CN103862196B - A kind of radiationless electrode material of multielement composite rare earth tungsten and preparation method thereof - Google Patents
A kind of radiationless electrode material of multielement composite rare earth tungsten and preparation method thereof Download PDFInfo
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- CN103862196B CN103862196B CN201410074969.3A CN201410074969A CN103862196B CN 103862196 B CN103862196 B CN 103862196B CN 201410074969 A CN201410074969 A CN 201410074969A CN 103862196 B CN103862196 B CN 103862196B
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 53
- 239000010937 tungsten Substances 0.000 title claims abstract description 53
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 24
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 22
- 239000007772 electrode material Substances 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 28
- 230000009467 reduction Effects 0.000 claims abstract description 22
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 20
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 16
- 229910052702 rhenium Inorganic materials 0.000 claims abstract description 16
- 230000004927 fusion Effects 0.000 claims abstract description 14
- 238000005275 alloying Methods 0.000 claims abstract description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 8
- 230000006698 induction Effects 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 238000005491 wire drawing Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 39
- 239000011812 mixed powder Substances 0.000 claims description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 24
- 239000001257 hydrogen Substances 0.000 claims description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims description 24
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 12
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 claims description 6
- 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 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 3
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims 2
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 36
- 238000003466 welding Methods 0.000 description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 9
- 238000010891 electric arc Methods 0.000 description 7
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 229910052776 Thorium Inorganic materials 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 6
- 230000003068 static effect Effects 0.000 description 6
- HRLYFPKUYKFYJE-UHFFFAOYSA-N tetraoxorhenate(2-) Chemical compound [O-][Re]([O-])(=O)=O HRLYFPKUYKFYJE-UHFFFAOYSA-N 0.000 description 6
- 238000011056 performance test Methods 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 230000005684 electric field Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- 229910052765 Lutetium Inorganic materials 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 description 2
- 229910003452 thorium oxide Inorganic materials 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- 229910000691 Re alloy Inorganic materials 0.000 description 1
- IADRPEYPEFONML-UHFFFAOYSA-N [Ce].[W] Chemical compound [Ce].[W] IADRPEYPEFONML-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- -1 compound rare-earth Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- FAYUQEZUGGXARF-UHFFFAOYSA-N lanthanum tungsten Chemical compound [La].[W] FAYUQEZUGGXARF-UHFFFAOYSA-N 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- XEIRTJPYRLBENS-UHFFFAOYSA-N thorium Chemical compound [Th].[Th] XEIRTJPYRLBENS-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/222—Non-consumable electrodes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
- B23K35/402—Non-consumable electrodes; C-electrodes
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of radiationless electrode material of multielement composite rare earth tungsten and preparation method thereof, radiationless electrode material of multielement composite rare earth tungsten contains lanthana, zirconium oxide, yittrium oxide, luteium oxide, rhenium and tungsten, wherein every kind of rare earth oxide accounts for this quality of materials percentage is 0.5% ~ 1.5%, it is 2% ~ 3% that total amount of the rare earth oxide accounts for this quality of materials percentage, it is 1% ~ 4% that alloying element rhenium accounts for this quality of materials percentage, and remaining is tungsten.The preparation method of radiationless electrode material of multielement composite rare earth tungsten include configuring solution, be dried, reduction, isostatic cool pressing, sintering, incipient fusion, Medium frequency induction is annealed, B202 swages, B201 swages, wire drawing, align, cut, polish and polish operation.The radiationless electrode material of multielement composite rare earth tungsten handling ease made, and serviceability is more preferably.
Description
Technical field
The present invention relates to a kind of tungsten electrode material and preparation method thereof, particularly relate to a kind of radiationless multiple elements design
Rare-earth tungsten electrode material and preparation method thereof.
Background technology
Non-melting electrode argon arc welding is also known as argon tungsten-arc welding or gas tungsten arc welding, i.e. the guarantor of inert gas
Protect down, utilize the arc-melting mother metal produced between workpiece and fill a kind of electric arc welding method of metal.
Non-melt tungsten electrode rises radio and produces the effect of electric arc, and filler wire is sent into from side, at the work of arc heat
It is fused together with lower filling metal and workpiece and forms weld seam.Tungsten fusing point is high, electron emissivity is strong, electronics
Work function is low, elastic modelling quantity is high, steam forces down, therefore is used as thermionic emission materials very early.Due to tungsten
Characteristic so that it is well suited for the electrode material for non-melting electrode argon arc welding welding.But, pure tungsten is crisp moulds transformation
Temperature is high, shapes difficulty, and recrystallization temperature is low, the electrode material coarse grains of general gained, seriously
Yield rate is prepared in the production of impact.On the other hand, in order to adapt to higher solder technology requirement, it is necessary to further
Reduce the electron work functon of pure tungsten, improve its anti-yaw damper performance.
For the problems referred to above, tungsten adds rare earth oxide and stimulates its electron work functon so that tungsten
The welding performance of electrode is improved: the arc starting performance making electrode is more preferable, and the stability of arc column is higher, and electrode burns
Loss rate is less.Common rare earth addition has thorium oxide, cerium oxide, lanthana, zirconium oxide and yittrium oxide etc.,
Gained be called thorium, cerium, lanthanum, zirconium and yttrium.Thorium is easy and simple to handle, can under excess load electric current works fine,
Still having now a lot of company to use this material, it is considered a part for high-quality welding.But the oxidation in thorium
Thorium trace radiates, and affects the healthy of manual solder technologist.Cerium tungsten has a non-radiation type, low melting rate,
The long welding life-span, the good starting the arc, but when cerium tungsten uses under high currents, oxide moves quickly into
Top at high hot-zone, i.e. electrode welding, oxide skewness, cause cerium advantage not exist.Lanthanum tungsten
Machine cuts performance is good, and creep-resistant property is more preferable, and recrystallization temperature is high, and ductility is good.Zirconium and single sample, only
Welding job can be carried out under communication environment.Yttrium is when welding, and arc bundle is elongated, and compression degree is big, in, big
During electric current, its fusion penetration is maximum.Have also appeared ternary even multielement rare earth at present to be combined, will be in addition to thorium oxide
Other rare earth oxide three or more group carries out compound adding to and makes in tungsten basal body.This do not have put
Penetrating property, between internal constituent element, electron transport properties is balanced, and electron work functon is lower, repeats the starting the arc easy,
Life-span is long.No matter it is to add single oxide, or add ternary or multivariant oxide, in terms of materialogy angle
Being all a kind of constituent element composite effect, each oxide particle is all individually to exist mutually, not relate in tungsten basal body
And the alloying of tungsten, the performance that still cannot give full play to, need now a kind of processing radiationless, easy and use badly
The more preferable tungsten electrode material of performance.
Summary of the invention
One of the technical problem to be solved is to provide a kind of processing radiationless, easy and serviceability more
Good tungsten electrode material.
For solving above technical problem, the technical scheme is that a kind of radiationless multiplex composite rare-earth tungsten electricity
Pole material, it it is critical only that: containing lanthana, zirconium oxide, yittrium oxide, luteium oxide, rhenium and tungsten, wherein
It is 0.5%～1.5% that every kind of rare earth oxide accounts for this quality of materials percentage, and total amount of the rare earth oxide accounts for this material matter
Amount percentage is 2%～3%, and it is 1%～4% that alloying element rhenium accounts for this quality of materials percentage, and remaining is tungsten.
The two of the technical problem to be solved are to provide a kind of processing radiationless, easy and serviceability more
The preparation method of good tungsten electrode material.
For solving above technical problem, the technical scheme is that a kind of radiationless multiplex composite rare-earth tungsten electricity
The preparation method of pole material, is characterized in that: comprise the following steps:
Step 1: with shared mass percent in the material, by lanthana, zirconium oxide, yittrium oxide and oxidation
Lutetium every kind rare earth oxide content is 0.5%～1.5%, and four kinds of total amount of the rare earth oxide are 2%～3%, and rhenium is
1%～4%, it is converted into lanthanum nitrate, zirconium nitrate, yttrium nitrate, lutecium nitrate and the amount of rehenic acid ammonium of correspondence, then
Weigh these compounds and be configured to mixed solution；
Step 2: with shared mass percent in the material, be 93～97% by tungsten, by the three of corresponding mass
Tungsten oxide, blue tungsten, tungsten powder or ammonium paratungstate powder add in above-mentioned mixed solution, stir, heating
It is dried and obtains mixed-powder；
Step 3: first by above-mentioned mixed-powder logical hydrogen reducing in reduction furnace, temperature at 400 DEG C～600 DEG C,
Time is 45min～75min, and then the powder of gained continues in reduction furnace logical hydrogen reducing, and temperature exists
700 DEG C～900 DEG C, the time is 45min～75min；By gained mixed-powder sieving for standby after twice reduction；
Step 4: the mixed-powder after above-mentioned reduction weighs 500g～2500g after stirring and inserts soft
Film jacket, jacket puts into cold isostatic press and is pressed into cylindrical billet, and pressing pressure is set in 1000Kg/cm2～3000Kg/cm2；
Step 5: the billet suppressed is carried out under hydrogen shield pre-sintering, sintering temperature is
1100 DEG C～1300 DEG C, 5/boat of boat charge～10/boat, time 30min～60min；
Step 6: pre-burned billet be placed in the incipient fusion agglomerating plant of hydrogen shield, at the fusing electricity of 90%
Flow down insulation 20min, cooling down；
Step 7: the billet after sintering incipient fusion carries out B203 rotary blooming, cogging temperature 1500 DEG C～1650 DEG C,
After through Medium frequency induction annealing, B202 swages, B201 swages, wire drawing, align, cut, polish and polish
After obtain.
By implement the present invention desirable following beneficial effect: described radiationless electrode material of multielement composite rare earth tungsten
Composition design taken into full account multielement rare earth oxide complex effect and the alloying effect of rhenium element, such as rhenium pair
The solid solution softening effect of tungsten, and employ luteium oxide first, accomplish the optimization of light rare earth and heavy rare earth element
Combination so that finished product is radiationless, handling ease, and serviceability is more preferably.Described radiationless multiplex composite rare-earth
The preparation method of tungsten electrode material considers hydraulic press and prepares com-pact density problem pockety, and uses cold
Static pressure machine is suppressed, and adds billet consistency and density uniformity, effectively reduces billet in cogging rotary swaging process
Cracking, improve yield rate.The radiationless multiplex composite rare-earth tungsten electrode material made according to affiliated preparation method
The processing characteristics of material is excellent, and sintering effect is good, well conducting in incipient fusion, and rotary blooming is easily processed, without broken strip,
Splitting phenomena produces.
Detailed description of the invention
A kind of radiationless electrode material of multielement composite rare earth tungsten, containing lanthana, zirconium oxide, yittrium oxide, oxidation
Lutetium, rhenium and tungsten, wherein every kind of rare earth oxide accounts for this quality of materials percentage is 0.5%～1.5%, rare earth oxygen
It is 2%～3% that compound total amount accounts for this quality of materials percentage, and alloying element rhenium accounts for this quality of materials percentage and is
1%～4%, remaining is tungsten.
Embodiment one:
Weigh 19.93g lanthanum nitrate, 26.13g zirconium nitrate, 25.44g yttrium nitrate, 14.28g lutecium nitrate and 21.6g
Ammonium rhenate powder end, is configured to mixed solution, is added by 1834.8g tungsten trioxide powder, stirs and add
Mixed-powder is obtained, by described mixed-powder logical hydrogen reducing in the reduction furnace that temperature is 400 DEG C after heated drying
45min, then by described mixed-powder logical hydrogen reducing 45min in the reduction furnace that temperature is 700 DEG C, will
Mixed powder sieving for standby after twice reduction.Mixed-powder after sizing weighs 500g after stirring
Inserting mantle jacket, jacket is put into cold isostatic press and is pressed into the cylindrical billet of weight 500g, and pressing pressure sets
It is scheduled on 1000Kg/cm2.The billet suppressed is carried out under hydrogen shield pre-sintering, and sintering temperature is
1100 DEG C, 5/boat of boat charge, sintering time is 30min, and pre-burned billet is placed in hydrogen shield
In incipient fusion agglomerating plant, under the blowout current of 90%, it is incubated 20mins carries out cooling down.Burn from incipient fusion
The billet taken out in knot equipment carries out B203 rotary blooming, cogging temperature 1500 DEG C, after move back through Medium frequency induction
Fire, B202 swages, B201 swages, wire drawing, align, cut, polish and polish after obtain.
Embodiment two:
Weigh 19.93g lanthanum nitrate, 26.13g zirconium nitrate, 25.44g yttrium nitrate, 14.28g lutecium nitrate and 21.6g
Ammonium rhenate powder end, is configured to mixed solution, is added by 1834.8g tungsten trioxide powder, stirs and add
Mixed-powder is obtained, by described mixed-powder logical hydrogen reducing in the reduction furnace that temperature is 500 DEG C after heated drying
60min, then by described mixed-powder logical hydrogen reducing 60min in the reduction furnace that temperature is 800 DEG C, will
Mixed powder sieving for standby after twice reduction.Mixed-powder after sizing weighs 1000g after stirring
Inserting mantle jacket, jacket is put into cold isostatic press and is pressed into the cylindrical billet of weight 1000g, and pressing pressure sets
It is scheduled on 1500Kg/cm2.The billet suppressed is carried out under hydrogen shield pre-sintering, and sintering temperature is
1200 DEG C, 8/boat of boat charge, sintering time is 50min, and pre-burned billet is placed in hanging down of hydrogen shield
In molten agglomerating plant, under the blowout current of 90%, it is incubated 20mins carries out cooling down.Sinter from incipient fusion
The billet taken out in equipment carries out B203 rotary blooming, cogging temperature 1580 DEG C, after anneal through Medium frequency induction,
B202 swages, B201 swages, wire drawing, align, cut, polish and polish after obtain.
Embodiment three:
Weigh 19.93g lanthanum nitrate, 26.13g zirconium nitrate, 25.44g yttrium nitrate, 14.28g lutecium nitrate and 21.6g
Ammonium rhenate powder end, is configured to mixed solution, is added by 1834.8g tungsten trioxide powder, stirs and add
Mixed-powder is obtained, by described mixed-powder logical hydrogen reducing in the reduction furnace of temperature 700 DEG C after heated drying
75min, then by described mixed-powder logical hydrogen reducing 75min in the reduction furnace that temperature is 1000 DEG C, will
Mixed powder sieving for standby after twice reduction.Mixed-powder after sizing weighs 2500g after stirring
Inserting mantle jacket, jacket is put into cold isostatic press and is pressed into the cylindrical billet of weight 2500g, and pressing pressure sets
It is scheduled on 3000Kg/cm2.The billet suppressed is carried out under hydrogen shield pre-sintering, and sintering temperature is
1300 DEG C, 10/boat of boat charge, sintering time is 60min, and pre-burned billet is placed in hydrogen shield
In incipient fusion agglomerating plant, under the blowout current of 90%, it is incubated 20mins carries out cooling down.Burn from incipient fusion
The billet taken out in knot equipment carries out B203 rotary blooming, cogging temperature 1650 DEG C, after move back through Medium frequency induction
Fire, B202 swages, B201 swages, wire drawing, align, cut, polish and polish after obtain.
Embodiment four differs only in embodiment one: rehenic acid ammonium is 64.82g, the tungsten trioxide powder of addition
For 1796.9g.Embodiment five differs only in embodiment two: rehenic acid ammonium is 43.21g, three oxygen of addition
Change tungsten powder is 1796.9g.Embodiment six differs only in embodiment three: rehenic acid ammonium is 43.21g, adds
The tungsten trioxide powder entered is 1796.9g.Embodiment seven differs only in embodiment one: rehenic acid ammonium is
64.82g, the tungsten trioxide powder of addition is 1778.0g.Embodiment eight differs only in embodiment two:
Rehenic acid ammonium is 64.82g, and the tungsten trioxide powder of addition is 1778.0g.Embodiment nine and the difference of embodiment three
Being only that: rehenic acid ammonium is 64.82g, the tungsten trioxide powder of addition is 1778.0g.
Embodiment ten differs only in embodiment seven: the tungsten trioxide powder of addition is replaced with 1765.8g
Blue tungsten powder.Embodiment 11 differs only in embodiment eight: replaced with by the tungsten trioxide powder of addition
1765.8g blue tungsten powder.Embodiment 12 differs only in embodiment nine: the tungsten trioxide powder that will add
Replace with 1765.8g indigo plant tungsten powder.
Embodiment 13 differs only in embodiment seven: the tungsten trioxide powder of addition is replaced with 1410g
Tungsten powder.Embodiment 14 differs only in embodiment eight: replaced with by the tungsten trioxide powder of addition
1410g tungsten powder.Embodiment 15 differs only in embodiment nine: replaced by the tungsten trioxide powder added
For 1410g tungsten powder.
Embodiment 16 differs only in embodiment seven: by the tungsten trioxide powder added and ammonium rhenate powder end
Replace with the tungsten using 1410g tungsten powder powder and 45g rhenium powder to obtain through nitrogen protection alcohol wet machinery ball milling
Rhenium pre-alloyed powder.Embodiment 17 differs only in embodiment eight: by add tungsten trioxide powder and
Ammonium rhenate powder end replaces with employing 1410g tungsten powder powder and 45g rhenium powder through nitrogen protection alcohol wet machinery ball milling
And the W-Re pre-alloyed powder obtained.Embodiment 18 differs only in embodiment nine: three oxygen that will add
Change tungsten powder and ammonium rhenate powder end is replaced and used 1410g tungsten powder powder and 45g rhenium powder wet through nitrogen protection alcohol
Machinery ball milling and the W-Re pre-alloyed powder that obtains.
Embodiment 19 differs only in embodiment seven: replaced with by the tungsten trioxide powder of addition
2176.8g ammonium paratungstate powder.Embodiment 20 differs only in embodiment eight: three oxidations that will add
Tungsten powder replaces with 2176.8g ammonium paratungstate powder.Embodiment 21 differs only in embodiment nine:
The tungsten trioxide powder of addition is replaced with 2176.8g ammonium paratungstate powder.
Electrode serviceability is tested.Test event includes striking performance test, anti-scorching performance test
Test with static characteristic of arc.Result is contrasted with wide variety of thorium in industrial production the most both at home and abroad.
Each electrode material composition is as shown in table 1:
Table 1
Striking performance test:
Experimental condition: a diameter of Φ 2.4mm, tip cone angle 45 degree, argon flow amount is 8L/min, and electrode is stretched
Go out length 3mm, arc length 3mm.Using straight polarity direct current mode, tungsten filament is negative electrode, and anode is water-cooled red copper.
Testing equipment: thyristor control DC TIG welding connects power supply, model YC-300TSP.Digital multimeter, type
Number DT9205A.Electronic balance JA1003.Result of the test: the test result of 1#, 2#, 3#, 4# electrode:
When 30A, 80A, 150A welding current, each repetition striking 30 times, arcing initiation success rate reaches 100%, draws
Arc function admirable.And obtain the critical arcing voltage of each electrode under 30A electric current, be shown in Table 2.
The critical arcing voltage of each electrode under 30A electric current:
| Electrode is numbered | Critical arcing voltage (V) |
| 1 | 30 |
| 2 | 29 |
| 3 | 29 |
| 4 | 33 |
| 5 | 35 |
Table 2
Electron emission capability is measured:
The parameter of electron emission capability standard is mainly zero field current density and electron work functon.Measure as long as general
Go out zero field current density, just can be calculated electron work functon.
Method of testing: self-control with turbomolecular pump and the experimental provision of ionic pump, system limits vacuum is 6 ×
10-6Pa, tested negative electrode and anode load this device by flange, constitute planar diode structure, tested the moon
Pole can be heated in the apparatus, activated, ageing and carry out measurement of emitting performance, and in test process, vacuum keeps
3 × 10-5More than Pa.The same set of computer of this device controls measurement of emitting performance system and matches, and is calculating
Machine completes the automatic measurement of the I-V characteristic of pulse or direct-current emission under controlling, can automatically determine and provide null field
Emission current value.
Due to extra electric field and the common effect of transmitting electronic space charge, the Electric Field Distribution of negative and positive interpolar is except complete
Outside full rejection field or acceleration fields, an also transitional region, this region Electric Field Distribution makes negative and positive interpolar have one
Individual position electric-field intensity is zero, when this zero-field position falls cathode surface, obtains one and characterizes emission of cathode
The important parameter zero-field emission current density of ability, its theoretical value:
j0=AT2Exp(-Φ/kT)；
In formula:
j0, zero-field emission current density (A/m2)；
K, Boltzmann constant；
A, the emission ratio relevant with material, 120A/cm desirable for tungsten2K；
Φ, electron work functon；
T, absolute temperature (K)；
Electron work functon also has certain impact to striking performance, and during striking, electrode temperature gradually rises,
Discharge condition is progressively transitioned into arc discharge.High frequency voltage applied in high-frequency arc strike makes electrode with female exactly
Produce spark discharge between material, cause space to ionize, make welding circuit electric current incrementally increase to needed for arc discharge
In the range of.When Igniting pattern neutralizes the just starting the arc, electrode surface is not the most heated to sufficiently high temperature,
Can't work as hot cathode.If the work function of electrode surface is low, then electrode produces thermionic emission institute
The temperature needed is the lowest, and electrode the most easily produces thermionic emission, under certain voltage, and the electric current of welding circuit
Increase to the time needed for producing the electric current of arc discharge the fewest, i.e. the easiest success of the starting the arc.
Measurement result: shown that five kinds of materials are at 1300 DEG C of zero-field emission current density design effective electrons with 1500 DEG C
Work function.
Table 3 is various zero-field emission current densities at different temperatures:
Table 3
The various electron work functon at different temperatures of table 4:
Table 4
1～No. 4 compound rare-earth is compared with No. 5 thoriums at 1300～1500 DEG C, and zero-field emission current density is big, electronics
Work function is little, and thermionic emission ability is good.The work function of material directly reflects its thermionic emission ability.
The zero-field emission highest current density of No. 3 electrodes, electron work functon is minimum, and electron emissivity is best.Mainly
It is owing to the rhenium constituent content of No. 3 electrodes interpolations is close to the optimal solid solubility of W-Re alloy 3.5%, even tissue
Property is good, favourable to electron emission capability.Preferably No. 3 electrodes carry out industrial production key technology research.
Anti-scorching performance test
Test condition electrode diameter is Φ 2.4mm, and in test, anode used is water-cooled red copper, welding current 180A,
Arc duration 20min, electrode extension 3mm, arc length 3mm, argon flow amount 8L/min, electric current
Type and polarity are straight polarity direct current.
Test equipment thyristor control DC TIG welding connects power supply, model YC-300TSP.Slide measure, model
CN61M, electronic balance JA1003.Test result is shown in Table 5
The anti-scorching performance of radiationless multiplex composite rare-earth tungsten electrode
| Electrode is numbered | Quality (g) before arcing | Quality (g) after arcing | Mass lost (g) |
| 1 | 12.8320 | 12.8292 | 0.0029 |
| 2 | 12.9321 | 12.9304 | 0.0017 |
| 3 | 13.0656 | 13.0646 | 0.0010 |
| 4 | 12.8166 | 12.8128 | 0.0038 |
| 5 | 12.7867 | 12.7763 | 0.0104 |
Table 5
Wherein the average scaling loss amount of 1,2, No. 3 multiple elements design is more much smaller than No. 4 tri compounds, No. 5 thoriums,
Wherein No. 3 have optimal anti-scorching performance, and this is primarily due in 1～No. 3 electrode containing rhenium element, W-Re
Alloying effect makes tissue crystal grain tiny, Properties of High Temperature Creep and anti-yaw damper better performances.
Static characteristic of arc is tested
Experimental condition: a diameter of Φ 2.4mm, tip cone angle 45 degree, argon flow amount is 8L/min, and electrode is stretched
Go out length 3mm, arc length 3mm.Using straight polarity direct current mode, tungsten filament is negative electrode, and anode is water-cooled red copper.
Testing equipment: thyristor control DC TIG welding connects power supply (model YC-300TSP), digital multimeter (type
Number DT9205A), electronic balance (model JA1003) test method and result: after arcing, incite somebody to action back rapidly
Road electric current is adjusted to 20A, is 20A, 30A, 40A, 50A, 60A at electric current successively by order from small to large,
When 80A, 100A, 140A, after arc burning is stable, measure corresponding steady-state current, magnitude of voltage (as
Table 6), the electric arc Jing Te of 1#, 2#, 3#, 4#, 5# electrode is made respectively according to the voltage recorded, current value
Linearity curve (VA characteristic curve), as shown in Figure 1.
The various magnitude of voltage under different steady-state currents of table 6:
Table 6
It will be noted from fig. 1 that its static characteristic of arc curve of 1#, 2#, 3#, 4# electrode is superior to No. 5 thoriums,
1# electrode arc transfer curve is suitable with thorium.And the static characteristic of arc curve under big electric current, 1# electrode with
4# is suitable, 2# and 3# electrode is superior to 4#.This is mainly under big electric current high heat effect, along with rhenium content
Increasing, the ability that rhenium stablizes tungsten basal body tissue is higher, it is ensured that the uniformity of electrode tissue structure and monolithic stability
Property, so that the static characteristic of electric arc is preferable.
By welding performance test result above, it is known that set by the material composition of Composite and alloying
Meter, use the comprehensive welding performance of multiplex composite rare-earth prepared by conventional production technology the most met and exceeded thorium and
Tri compound, it is possible to substitute thorium under various operating modes, be truly realized radiationless.
It must be noted that some non-restrictive explanations that the present invention is simply made by above-described embodiment.But this area
Artisans will appreciate that, under without departing from the purpose and scope of the invention, the present invention can be made amendment,
Replace and change, these amendments, replace and change and still belong to protection scope of the present invention.
Claims (2)
1. a radiationless electrode material of multielement composite rare earth tungsten, it is characterized in that: containing lanthana, zirconium oxide, yittrium oxide, luteium oxide, rhenium and tungsten, wherein every kind of rare earth oxide accounts for this quality of materials percentage is 0.5% ~ 1.5%, it is 2% ~ 3% that total amount of the rare earth oxide accounts for this quality of materials percentage, it is 1% ~ 4% that alloying element rhenium accounts for this quality of materials percentage, and remaining is tungsten；
Wherein, the preparation method of described radiationless electrode material of multielement composite rare earth tungsten, comprise the following steps:
Step 1: with shared mass percent in the material, it is 0.5% ~ 1.5% by lanthana, zirconium oxide, yittrium oxide and luteium oxide every kind rare earth oxide content, four kinds of total amount of the rare earth oxide are 2% ~ 3%, rhenium is 1% ~ 4%, it is converted into lanthanum nitrate, zirconium nitrate, yttrium nitrate, lutecium nitrate and the amount of rehenic acid ammonium of correspondence, then weighs these compounds and be configured to mixed solution；
Step 2: with shared mass percent in the material, be 93% ~ 97% by tungsten, adds the tungstic acid of corresponding mass, blue tungsten, tungsten powder or ammonium paratungstate powder in above-mentioned mixed solution, stirs, and heat drying obtains mixed-powder；
Step 3: first by above-mentioned mixed-powder logical hydrogen reducing in reduction furnace, temperature is at 400 DEG C ~ 600 DEG C, and the time is 45min ~ 75min, and then the powder of gained continues in reduction furnace logical hydrogen reducing, temperature is at 700 DEG C ~ 900 DEG C, and the time is 45 min ~ 75min；By gained mixed-powder sieving for standby after twice reduction；
Step 4: the mixed-powder after above-mentioned reduction weighs 500g ~ 2500g after stirring and inserts mantle jacket, jacket is put into cold isostatic press and is pressed into cylindrical billet, and pressing pressure is set in 1000 Kg/cm2~3000 Kg/cm2；
Step 5: the billet suppressed is carried out under hydrogen shield pre-sintering, sintering temperature is 1100 DEG C ~ 1300 DEG C, 5/boat ~ 10 piece of boat charge/boat, time 30 min ~ 60min；
Step 6: pre-burned billet be placed in the incipient fusion agglomerating plant of hydrogen shield, is incubated 20min, cooling down under the blowout current of 90%；
Step 7: the billet after sintering incipient fusion carries out B203 rotary blooming, cogging temperature 1500 DEG C ~ 1650 DEG C, after through Medium frequency induction annealing, B202 swages, B201 swages, wire drawing, align, cut, polish and polish after obtain.
2. a preparation method for radiationless electrode material of multielement composite rare earth tungsten, is characterized in that: comprise the following steps:
Step 1: with shared mass percent in the material, it is 0.5% ~ 1.5% by lanthana, zirconium oxide, yittrium oxide and luteium oxide every kind rare earth oxide content, four kinds of total amount of the rare earth oxide are 2% ~ 3%, rhenium is 1% ~ 4%, it is converted into lanthanum nitrate, zirconium nitrate, yttrium nitrate, lutecium nitrate and the amount of rehenic acid ammonium of correspondence, then weighs these compounds and be configured to mixed solution；
Step 2: with shared mass percent in the material, be 93% ~ 97% by tungsten, adds the tungstic acid of corresponding mass, blue tungsten, tungsten powder or ammonium paratungstate powder in above-mentioned mixed solution, stirs, and heat drying obtains mixed-powder；
Step 3: first by above-mentioned mixed-powder logical hydrogen reducing in reduction furnace, temperature is at 400 DEG C ~ 600 DEG C, and the time is 45min ~ 75min, and then the powder of gained continues in reduction furnace logical hydrogen reducing, temperature is at 700 DEG C ~ 900 DEG C, and the time is 45 min ~ 75min；By gained mixed-powder sieving for standby after twice reduction；
Step 4: the mixed-powder after above-mentioned reduction weighs 500g ~ 2500g after stirring and inserts mantle jacket, jacket is put into cold isostatic press and is pressed into cylindrical billet, and pressing pressure is set in 1000 Kg/cm2~3000 Kg/cm2；
Step 5: the billet suppressed is carried out under hydrogen shield pre-sintering, sintering temperature is 1100 DEG C ~ 1300 DEG C, 5/boat ~ 10 piece of boat charge/boat, time 30 min ~ 60min；
Step 6: pre-burned billet be placed in the incipient fusion agglomerating plant of hydrogen shield, is incubated 20min, cooling down under the blowout current of 90%；
Step 7: the billet after sintering incipient fusion carries out B203 rotary blooming, cogging temperature 1500 DEG C ~ 1650 DEG C, after through Medium frequency induction annealing, B202 swages, B201 swages, wire drawing, align, cut, polish and polish after obtain.
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| CN104439763A (en) * | 2014-11-06 | 2015-03-25 | 北矿新材科技有限公司 | Preparation method of multi-element composite rare earth doped tungsten powder |
| CN104874943B (en) * | 2015-05-18 | 2018-06-22 | 廊坊开发区阳雨钨业股份有限公司 | Inert gas-shielded arc welding is connect with tungsten bar production method |
| CN105328364A (en) * | 2015-11-27 | 2016-02-17 | 北京矿冶研究总院 | Preparation method of tungsten electrode material |
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| CN106964783A (en) * | 2017-04-21 | 2017-07-21 | 鹤山市沃得钨钼实业有限公司 | A kind of manufacture method of nano rare earth tungsten electrode |
| CN109226748B (en) * | 2018-08-15 | 2020-07-31 | 赣州虹飞钨钼材料有限公司 | Preparation method of composite tungsten electrode material |
| CN109352274B (en) * | 2018-11-06 | 2019-10-01 | 湖北第二师范学院 | One kind flexible can bend minimally invasive tungsten needle electrode surgery knife and its production method |
| CN110587176B (en) * | 2019-09-20 | 2020-11-20 | 北京矿冶科技集团有限公司 | Zirconia micro-doped tungsten electrode material, electrode, preparation method and use |
| CN111041315A (en) * | 2019-11-27 | 2020-04-21 | 洛阳爱科麦钨钼科技股份有限公司 | Quaternary composite rare earth tungsten alloy electrode material and preparation method thereof |
| CN113102747A (en) * | 2020-01-13 | 2021-07-13 | 天津大学 | Preparation method for doping rare earth oxide in metal powder for additive manufacturing |
| CN116890117B (en) * | 2023-07-26 | 2024-03-26 | 山东迈科钨钼科技股份有限公司 | Composite tungsten filament and preparation method thereof |
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