen atmosphere in the lanthanum tungsten coated composite powder, one time reduction temperature is controlled at 600～700 ℃, and the time is 2-3 hour, and the secondary reduction temperature is controlled at 800-970 ℃, the secondary reduction time is 3-5 hour, and hydrogen flowing quantity is 1.39 * 10 in the process
-4～5.56 * 10
-4m
3/ S.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97100727A CN1054563C (en) | 1997-02-27 | 1997-02-27 | Production method of lanthanum-tungsten electrode |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97100727A CN1054563C (en) | 1997-02-27 | 1997-02-27 | Production method of lanthanum-tungsten electrode |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1160617A CN1160617A (en) | 1997-10-01 |
| CN1054563C true CN1054563C (en) | 2000-07-19 |
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ID=5165273
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|---|---|---|---|
| CN97100727A Expired - Fee Related CN1054563C (en) | 1997-02-27 | 1997-02-27 | Production method of lanthanum-tungsten electrode |
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| JP5379863B2 (en) * | 2009-10-19 | 2013-12-25 | 日本タングステン株式会社 | Discharge method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS558644A (en) * | 1978-06-30 | 1980-01-22 | Matsushita Electric Ind Co Ltd | Magnetic tape device |
| US4923673A (en) * | 1988-10-17 | 1990-05-08 | Gesellschaft Fur Wolfram-Industrie Mbh | Method for producing alloyed tungsten rods |
| CN1015238B (en) * | 1989-09-27 | 1992-01-01 | 北京高熔金属材料厂 | Preparation method for tungsten cerium powder |
| EP0573195A1 (en) * | 1992-06-01 | 1993-12-08 | General Electric Company | Method of forming fine dispersion of metal oxide in tungsten |
| JPH06297189A (en) * | 1993-04-14 | 1994-10-25 | Toho Kinzoku Kk | Tungsten electrode material |
| EP0759478A1 (en) * | 1995-07-26 | 1997-02-26 | Osram Sylvania Inc. | Method of making an alloy of tungsten and lanthana |
-
1997
- 1997-02-27 CN CN97100727A patent/CN1054563C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS558644A (en) * | 1978-06-30 | 1980-01-22 | Matsushita Electric Ind Co Ltd | Magnetic tape device |
| US4923673A (en) * | 1988-10-17 | 1990-05-08 | Gesellschaft Fur Wolfram-Industrie Mbh | Method for producing alloyed tungsten rods |
| CN1015238B (en) * | 1989-09-27 | 1992-01-01 | 北京高熔金属材料厂 | Preparation method for tungsten cerium powder |
| EP0573195A1 (en) * | 1992-06-01 | 1993-12-08 | General Electric Company | Method of forming fine dispersion of metal oxide in tungsten |
| JPH06297189A (en) * | 1993-04-14 | 1994-10-25 | Toho Kinzoku Kk | Tungsten electrode material |
| EP0759478A1 (en) * | 1995-07-26 | 1997-02-26 | Osram Sylvania Inc. | Method of making an alloy of tungsten and lanthana |
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| Publication number | Publication date |
|---|---|
| CN1160617A (en) | 1997-10-01 |
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