CN104087903A - Molybdenum-sodium tube-type target material, manufacturing method of molybdenum-sodium tube-type target material and molybdenum-sodium target material - Google Patents
Molybdenum-sodium tube-type target material, manufacturing method of molybdenum-sodium tube-type target material and molybdenum-sodium target material Download PDFInfo
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- CN104087903A CN104087903A CN201410360172.XA CN201410360172A CN104087903A CN 104087903 A CN104087903 A CN 104087903A CN 201410360172 A CN201410360172 A CN 201410360172A CN 104087903 A CN104087903 A CN 104087903A
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- QMXBEONRRWKBHZ-UHFFFAOYSA-N [Na][Mo] Chemical compound [Na][Mo] QMXBEONRRWKBHZ-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 239000013077 target material Substances 0.000 title abstract 12
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000011734 sodium Substances 0.000 claims abstract description 31
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 27
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 27
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 21
- 239000011733 molybdenum Substances 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001257 hydrogen Substances 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000012545 processing Methods 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 229920000642 polymer Polymers 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 238000007872 degassing Methods 0.000 claims description 5
- 239000011812 mixed powder Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 238000003466 welding Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- 235000015424 sodium Nutrition 0.000 claims 8
- 238000007493 shaping process Methods 0.000 claims 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 229910000975 Carbon steel Inorganic materials 0.000 claims 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 2
- 239000010962 carbon steel Substances 0.000 claims 2
- 238000000280 densification Methods 0.000 claims 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical group [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims 2
- 239000010935 stainless steel Substances 0.000 claims 2
- 229910001220 stainless steel Inorganic materials 0.000 claims 2
- 229910052719 titanium Inorganic materials 0.000 claims 2
- 239000010936 titanium Substances 0.000 claims 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims 1
- 229910052786 argon Inorganic materials 0.000 claims 1
- 238000003754 machining Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 229910000029 sodium carbonate Inorganic materials 0.000 claims 1
- 235000017550 sodium carbonate Nutrition 0.000 claims 1
- 235000013024 sodium fluoride Nutrition 0.000 claims 1
- 239000011775 sodium fluoride Substances 0.000 claims 1
- 229940001516 sodium nitrate Drugs 0.000 claims 1
- 235000010344 sodium nitrate Nutrition 0.000 claims 1
- 239000004317 sodium nitrate Substances 0.000 claims 1
- 238000005476 soldering Methods 0.000 claims 1
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 5
- 229910001182 Mo alloy Inorganic materials 0.000 description 4
- 238000010073 coating (rubber) Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
Abstract
The invention provides a molybdenum-sodium tube-type target material, a manufacturing method of the molybdenum-sodium tube-type target material, and a molybdenum-sodium target material. The molybdenum-sodium target material comprises two metal elements namely molybdenum and sodium, wherein a micro-structure on a cross section of the molybdenum-sodium target material contains sodium phase enriched islands; and the largest area of each island is not more than 1mm<2>. The manufacturing method of the molybdenum-sodium tube-type target material mainly comprises the following step: preparing the high-purity and high-compactness molybdenum-sodium tube-type target material by virtue of working procedures namely powder mixing, briquetting, hydrogen sintering, hot isostatic pressing treatment and mechanical finished products processing. A produced magnetron sputtering molybdenum-sodium tube-type target material provided by the invention is low in cost, high in target material purity, high in density and large in finished product size.
Description
Technical field
The present invention relates to a kind of molybdenum alloy target and manufacture method thereof, especially relate to molybdenum sodium cast target and manufacture method and the molybdenum sodium target of a kind of rolling processing high purity, high-compactness.
Background technology
When the Nonrenewable energy resources such as electric power, coal, oil signal for help repeatedly, when energy problem becomes the bottleneck of restriction international community Economic development day by day, countries in the world are found new energy solution one after another.Sun power is the inexhaustible renewable energy sources of the mankind. is also clean energy, do not produce any environmental pollution.Therefore, solar energy power generating can occupy the important seat of world energy sources consumption in the near future, not only wants Substitute For Partial conventional energy resources, and will become the main body of world energy supplies.Tubulose molybdenum base target can be used for the back electrode preparation of thin-film solar cells, can greatly improve the open circuit voltage of thin-film solar cells, improves efficiency of conversion, and therefore in whole solar energy industry chain, demand is increasing.
Along with raising and the expanding economy of people's living standard, more and more people are more and more higher to the requirement of flat-panel monitor, are mainly manifested in maximization aspect and the quality aspect of flat-panel monitor.The maximization of flat-panel monitor requires the maximization of sputtered film, thereby requires the maximization of planar targets, the length of target has been proposed to more and more higher requirement.For meeting the requirement of length, traditional pass through the technique that several sections short targets are welded, weld seam has more fine structure and pore, causes etched inhomogeneously, and causes the inhomogeneous consequence of coat-thickness.And molybdenum base target is in welding region and fragility thereof, has comparison major rupture risk.
At present, the molybdenum alloy target that lacks high purity, high-compactness.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of molybdenum sodium cast target and manufacture method and molybdenum sodium target, makes the purity of molybdenum alloy target and density higher.
Technical solution of the present invention is:
The invention provides a kind of molybdenum sodium target, comprise molybdenum, two kinds of metallic elements of sodium, in the microtexture on the cross section of described molybdenum sodium target, have the isolated island of rich sodium phase, wherein, the maximum area of each isolated island is not more than 1 square of mm or 1mm
2.And then sodium element content is 1wt%～5wt%, the average grain size of rich molybdenum phase is not more than 200 μ m.
In addition, a kind of molybdenum sodium cast target of the present invention, wherein, described molybdenum sodium cast target comprises molybdenum, two kinds of metallic elements of sodium, and wherein sodium element content is 1wt%～5wt%.Above-mentioned molybdenum sodium cast target, wherein, the purity of described molybdenum sodium cast target is greater than 99.9%, and density is greater than 90%.
The manufacture method that the invention provides a kind of molybdenum sodium cast target, wherein, the method comprises the following steps:
Steps A, mixed powder: after Mo powder (molybdenum powder) and sodium source powder are weighed in proportion, mix with three-dimensional material mixer, wherein the massfraction of Na (sodium) element is 1wt%～5wt%;
Step B, briquetting: the powder mixing is formed to pipe by isostatic cool pressing;
Step C, hydrogen sintering: pressed compact is reduced in flowing hydrogen atmosphere sintering furnace to sintering;
Step D, carries out shaping by the pipe after hydrogen sintering, reaches target size;
Step e, as sheath material, carries out jacket by the pipe after shaping with stainless steel plate, carbon steel sheet or titanium plate, and the inwall of described pipe, outer wall and two ends are wrapped up;
Step F is carried out the pipe of jacket hot isostatic pressing densification place in hot isostatic pressing stove;
Step G, carries out machining by pipe after hot isostatic pressing densification, makes pipe reach size and the surfaceness of setting.
A kind of molybdenum sodium cast target making method of the present invention, wherein, described method comprises:
Steps A, standby powder, select the molybdenum mixing and the Sodium orthomolybdate powder of purity >99.95%, pack in rubber coating, at rubber coating, be inserted in columniform setting steel bushing outward, in described rubber coating, put into a core bar, this core bar is positioned at the central axis of described setting steel bushing, seals described rubber coating;
Step B, briquetting, passes through isostatic cool pressing briquetting by packaged powder together with setting steel bushing, forms the tubular type molybdenum sodium ingot with central shaft hole;
Step C, sintering, puts into process furnace sintering by described tubular type ingot blank;
Step D, hot isostatic pressing, carries out hip treatment by the ingot blank completing after sintering;
Step e, mechanical workout, by hollow forging via the molybdenum sodium pipe target that is machined to specified dimension.
Above-mentioned molybdenum sodium cast target making method, wherein, also comprises step after described step e:
Thermal treatment, the annealing furnace of molybdenum sodium hollow forging being put into vacuum, rare gas element or hydrogen atmosphere heats, and Heating temperature is 950 ℃～1450 ℃, and is incubated 1 hour～4 hours, afterwards furnace cooling;
Carry out again mechanical workout.
Above-mentioned molybdenum sodium cast target making method, wherein, the pressure of described hot isostatic pressing is 150MPa～190MPa, and temperature is 1400 ℃～1800 ℃, and the time is 3h～5h.
Above-mentioned molybdenum sodium cast target making method, wherein, is also included in described molybdenum and receives the step of adding polymer protective film on the surface of pipe target endoporus, and described polymer protective film is added on described molybdenum sodium pipe target internal surface via spraying or the mode of smearing.
By above explanation, learnt, the present invention has advantages of as follows really:
The present invention, by HIP blank band jacket is carried out to thermoplasticity processing, obtains and approaches after the rolling blank of finished product required thickness, then can obtain finished product molybdenum alloy target by milling, mill processing.Thermoplasticity processing cuts into thin stock material working method with respect to large thickness blank line, can significantly cut down finished cost on the one hand, can also significantly shorten the process-cycle on the other hand, enhances productivity.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of molybdenum sodium cast target making method of the present invention;
Fig. 2 is the metallographic structure figure in cross section of the molybdenum sodium cast target of the embodiment of the present invention, wherein, shows the isolated island of a plurality of rich sodium phases; (scale that adopts 50 μ m, magnification is 200 times);
Fig. 3 is the metallographic structure figure in cross section of the molybdenum sodium cast target of the embodiment of the present invention, wherein, shows the isolated island (scale that adopts 20 μ m, magnification is 500 times) of single rich sodium phase;
Fig. 4 be the embodiment of the present invention molybdenum sodium cast target cross section metallographic structure figure wherein, show the isolated island (scale that adopts 20 μ m, magnification is 500 times) of the single rich sodium phase of another one.
Embodiment
For technical characterictic of the present invention, object and effect being had more clearly, understand, now contrast accompanying drawing explanation the specific embodiment of the present invention.
As shown in Figure 1, the manufacture method of a kind of molybdenum sodium cast target of the present invention, wherein, the method comprises the following steps:
Steps A, mixed powder: after Mo powder and Sodium orthomolybdate powder are weighed in proportion, mix with three-dimensional material mixer, wherein the massfraction of Na element is 1wt%～5wt%;
Step B, briquetting: the powder mixing is formed to pipe by isostatic cool pressing;
Step C, hydrogen sintering: pressed compact is reduced in flowing hydrogen atmosphere sintering furnace to sintering;
Step D, hip treatment: the molybdenum sodium pipe after sintering is put into hot isostatic pressing stove and carry out hip treatment (HIP);
Step e, mechanical workout: the pipe after HIP, through car and/or mill machining process, is prepared finished product.
A kind of molybdenum sodium cast target of the present invention, wherein, described molybdenum sodium cast target comprises molybdenum, two kinds of metallic elements of sodium, and wherein sodium element content is 1wt%～5wt%.Fig. 2 to Fig. 4 is the metallographic structure figure (or crystalline phase organization chart) in cross section of the molybdenum sodium cast target of the embodiment of the present invention, as shown in Figure 2, in microtexture on the cross section of molybdenum sodium target, comprise: the molybdenum element phase (background colour in figure, also can be called base phase) and be embedded in rich molybdenum phase 1 (conjunctive tissue of molybdenum and sodium) in molybdenum element phase (base phase), wherein, rich molybdenum forms the shape of a plurality of isolated islands mutually, and the maximum area of the isolated island of single rich sodium phase 1 is not more than 1mm
2, for example, be 0.2mm
2, 0.3mm
2, 0.6mm
2etc..Like this, rich sodium phase size is reasonable, is evenly distributed, and is conducive to form higher density and purity.
Above-mentioned molybdenum sodium cast target, wherein, the purity of described molybdenum sodium cast target is greater than 99.9%, and density is greater than 90%.Wherein, as shown in Figure 3 and Figure 4, rich molybdenum mutually 1 average grain size is not more than 200 μ m, for example, be 40 to 50 μ m, 85 to 95 μ m, 165 to 175 μ m etc.Molybdenum as rich in Fig. 3 mutually 1 grain-size is 46 μ m, and the rich molybdenum of Fig. 4 mutually 1 grain-size is 60 μ m.Like this, rich sodium phase size is less, distributes more even, is more conducive to form higher density and purity.
A kind of molybdenum sodium cast target making method of the present invention, wherein, described method comprises:
Steps A, standby powder, select the molybdenum mixing and the Sodium orthomolybdate powder of purity >99.95%, pack in rubber coating, at rubber coating, be inserted in columniform setting steel bushing outward, in described rubber coating, put into a core bar, this core bar is positioned at the central axis of described setting steel bushing, seals described rubber coating;
Step B, briquetting, passes through isostatic cool pressing briquetting by packaged molybdenum sodium powder together with setting steel bushing, forms the tubular type molybdenum ingot with central shaft hole;
Step C, sintering, puts into process furnace sintering by described tubular type molybdenum sodium ingot blank;
Step D, hot isostatic pressing, carries out hip treatment by the molybdenum ingot completing after sintering;
Step e, mechanical workout, by molybdenum sodium hollow forging via the molybdenum sodium pipe target that is machined to specified dimension.
Above-mentioned molybdenum sodium cast target making method, wherein, also comprises step after described step e:
Thermal treatment, the annealing furnace of molybdenum sodium hollow forging being put into vacuum, rare gas element or hydrogen atmosphere heats, Heating temperature is 950 ℃～1450 ℃, and be incubated 1～4h (hour), furnace cooling afterwards;
Carry out again mechanical workout.
Above-mentioned molybdenum sodium cast target making method, wherein, the pressure of described hot isostatic pressing is 150MPa～190MPa, and temperature is 1400 ℃～1800 ℃, and the time is 3h～5h.
Above-mentioned molybdenum sodium cast target making method, wherein, is also included in the step of adding polymer protective film on the surface of described molybdenum sodium pipe target endoporus, and described polymer protective film is added on described molybdenum sodium pipe target internal surface via the mode spraying or smear.As shown in Figure 2, in the microtexture on the cross section of molybdenum sodium target, comprising: molybdenum element phase and be embedded in the rich molybdenum phase (conjunctive tissue of molybdenum and sodium) of molybdenum element in mutually, wherein, the maximum area of the isolated island of rich sodium phase is not more than 1 square of mm (1mm
2).According to above-mentioned technique, can make molybdenum sodium cast target, certainly, can also in briquetting process, need not form the tubular type molybdenum ingot with central shaft hole, but form solid molybdenum ingot, thereby obtain molybdenum sodium target.
Take preferred embodiment of the present invention as example, illustrate it below and implement parameter and 4 concrete technical process:
The concrete technical process that table 1 molybdenum sodium cast target is made
Wherein, rich sodium phase size is rich sodium phase average size
In 4 projects above,, the particular case of projects is as follows:
In the 1st project, mixed powder parameter is: the massfraction of Na element is 1wt%, and briquetting parameter is: briquetting pressure is 50Mpa, the briquetting time be 5min (minute), sintering parameter is: 600 ℃ of sintering temperatures, sintering time 2h (hour), degassing parameter is: 400 ℃ of degassed temperature, and the degassed time is 2h, HIP parameter is: the pressure of hot isostatic pressing is 150Mpa, the temperature of hot isostatic pressing is 700 ℃, and the time of hot isostatic pressing is 3h, isolated island parameter: isolated island maximum area is 0.2mm
2, rich sodium phase size is 46 μ m.
In the 2nd project, mixed powder parameter is: the massfraction of Na element is 2wt%, and briquetting parameter is: briquetting pressure is 170Mpa, the briquetting time be 10min (minute), sintering parameter is: 800 ℃ of sintering temperatures, sintering time 6h (hour), degassing parameter is: 440 ℃ of degassed temperature, and the degassed time is 2h, HIP parameter is: the pressure of hot isostatic pressing is 170Mpa, the temperature of hot isostatic pressing is 700 ℃, and the time of hot isostatic pressing is 3h, isolated island parameter: isolated island maximum area is 0.3mm
2, rich sodium phase size is 90 μ m.
In the 3rd project, mixed powder parameter is: the massfraction of Na element is 3.5wt%, and briquetting parameter is: briquetting pressure is 230Mpa, the briquetting time be 15min (minute), sintering parameter is: 900 ℃ of sintering temperatures, sintering time 8h (hour), degassing parameter is: 520 ℃ of degassed temperature, and the degassed time is 2h, HIP parameter is: the pressure of hot isostatic pressing is 220Mpa, the temperature of hot isostatic pressing is 700 ℃, and the time of hot isostatic pressing is 3h, isolated island parameter: isolated island maximum area is 0.6mm
2, rich sodium phase size is 167 μ m.
In the 4th project, mixed powder parameter is: the massfraction of Na element is 5wt%, and briquetting parameter is: briquetting pressure is 300Mpa, the briquetting time be 20min (minute), sintering parameter is: 1000 ℃ of sintering temperatures, sintering time 10h (hour), degassing parameter is: 600 ℃ of degassed temperature, and the degassed time is 10h, HIP parameter is: the pressure of hot isostatic pressing is 250Mpa, the temperature of hot isostatic pressing is 1500 ℃, and the time of hot isostatic pressing is 5h, isolated island parameter: isolated island maximum area is 0.9mm
2, rich sodium phase size is 196 μ m.
The invention provides a kind of technique simple, production cost is low, and target purity is high, and density is high, the manufacture method of the magnetron sputtering molybdenum sodium cast target that final dimension is large.
In preferred embodiment, the technical side of integral body of the present invention can be by mainly comprising that the technical process of HIP operation completes the making of molybdenum sodium cast target: the powder of take is raw material via the molybdenum sodium ingot of hydrogen sintering; The cylindrical molybdenum sodium ingot of machined one-tenth specified dimension cylindrical and endoporus; After isostatic cool pressing (HIP) technique, further improve density; Be machined into again the finished product molybdenum sodium cast target of specified dimension.
According to above-mentioned purpose and whole technical scheme, the technical process of the concrete technical scheme of the present invention is: adopt the molybdenum sodium ingot of vacuum melting or powder metallurgy to prepare molybdenum sodium cast target through HIP technique.According to above-mentioned technique, can make molybdenum sodium cast target, certainly, can also in briquetting process, need not form the tubular type molybdenum ingot with central shaft hole, but form solid molybdenum ingot, thereby obtain molybdenum sodium target.
The foregoing is only the schematic embodiment of the present invention, not in order to limit scope of the present invention.Any those skilled in the art, not departing from equivalent variations and the modification of having done under the prerequisite of design of the present invention and principle, all should belong to the scope of protection of the invention.
Claims (11)
1. a molybdenum sodium target, comprises molybdenum, two kinds of metallic elements of sodium, it is characterized in that, in the microtexture on the cross section of described molybdenum sodium target, have the isolated island of rich sodium phase, wherein, the maximum area of each isolated island is not more than 1mm
2.
2. molybdenum sodium target as claimed in claim 1, is characterized in that, sodium element content is 1wt%～5wt%, and the average grain size of rich molybdenum phase is not more than 200 μ m.
3. a manufacture method for molybdenum sodium cast target, is characterized in that, the method comprises the following steps:
Steps A, mixed powder: after molybdenum powder and sodium source powder are weighed in proportion, mix with three-dimensional material mixer, wherein the massfraction of sodium element is 1wt%～5wt%;
Step B, briquetting: the powder mixing is formed to pipe by briquetting;
Step C, hydrogen sintering: pipe is reduced in flowing hydrogen atmosphere sintering furnace to sintering;
Step D, carries out shaping by the pipe after hydrogen sintering, reaches target size;
Step e, as sheath material, carries out jacket by the pipe after shaping with stainless steel plate, carbon steel sheet or titanium plate, and the inwall of described pipe, outer wall and two ends are wrapped up;
Step F is carried out the pipe of jacket hot isostatic pressing densification place in hot isostatic pressing stove;
Step G, carries out machining by pipe after hot isostatic pressing densification, makes pipe reach size and the surfaceness of setting.
4. the manufacture method of molybdenum sodium cast target as claimed in claim 3, is characterized in that, described sodium source is Sodium Fluoride, sodium carbonate, sodium bicarbonate, SODIUMNITRATE or Sodium orthomolybdate.
5. the manufacture method of molybdenum sodium cast target as claimed in claim 3, is characterized in that, described step F is specially: pack the pipe through shaping into jacket, then put into degasification furnace, limit heating edge is degassed, and vacuum tightness reaches 1 * 10
-2after Pa, with welding machine by jacket soldering and sealing.
6. the manufacture method of molybdenum sodium cast target as claimed in claim 3, it is characterized in that, tube blank size after shaping processing is 180mm * 250mm * 35mm, surfaceness is not more than Ra12.5, the material of jacket is stainless steel plate, carbon steel sheet or the titanium plate that 1.5mm is thick, jacket is of a size of 182mm * 252mm * 36mm, and any side jacket inwall is not more than 1.5mm with the gap between adjacent with it pipe.
7. the manufacture method of molybdenum sodium cast target as claimed in claim 5, is characterized in that, 400 ℃～600 ℃ of described degassed temperature, and described welding machine is argon welder or plasma welding machine.
8. the manufacture method of molybdenum sodium cast target as claimed in claim 5, is characterized in that, in step G, the pressure of described hot isostatic pressing is 150MPa～190MPa, and temperature is 700 ℃～1500 ℃, and the time is 3h～5h.
9. the making method of molybdenum sodium cast target as claimed in claim 3; it is characterized in that; also comprise: the step of adding polymer protective film in the inner wall surface of described molybdenum sodium cast target, described polymer protective film is added in the inner wall surface of described molybdenum sodium cast target via the mode spraying or smear.
10. a molybdenum sodium cast target, is characterized in that, described molybdenum sodium cast target comprises molybdenum, two kinds of metallic elements of sodium, and wherein sodium element content is 1wt%～5wt%.
11. molybdenum sodium cast targets as claimed in claim 10, is characterized in that, the purity of described molybdenum sodium cast target is greater than 99.9%, and density is greater than 90%.
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| CN201410360172.XA CN104087903A (en) | 2014-07-25 | 2014-07-25 | Molybdenum-sodium tube-type target material, manufacturing method of molybdenum-sodium tube-type target material and molybdenum-sodium target material |
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| CN201410360172.XA CN104087903A (en) | 2014-07-25 | 2014-07-25 | Molybdenum-sodium tube-type target material, manufacturing method of molybdenum-sodium tube-type target material and molybdenum-sodium target material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480437A (en) * | 2014-12-30 | 2015-04-01 | 山东昊轩电子陶瓷材料有限公司 | Production method for integrally formed cylindrical target |
| CN105112859A (en) * | 2015-09-17 | 2015-12-02 | 金堆城钼业股份有限公司 | Method for preparing Na-doped molybdenum planar targets |
| CN108103464A (en) * | 2017-11-21 | 2018-06-01 | 航天海鹰(哈尔滨)钛业有限公司 | A kind of preparation method of Fe, Al, Co, Cu, Cr, Mn alloy target material |
| CN108213440A (en) * | 2017-12-25 | 2018-06-29 | 安泰天龙钨钼科技有限公司 | A kind of preparation method of Mo Re alloys tubing |
| CN109097747A (en) * | 2018-09-12 | 2018-12-28 | 芜湖映日科技有限公司 | A kind of production method of cast target |
| CN109735809A (en) * | 2018-12-12 | 2019-05-10 | 金堆城钼业股份有限公司 | A kind of preparation method of large scale molybdenum base alkali metal alloy target |
| CN110396667A (en) * | 2019-07-01 | 2019-11-01 | 洛阳科威钨钼有限公司 | A kind of preparation method of molybdenum sodium alloy rotary target |
| CN111593305A (en) * | 2020-04-08 | 2020-08-28 | 辽宁工业大学 | Method for preparing molybdenum-sodium target material by doping sodium hydroxide |
| CN111850485A (en) * | 2019-04-29 | 2020-10-30 | 汉能新材料科技有限公司 | Preparation method of molybdenum alloy target |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102333606A (en) * | 2009-02-25 | 2012-01-25 | 克莱麦克斯工程材料有限公司 | Sodium/molybdenum powder compact and production method thereof |
| CN103045925A (en) * | 2013-01-29 | 2013-04-17 | 洛阳高新四丰电子材料有限公司 | Preparation process of sputtered rotary molybdenum-sodium-alloy tubular target |
| CN103160791A (en) * | 2013-03-26 | 2013-06-19 | 无锡舒玛天科新能源技术有限公司 | Preparation method of sodium-doped molybdenum plane sputtering target material |
| CN103320756A (en) * | 2013-06-20 | 2013-09-25 | 安泰科技股份有限公司 | Method for preparing high-purity, high-density and large-size molybdenum alloy target |
| CN103572229A (en) * | 2013-11-05 | 2014-02-12 | 研创应用材料（赣州）有限公司 | Preparation method of flexible base material and thin film for vacuum reel-to-reel coating |
| CN103567445A (en) * | 2012-07-25 | 2014-02-12 | 宁波江丰电子材料有限公司 | Manufacturing method of molybdenum targets |
-
2014
- 2014-07-25 CN CN201410360172.XA patent/CN104087903A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102333606A (en) * | 2009-02-25 | 2012-01-25 | 克莱麦克斯工程材料有限公司 | Sodium/molybdenum powder compact and production method thereof |
| CN103567445A (en) * | 2012-07-25 | 2014-02-12 | 宁波江丰电子材料有限公司 | Manufacturing method of molybdenum targets |
| CN103045925A (en) * | 2013-01-29 | 2013-04-17 | 洛阳高新四丰电子材料有限公司 | Preparation process of sputtered rotary molybdenum-sodium-alloy tubular target |
| CN103160791A (en) * | 2013-03-26 | 2013-06-19 | 无锡舒玛天科新能源技术有限公司 | Preparation method of sodium-doped molybdenum plane sputtering target material |
| CN103320756A (en) * | 2013-06-20 | 2013-09-25 | 安泰科技股份有限公司 | Method for preparing high-purity, high-density and large-size molybdenum alloy target |
| CN103572229A (en) * | 2013-11-05 | 2014-02-12 | 研创应用材料（赣州）有限公司 | Preparation method of flexible base material and thin film for vacuum reel-to-reel coating |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480437A (en) * | 2014-12-30 | 2015-04-01 | 山东昊轩电子陶瓷材料有限公司 | Production method for integrally formed cylindrical target |
| CN105112859A (en) * | 2015-09-17 | 2015-12-02 | 金堆城钼业股份有限公司 | Method for preparing Na-doped molybdenum planar targets |
| CN105112859B (en) * | 2015-09-17 | 2018-03-30 | 金堆城钼业股份有限公司 | A kind of preparation method of natrium doping molybdenum planar targets |
| CN108103464A (en) * | 2017-11-21 | 2018-06-01 | 航天海鹰(哈尔滨)钛业有限公司 | A kind of preparation method of Fe, Al, Co, Cu, Cr, Mn alloy target material |
| CN108103464B (en) * | 2017-11-21 | 2019-11-22 | 航天海鹰(哈尔滨)钛业有限公司 | A kind of preparation method of Fe, Al, Co, Cu, Cr, Mn alloy target material |
| CN108213440A (en) * | 2017-12-25 | 2018-06-29 | 安泰天龙钨钼科技有限公司 | A kind of preparation method of Mo Re alloys tubing |
| CN109097747A (en) * | 2018-09-12 | 2018-12-28 | 芜湖映日科技有限公司 | A kind of production method of cast target |
| CN109735809A (en) * | 2018-12-12 | 2019-05-10 | 金堆城钼业股份有限公司 | A kind of preparation method of large scale molybdenum base alkali metal alloy target |
| CN111850485A (en) * | 2019-04-29 | 2020-10-30 | 汉能新材料科技有限公司 | Preparation method of molybdenum alloy target |
| CN110396667A (en) * | 2019-07-01 | 2019-11-01 | 洛阳科威钨钼有限公司 | A kind of preparation method of molybdenum sodium alloy rotary target |
| CN111593305A (en) * | 2020-04-08 | 2020-08-28 | 辽宁工业大学 | Method for preparing molybdenum-sodium target material by doping sodium hydroxide |
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