CN115125474A - Seamless-connection high-temperature-resistant plasma electrode and preparation method thereof - Google Patents
Seamless-connection high-temperature-resistant plasma electrode and preparation method thereof Download PDFInfo
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- CN115125474A CN115125474A CN202210749600.2A CN202210749600A CN115125474A CN 115125474 A CN115125474 A CN 115125474A CN 202210749600 A CN202210749600 A CN 202210749600A CN 115125474 A CN115125474 A CN 115125474A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- FAYUQEZUGGXARF-UHFFFAOYSA-N lanthanum tungsten Chemical compound [La].[W] FAYUQEZUGGXARF-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910000858 La alloy Inorganic materials 0.000 claims abstract description 42
- 238000005245 sintering Methods 0.000 claims abstract description 40
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 24
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000010949 copper Substances 0.000 claims abstract description 23
- 229910052802 copper Inorganic materials 0.000 claims abstract description 23
- 239000001257 hydrogen Substances 0.000 claims abstract description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 19
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 19
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 238000004321 preservation Methods 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000011049 filling Methods 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 35
- 239000002245 particle Substances 0.000 claims description 26
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 150000002431 hydrogen Chemical class 0.000 claims description 8
- 150000002815 nickel Chemical class 0.000 claims description 5
- 239000012266 salt solution Substances 0.000 claims description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 abstract description 17
- 239000010937 tungsten Substances 0.000 abstract description 17
- 230000017525 heat dissipation Effects 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 3
- 238000009694 cold isostatic pressing Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- WLTSUBTXQJEURO-UHFFFAOYSA-N thorium tungsten Chemical compound [W].[Th] WLTSUBTXQJEURO-UHFFFAOYSA-N 0.000 description 6
- 229910001264 Th alloy Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 2
- 229910052776 Thorium Inorganic materials 0.000 description 2
- 229910001080 W alloy Inorganic materials 0.000 description 2
- 238000005219 brazing Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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Abstract
The invention provides a seamless connected high-temperature resistant plasma electrode and a preparation method thereof, wherein the method comprises the following steps: (1) placing a tungsten lanthanum alloy blank containing 1.0-3.0 mass% of lanthanum into an inner cavity of a sintering die; (2) putting copper powder into an inner cavity of a die, and covering and filling the tungsten lanthanum alloy blank; (3) placing the mixture into a sintering furnace, vacuumizing, introducing hydrogen, heating to 500-600 ℃, carrying out heat preservation treatment in a first temperature zone, introducing hydrogen, heating to 800-plus-one temperature of 900 ℃, carrying out heat preservation treatment in a second temperature zone, introducing hydrogen, heating to 1350-plus-one temperature of 1400 ℃, carrying out heat preservation in a third temperature zone, introducing nitrogen, cooling and cooling; (4) demolding to obtain a seamless connected high-temperature resistant plasma electrode; the plasma electrode preparation process effectively avoids gaps generated by sintering surfaces between copper and tungsten, realizes seamless combination between tungsten and copper, effectively improves the conductivity of the electrode, has excellent heat dissipation and low electron work function, and fully prolongs the service life of the plasma electrode.
Description
Technical Field
The invention relates to the technical field of thermal spraying electrodes, in particular to a seamless connected high-temperature resistant plasma electrode and a preparation method thereof.
Background
With the rapid development of modern industrial production, the automation performance of the existing waste gas treatment equipment is continuously improved. Exhaust gas treatment equipment realizes NH by using high-temperature ion flame 3 、SiH 4 、N 2 O, TMA, etc., and the plasma electrode used in the plasma torch assembly needs to combine the characteristics of high electrical and thermal conductivity.
Conventional plasma electrodes made of copper or copper alloys have been difficult to efficiently adapt for use in high temperature plasma torch assemblies. Although the existing copper-inlaid tungsten electrode which is formed by combining materials with different mechanical properties and physical properties has better high-temperature resistance and wear resistance than a single copper electrode to a certain extent, the existing copper-inlaid tungsten electrode is usually manufactured by combining a plasma electrode in modes of brazing, interference fit and the like. In the existing brazing combination mode, gaps and holes often exist in the plasma electrode made of tungsten, tungsten alloy and copper metal materials, the combination stability between tungsten and copper is poor, the combination surface of tungsten and copper gradually generates desoldering along with long-term high-temperature accumulation, the heat conduction is blocked, the current transmission capacity is reduced, the heat dissipation performance is poor, the burning loss resistance is low, and the problem that the service life of the electrode is short is caused. Therefore, there is a need for a process for manufacturing a seamless plasma electrode capable of resisting high-temperature plasma fire waste gas combustion, which not only needs to greatly enhance the uniformity and bonding strength between tungsten and copper materials, but also has excellent high-temperature resistance and conductivity, so as to sufficiently prolong the service life of the electrode.
Disclosure of Invention
In view of the above, the invention provides a seamless connected high-temperature resistant plasma electrode and a preparation method thereof, which not only realize seamless combination between tungsten and copper and tight and uniform combination, but also effectively improve the conductivity of the combined electrode, have excellent heat dissipation and low electron work function, and prolong the service life of the electrode.
The technical scheme of the invention is realized as follows:
the invention provides a preparation process of a seamless connection high-temperature resistant plasma electrode, which comprises the following steps:
step 1: placing a tungsten lanthanum alloy blank containing 1.0-3.0 mass% of lanthanum into an inner cavity of a sintering die;
step 2: putting copper powder into an inner cavity of a die, and covering and filling tungsten lanthanum alloy blanks;
and step 3: placing a sintering mold into a sintering furnace, vacuumizing the sintering furnace, introducing hydrogen with the flow rate of 300-500sccm, heating to 500-600 ℃ at the speed of 10-15 ℃/min, carrying out heat preservation treatment in a first temperature region for 30-40min, introducing 100-150sccm increment hydrogen, heating to 800-900 ℃ at the speed of 20-25 ℃/min, carrying out heat preservation treatment in a second temperature region for 60-80min, introducing 150-200sccm increment hydrogen, heating to 1350-1400 ℃ at the speed of 30-35 ℃/min, carrying out heat preservation in a third temperature region for 120-180min, introducing nitrogen, cooling and cooling;
and 4, step 4: and taking out the sintering mold, and demolding to obtain the seamless connected high-temperature resistant plasma electrode.
Further, the tungsten lanthanum alloy blank is prepared by mixing tungsten lanthanum powder and polyvinylpyrrolidone powder according to the mass ratio of (10-13) to (1-3), calcining at 180 ℃ for 30-40min under 150-.
More preferably, the mass percentage of lanthanum in the tungsten lanthanum powder is 2.0%.
Further, the tungsten lanthanum powder is mixed particle powder formed by mixing tungsten powder with the particle size of 0.5-1 mu m and lanthanum powder with the particle size of 8-15 mu m.
Further explaining, in the step 1, spraying a nickel salt solution on the outer surface of the tungsten lanthanum alloy blank, and drying the tungsten lanthanum alloy blank in a vacuum oven at 60-70 ℃ for 1-2 h.
More preferably, the nickel salt solution is a nickel acetate solution with the mass concentration of 0.1-1%.
Further, the copper powder is any one of red copper, oxygen-free copper or copper alloy, and the particle powder of the copper powder with the particle size of 0.5-3 mu m.
The seamless connected high-temperature resistant plasma electrode prepared according to the preparation process is structurally shown in figure 1.
Compared with the prior art, the invention has the beneficial effects that:
the high-temperature-resistant and seamless-connection plasma electrode prepared by the invention is mainly an electrode structure of copper-inlaid tungsten-lanthanum alloy formed by sintering tungsten-lanthanum alloy materials and copper in a combined manner, and is characterized in that a tungsten-lanthanum alloy blank containing lanthanum with certain mass and copper powder with low fineness are adopted, and three-section sintering treatment in different temperature regions is carried out, so that gaps are effectively prevented from being generated on a sintering surface between copper and tungsten under a high-temperature condition, and seamless combination between tungsten and copper is realized, therefore, energy consumption caused by gap discharge generated in the using process of the electrode is avoided, the combination is compact and uniform, the heat dissipation is excellent, the discharge is stable, the electronic work function is low, the burning loss resistance is excellent, and the plasma electrode performance is improved.
The plasma electrode of the copper-inlaid tungsten-lanthanum alloy prepared by the invention not only well avoids the situation that the tungsten head is separated from the copper base due to different thermal expansion properties of copper and tungsten in the working process, but also has no radioactivity in the use process of the tungsten-lanthanum alloy material, and the service life of the electrode is improved by about 30 percent compared with that of tungsten-thorium alloy.
Drawings
FIG. 1 is a schematic structural diagram of a plasma electrode manufacturing process of the present invention, in which 1 is a mold, 2 is a W-La alloy blank, and 3 is copper powder.
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.
Example 1-a process for preparing a seamless joined high temperature resistant plasma electrode comprising the steps of:
step 1: placing a tungsten lanthanum alloy blank containing lanthanum with the mass of 1.0% into an inner cavity of a sintering mold; the tungsten lanthanum alloy blank is formed by performing cold isostatic pressing on tungsten lanthanum powder under the pressure of 300MPa to form a tungsten lanthanum alloy blank, the tungsten lanthanum powder is mixed particle powder formed by mixing tungsten powder with the particle size of 0.5-0.8 mu m and lanthanum powder with the particle size of 8-10 mu m, and the mass percentage of lanthanum is 1.0%;
step 2: placing red copper powder with the particle size of 0.5-1 μm into an inner cavity of a die, and covering and filling tungsten-lanthanum alloy blanks;
and step 3: placing the sintering mold into a sintering furnace, vacuumizing the sintering furnace, introducing hydrogen with the flow rate of 300sccm, heating to 500 ℃ at the speed of 10 ℃/min, performing heat preservation treatment of a first temperature zone for 40min, introducing 100sccm increment hydrogen, heating to 800 ℃ at the speed of 20 ℃/min, performing heat preservation treatment of a second temperature zone for 80min, introducing 150sccm increment hydrogen, heating to 1350 ℃ at the speed of 30 ℃/min, performing heat preservation of a third temperature zone for 180min, introducing nitrogen, cooling and cooling;
and 4, step 4: and taking out the sintering mold, and demolding to obtain the seamless connection high-temperature-resistant plasma electrode.
Example 2-a process for preparing a seamlessly connected, high temperature resistant plasma electrode, comprising the steps of:
step 1: placing a tungsten lanthanum alloy blank containing lanthanum with the mass of 3.0% into an inner cavity of a sintering die; the tungsten lanthanum alloy blank is formed by performing cold isostatic pressing on tungsten lanthanum powder under the pressure of 350MPa to form a tungsten lanthanum alloy blank, the tungsten lanthanum powder is mixed particle powder formed by mixing tungsten powder with the particle size of 0.8-1 mu m and lanthanum powder with the particle size of 10-15 mu m, and the mass percentage of lanthanum is 3.0%;
step 2: placing red copper powder with the particle size of 1.5-3 mu m into an inner cavity of a die, and covering and filling the tungsten lanthanum alloy blank;
and step 3: placing the sintering mold into a sintering furnace, vacuumizing the sintering furnace, introducing hydrogen with the flow rate of 500sccm, heating to 600 ℃ at the speed of 15 ℃/min, performing heat preservation treatment of a first temperature zone for 30min, introducing 150sccm increment hydrogen, heating to 900 ℃ at the speed of 25 ℃/min, performing heat preservation treatment of a second temperature zone for 60min, introducing 200sccm increment hydrogen, heating to 1400 ℃ at the speed of 35 ℃/min, performing heat preservation of a third temperature zone for 120min, introducing nitrogen, cooling and cooling;
and 4, step 4: and taking out the sintering mold, and demolding to obtain the seamless connected high-temperature resistant plasma electrode.
Example 3-a process for preparing a seamlessly connected, high temperature resistant plasma electrode, comprising the steps of:
step 1: placing a tungsten lanthanum alloy blank containing 2.0 mass percent of lanthanum into an inner cavity of a sintering die; the tungsten lanthanum alloy blank is formed by performing cold isostatic pressing on tungsten lanthanum powder under the pressure of 320MPa to form a tungsten lanthanum alloy blank, the tungsten lanthanum powder is mixed particle powder formed by mixing tungsten powder with the particle size of 0.6-0.8 mu m and lanthanum powder with the particle size of 10-12 mu m, and the mass percentage of lanthanum is 2.0%;
and 2, step: placing red copper powder with the particle size of 1-2 mu m into an inner cavity of a die, and covering and filling tungsten-lanthanum alloy blanks;
and 3, step 3: placing the sintering mold into a sintering furnace, vacuumizing the sintering furnace, introducing hydrogen with the flow of 400sccm, heating to 550 ℃ at the speed of 13 ℃/min, carrying out heat preservation treatment in a first temperature zone for 35min, introducing hydrogen with the increment of 120sccm, heating to 850 ℃ at the speed of 23 ℃/min, carrying out heat preservation treatment in a second temperature zone for 70min, introducing hydrogen with the increment of 180sccm, heating to 1400 ℃ at the speed of 33 ℃/min, carrying out heat preservation in a third temperature zone for 160min, introducing nitrogen, cooling and cooling;
and 4, step 4: and taking out the sintering mold, and demolding to obtain the seamless connected high-temperature resistant plasma electrode.
Example 4-a process for producing a seamless joined high temperature plasma electrode, such as the process for producing a plasma electrode of example 3, wherein the tungsten lanthanum alloy ingot is replaced with a tungsten lanthanum powder and polyvinylpyrrolidone powder, the mixture is calcined at 165 ℃ for 35min after being mixed at a mass ratio of 11:2, hydrogen is added for reduction at 180 ℃, and the tungsten lanthanum alloy ingot is formed by cold isostatic pressing under 320MPa, and the conditions of the other steps are the same as those of example 3.
Example 5-a process for preparing a seamless-connected high-temperature-resistant plasma electrode, such as the process for preparing the plasma electrode of example 4, wherein, in step 1, nickel acetate solution with a mass concentration of 0.1-1% is sprayed and coated on the outer surface of the prepared tungsten lanthanum alloy blank to completely cover the surface of the tungsten lanthanum alloy blank, and the tungsten lanthanum alloy blank is dried in a 65 ℃ vacuum oven for 2 hours and then placed in an inner cavity of a sintering mold; the rest of the procedure conditions were the same as in example 4.
Comparative example 1-process for manufacturing a plasma electrode, as in the method of manufacturing a plasma electrode of example 3, in step 1, a tungsten powder material having a particle size of 0.6 to 0.8 μm is used, and the material is cold isostatic pressed under a pressure of 320MPa to form a tungsten blank, which is placed in an inner cavity of a sintering mold; the rest of the procedure conditions were the same as in example 3.
Comparative example 2-process for producing a plasma electrode, like the process for producing a plasma electrode of example 3, in step 1, a tungsten-thorium alloy billet is used instead of a tungsten-lanthanum alloy billet, that is, the tungsten-thorium alloy billet is a tungsten-thorium alloy billet formed by subjecting tungsten-thorium powder to cold isostatic pressing under a pressure of 320MPa, the tungsten-thorium powder is a mixed particle powder formed by mixing tungsten powder having a particle size of 0.6 to 0.8 μm and thorium powder having a particle size of 10 to 12 μm, and the mass proportion of thorium is 2.0%; placing the mixture into an inner cavity of a sintering mold; the rest of the procedure conditions were the same as in example 3.
Example 6
The plasma electrode samples sintered by the preparation processes of the above examples 1 to 5 and comparative examples 1 to 2 were respectively subjected to tests of hardness, sintered density, conductivity, electron emission property and burnout resistance.
(1) Hardness: the Vickers hardness of the plasma electrode samples was measured using a digital display small load Vickers hardness tester model HVS-5 (the hardness values were averaged over 7 points).
(2) Sintering density: and testing the density of the plasma electrode sample by adopting a drainage method.
(3) Conductivity: the plasma electrode was measured for conductivity using a model HZ2522 digital sensitive micro-ohmmeter.
(4) Electronic work function: the electron work function of the plasma electrode at 2000 ℃ was measured using a WF-3 type electron work function tester.
The test results are shown in the following table 1:
TABLE 1
From the results in table 1, it is known that the plasma electrodes prepared in examples 1-3 have mechanical properties and physical properties significantly better than those of the plasma electrode prepared by combining single tungsten material and copper in comparative example 1, which indicates that the electrode structure of copper-inlaid tungsten-lanthanum alloy formed by sintering tungsten-lanthanum alloy material and copper in combination according to the present invention employs tungsten-lanthanum alloy blank containing a certain amount of lanthanum and low-fineness copper powder, and through sintering treatment in three different temperature regions, gaps generated on the sintered surface between copper and tungsten are effectively insulated, the bonding surface is compact and uniform without bubbles and gaps, the sintering hardness and density are significantly improved, and meanwhile, the plasma electrode has excellent heat dissipation, stable discharge, good conductivity and low electron work function, thereby greatly prolonging the service life of the plasma electrode.
Compared with the example 4, the density of the sintered plasma electrode material in the example 4 is further improved, and the electron work function is further reduced, which shows that in the preparation process of the tungsten-lanthanum alloy blank, the polyvinylpyrrolidone powder and the tungsten-lanthanum powder are added to be combined, and after low-temperature calcination and reduction treatment, the mixture is subjected to cold isostatic pressing to form the tungsten-lanthanum alloy blank, so that the mixing ductility and compactness of the tungsten-lanthanum powder are further promoted, tungsten, lanthanum and copper are uniformly and transitionally permeated in the sintering process, and seamless combination is realized. It can also be seen from example 5 that, by performing surface treatment on the tungsten lanthanum alloy blank by using a nickel salt solution with a certain concentration, the hardness and density after sintering are improved, the connection strength between the tungsten alloy and the copper is improved, the burning resistance of the plasma electrode is enhanced, and the service life of the electrode is fully prolonged.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A preparation process of a seamless connection high-temperature-resistant plasma electrode is characterized by comprising the following steps: the method comprises the following steps:
step 1: placing a tungsten lanthanum alloy blank containing 1.0-3.0 mass% of lanthanum into an inner cavity of a sintering die;
and 2, step: putting copper powder into an inner cavity of a die, and covering and filling tungsten lanthanum alloy blanks;
and step 3: placing a sintering mold into a sintering furnace, vacuumizing the sintering furnace, introducing hydrogen with the flow rate of 300-500sccm, heating to 500-600 ℃ at the speed of 10-15 ℃/min, carrying out heat preservation treatment in a first temperature region for 30-40min, introducing 100-150sccm increment hydrogen, heating to 800-900 ℃ at the speed of 20-25 ℃/min, carrying out heat preservation treatment in a second temperature region for 60-80min, introducing 150-200sccm increment hydrogen, heating to 1350-1400 ℃ at the speed of 30-35 ℃/min, carrying out heat preservation in a third temperature region for 120-180min, introducing nitrogen, cooling and cooling;
and 4, step 4: and taking out the sintering mold, and demolding to obtain the seamless connected high-temperature resistant plasma electrode.
2. The process of claim 1, wherein the process comprises the steps of: the tungsten lanthanum alloy blank is prepared by mixing tungsten lanthanum powder and polyvinylpyrrolidone powder according to the mass ratio of (10-13) to (1-3), calcining at 180 ℃ for 30-40min under 150-.
3. The process of claim 2, wherein the step of forming a seamless, high temperature resistant plasma electrode comprises: the mass percentage of lanthanum in the tungsten lanthanum powder is 2.0%.
4. The process of claim 3, wherein the step of forming a seamless, high temperature resistant plasma electrode comprises: the tungsten lanthanum powder is mixed particle powder formed by mixing tungsten powder with the particle size of 0.5-1 mu m and lanthanum powder with the particle size of 8-15 mu m.
5. The process of claim 1, wherein the process comprises the steps of: step 1, spraying a nickel salt solution on the outer surface of the tungsten lanthanum alloy blank, and drying the tungsten lanthanum alloy blank in a vacuum oven at 60-70 ℃ for 1-2 h.
6. The process of claim 5, wherein the step of forming a seamless, high temperature resistant plasma electrode comprises: the nickel salt solution is a nickel acetate solution with the mass concentration of 0.1-1%.
7. The process for preparing a seamlessly connected high-temperature resistant plasma electrode of claim 1, wherein: the copper powder is any one of red copper, oxygen-free copper or copper alloy, and the particle powder of the copper powder with the particle size of 0.5-3 mu m.
8. A seamless joined high temperature resistant plasma electrode prepared by the process of any one of claims 1 to 7.
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| CN115125474B (en) | 2024-03-22 |
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