CN108273994B - Preparation device and method of high-density molybdenum-niobium alloy target - Google Patents
Preparation device and method of high-density molybdenum-niobium alloy target Download PDFInfo
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- CN108273994B CN108273994B CN201810296517.8A CN201810296517A CN108273994B CN 108273994 B CN108273994 B CN 108273994B CN 201810296517 A CN201810296517 A CN 201810296517A CN 108273994 B CN108273994 B CN 108273994B
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- gypsum board
- upper side
- heat
- molybdenum
- target material
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- DTSBBUTWIOVIBV-UHFFFAOYSA-N molybdenum niobium Chemical compound [Nb].[Mo] DTSBBUTWIOVIBV-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910001257 Nb alloy Inorganic materials 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011248 coating agent Substances 0.000 claims abstract description 60
- 238000000576 coating method Methods 0.000 claims abstract description 60
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 59
- 239000010440 gypsum Substances 0.000 claims abstract description 59
- 239000002360 explosive Substances 0.000 claims abstract description 55
- 238000009413 insulation Methods 0.000 claims abstract description 23
- 239000004576 sand Substances 0.000 claims abstract description 23
- 239000013077 target material Substances 0.000 claims description 45
- 229910052720 vanadium Inorganic materials 0.000 claims description 27
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 27
- 239000000853 adhesive Substances 0.000 claims description 24
- 230000001070 adhesive effect Effects 0.000 claims description 24
- 238000000605 extraction Methods 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- -1 polyoxymethylene Polymers 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052681 coesite Inorganic materials 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 6
- 229920006324 polyoxymethylene Polymers 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 claims description 6
- 229910052682 stishovite Inorganic materials 0.000 claims description 6
- 229910052905 tridymite Inorganic materials 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000011435 rock Substances 0.000 claims description 3
- 125000005396 acrylic acid ester group Chemical group 0.000 claims 1
- 239000002131 composite material Substances 0.000 claims 1
- 238000005056 compaction Methods 0.000 abstract description 6
- 238000004880 explosion Methods 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000005474 detonation Methods 0.000 description 4
- 238000005477 sputtering target Methods 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 241000283074 Equus asinus Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- FFMMWFUIRQUAKA-UHFFFAOYSA-O azanium;2-methyl-1,3,5-trinitrobenzene;nitrate Chemical compound [NH4+].[O-][N+]([O-])=O.CC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O FFMMWFUIRQUAKA-UHFFFAOYSA-O 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
- B22F3/02—Compacting only
- B22F3/08—Compacting only by explosive forces
-
- 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
- B22F3/003—Apparatus, e.g. furnaces
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The application discloses a preparation device and a preparation method of a high-density molybdenum-niobium alloy target, wherein the device comprises a gypsum board (2), a target mold frame (4), a heat insulation layer (6), explosives (7) and detonators (8), and a heat collection coating (3) is arranged on the upper side of the gypsum board (2). The preparation method comprises the following operation steps: a. tamping the sand foundation (1) on a flat ground (9); b. placing a gypsum board (2) on the upper side of a sand base (1), coating a heat collecting coating (3) on the upper side of the gypsum board (2), placing a target template frame (4) with a target on the gypsum board (2), and placing the gypsum board for irradiation under sunlight; c. the temperature of the target reaches 80-90 ℃, and a heat insulation layer (6) is placed on the upper side of the target mold frame (4); d. and (3) placing the explosive (7) on the upper side of the heat insulation layer (6) within 2-3 min, and detonating. The device and the method adopt solar energy to preheat the molybdenum-niobium alloy target (5), and then adopt explosion compaction to prepare the high-density target with the density reaching 9.9g/cm 3, and meanwhile, the target has no cracks.
Description
Technical Field
The invention relates to a preparation device and a preparation method of a high-density molybdenum-niobium alloy target, and belongs to the technical field of display preparation.
Background
At present, molybdenum powder and niobium powder are placed in a mixing tank of a mixer to be stirred and mixed uniformly, and the molybdenum-niobium alloy sputtering target is obtained through the modes of cold isostatic pressing, presintering, hot isostatic pressing and the like. However, most of the density of the molybdenum-niobium alloy sputtering target material prepared by the method is lower than 9.0g/cm < 3 >, the quality requirement of the plane display industry which rapidly advances cannot be met, the density of the molybdenum-niobium target material can be improved by adopting an explosion compaction process, but the impact wave generated by explosion of explosive or impact of a flying piece is directly utilized to often lead the molybdenum-niobium target material to generate cracks, and even explosive damage is used for frying the molybdenum-niobium target material.
At present, the preheating method often has an electric heating method, the temperature can be accurately controlled by the advantage of the electric heating method, but the electric heating method generally needs an external electric donkey, so that the whole system is complex, an explosive detonator needs to avoid the heating process for safety, and the explosive detonator only slides into a sample area through a guide rail when detonating, but the safety cannot be ensured. The self-slow-heating high-temperature synthesis heating method (SHS) has the advantages of large reaction heat, quick reaction, no need of an external heat source and capability of preheating the powder, but the method has high heat insulation requirement on the explosive, and the multilayer heat insulation material is placed between the explosive and the powder, so that the shock wave propagation condition is complex, and the accurate control of the technological parameters is not facilitated.
Disclosure of Invention
The technical problem to be solved by the invention is that the density of the molybdenum-niobium alloy sputtering target material is mostly lower than 9.0g/cm < 3 >, and the quality requirement of the flat panel display industry can not be met; the device and the method for preparing the high-density molybdenum-niobium alloy sputtering target material are complex, and the technological parameters cannot be controlled accurately.
The technical scheme adopted for solving the technical problems is as follows: the preparation device of the high-density molybdenum-niobium alloy target comprises a gypsum board, a target mold frame, a heat insulation layer, explosives and detonators, wherein a heat collection coating is arranged on the upper side of the gypsum board.
The device further comprises a sand base, the gypsum board, the target material die frame, the heat insulation layer and the explosive are sequentially arranged from bottom to top, and the detonator is inserted into the middle of the explosive.
Wherein, in the device, the heat insulation layer material is an ultralow heat conduction PI film.
Wherein, the thickness of the heat-collecting coating in the device is 3-5 mm.
Wherein, the thickness of the gypsum board in the device is 15-20 mm.
Wherein, in the device, a heat collection coating is also arranged between the heat insulation layer and the target material die frame.
The target material die frame in the device is formed by splicing a plurality of panels.
Wherein, in the device, a heat collection coating is arranged on the side wall of the target material die frame.
Wherein, in above-mentioned device the explosive is the emulsion explosive of rock No.2, and thickness is: 0.33 to 0.44g/cm 2.
The method for preparing the high-density molybdenum-niobium alloy target comprises the following operation steps:
a. Tamping a sand foundation on a flat ground;
b. placing a gypsum board on the upper side of the sand base, coating a heat-collecting coating on the upper side of the gypsum board, placing a target template frame with a molybdenum-niobium alloy target inside on the upper side of the gypsum board, and placing the gypsum board for irradiation in sunlight;
c. The temperature of the molybdenum-niobium alloy target reaches 80-90 ℃, and a heat insulation layer is placed on the upper side of a target mold frame;
d. and (3) placing the explosive on the upper side of the heat insulation layer within 2-3 min, inserting the detonator into the middle part of the explosive, and detonating.
Wherein the heat-collecting coating in the step b in the device is formed by mixing vanadium extraction tailings and an adhesive at the temperature of 80-90 ℃, the vanadium extraction tailings account for 60-70% of the total mass of the vanadium extraction tailings and the adhesive, and the particle size of the vanadium extraction tailings is smaller than 74um; the adhesive is prepared from polyethylene glycol, polyoxymethylene, acrylic ester, polymethyl methacrylate and sodium styrene sulfonate, wherein the mass percentage of the adhesive is 70 percent to 20 percent to 8 percent to 1 percent in sequence; the preparation of the adhesive needs to be heated to 70-100 ℃; the vanadium extraction tailings contain TFe32.8％,TiO212.9％,V2O52.08％,MnO7.84％,SiO214.4％,Al2O33.2％,GaO2.5％,MgO3.57％,Cr2O32.24％, and the balance of unavoidable impurities.
And b, after the upper side of the gypsum board in the step b is coated with the heat collecting coating, placing the gypsum board for irradiation for a period of time, placing a target template frame internally provided with a molybdenum-niobium alloy target on the upper side of the gypsum board, and then placing the gypsum board for irradiation.
Wherein, in the step b of the device, hot water can be added to be mixed with the heat-collecting coating and then the mixture is smeared on the upper side of the gypsum board.
Wherein, in the step b, the clearance between the molybdenum-niobium alloy target and the target mould frame is 0.5-1 mm.
The beneficial effects of the invention are as follows: the device and the method are simple, and the required materials can be purchased and manufactured on site, so that the cost is low, and meanwhile, the requirements on manufacturing and using environments are low. The upper side of the gypsum board is coated with a heat-collecting coating, and the heat-collecting coating is directly irradiated by solar energy to indirectly heat the molybdenum-niobium alloy target. When the temperature reaches a certain level, the density of the molybdenum-niobium alloy target material can be improved from less than or equal to 9.0g/cm 3 to 9.9g/cm 3 by detonating the explosive, and meanwhile, the target material obtained by the device and the method can not generate cracks, has good sintering compaction effect, meets the quality requirement of the flat panel display industry, and can accurately control the technological parameters.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention.
Marked in the figure as: 1 is sand base, 2 is gypsum board, 3 is heat-collecting coating, 4 is target mould frame, 5 is molybdenum-niobium alloy target, 6 is insulating layer, 7 is explosive, 8 is detonator, 9 is flat ground.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
As shown in fig. 1, the preparation device of the high-density molybdenum-niobium alloy target material comprises a gypsum board 2, a target material mold frame 4, a heat insulation layer 6, an explosive 7 and a detonator 8, wherein a heat collection coating 3 is arranged on the upper side of the gypsum board 2. It will be appreciated by those skilled in the art that the device may be manufactured in situ, and that the plasterboard 2, the insulating layer 6, the explosive 7 and the detonator 8 may be purchased directly and the heat collecting coating 3 may be sprayed onto the plasterboard 2 in situ. The size of the molybdenum-niobium alloy target 5 manufactured according to the requirement is determined by the target mold frame 4.
Preferably, the device further comprises a sand base 1, wherein the sand base 1, the gypsum board 2, the target material mould frame 4, the heat insulation layer 6 and the explosive 7 are sequentially arranged from bottom to top, and the detonator 8 is inserted into the middle of the explosive 7. It will be appreciated by those skilled in the art that the present apparatus is further preferred to include the sand base 1, and that the sand base 1 of the present apparatus may be produced by stacking and compacting sand on site according to the site environment in actual operation, as long as the sand base 1 is used to buffer the force of explosion. Simultaneously, the sand base 1, the gypsum board 2, the target material die frame 4, the heat insulation layer 6 and the explosive 7 are sequentially stacked from bottom to top, so that the upper end face of the sand base 1 is contacted with the lower end face of the gypsum board 2, the upper end face of the target material die frame 4 is contacted with the lower end face of the heat insulation layer 6, the lower end face is contacted with the heat collection coating 3 on the upper end face of the gypsum board 2, and the target material die frame 4 is of a hollow tubular structure. The explosive 7 is directly placed on the insulating layer 6, and the detonator 8 is inserted into the explosive 7, so that the device can be manufactured. In actual use, the molybdenum-niobium alloy target 5 is only required to be placed on the target die frame 4. For further fixing the explosive 7, it may be preferable that the explosive 7 is a packaged and fixed block structure, so that the acting force during explosion is more stable. The gypsum board 2 of the device mainly plays a supporting role, so that other boards can be used.
Preferably, in the above device, the heat insulation layer 6 is an ultralow heat conduction PI film. As will be appreciated by those skilled in the art, since the molybdenum-niobium alloy target 5 is directly placed on the heat collecting coating 3, the temperature will gradually rise, and heat will be transferred from bottom to top to the explosive 7, which may cause self-detonation of the explosive 7, and there are certain uncontrollable factors. In consideration of this problem, the present device is provided with a heat insulating layer 6 below the explosive 7, and the present device is further preferably provided with an ultralow heat conductive PI film having a good heat insulating effect as the heat insulating layer 6.
Preferably, the thickness of the heat collecting coating 3 in the above device is 3-5 mm. It can be understood by those skilled in the art that, since the heat collecting coating 3 of the device is mainly used for preheating the molybdenum-niobium alloy target 5, the required heat is not too much, so that the thickness of the heat collecting coating 3 of the device is more preferably 3-5 mm, and the preheating effect of the device is satisfied.
Preferably, the gypsum board 2 in the above device has a thickness of 15 to 20mm. It will be appreciated by those skilled in the art that the present device is merely further preferred for gypsum board 2 thickness, as long as the support of the device is satisfied.
Preferably, a heat-collecting coating 3 is further disposed between the heat-insulating layer 6 and the target mold frame 4 in the above device. As will be appreciated by those skilled in the art, in consideration of the situation that the illumination intensity is insufficient, the preheating time will be increased, so it is further preferable that the heat collecting coating 3 is further disposed between the heat insulating layer 6 and the target mold frame 4, so that the area irradiated by the sunlight is further increased, the absorbed heat is more, the temperature is raised faster, and the thickness of the heat collecting coating 3 is further preferably 1-1.5 mm.
Preferably, in the above device, the target mold frame 4 is formed by splicing a plurality of panels. Those skilled in the art will appreciate that a single size mold frame is not suitable because the molybdenum niobium alloy target 5 sometimes is not uniform in size. Therefore, the target material die frame 4 is preferably formed by splicing the panels, and the device can be practically provided with jacks on the same panel, and plugs are arranged at the other ends of the jacks, so that the panels can be mutually spliced. Or the target material mold frame 4 which is matched with the molybdenum-niobium alloy target material 5 is connected and fixed by adopting screws or bolts and the like.
Preferably, in the above device, the heat collecting coating 3 is disposed on the side wall of the target mold frame 4. It will be appreciated by those skilled in the art that in order to further increase the contact area with sunlight and shorten the heating time, the device is further preferably provided with a heat collecting coating 3 on the side wall of the target mold frame 4.
Preferably, in the above device, the explosive 7 is rock emulsion explosive 7 No. 2, and the thickness is: 0.33 to 0.44g/cm 2. As will be appreciated by those skilled in the art, to further increase the force applied to the molybdenum niobium alloy target 5 during an explosion, the device further preferably comprises an explosive 7, namely a rock emulsion explosive 7, of number 2, and has a thickness of: 0.33 to 0.44g/cm 2.
The method for preparing the high-density molybdenum-niobium alloy target comprises the following operation steps:
a. Tamping the sand foundation 1 on a flat ground 9;
b. Placing a gypsum board 2 on the upper side of a sand base 1, coating a heat collecting coating 3 on the upper side of the gypsum board 2, placing a target material mould frame 4 internally provided with a molybdenum-niobium alloy target material 5 on the upper side of the gypsum board 2, and placing the gypsum board for irradiation in sunlight;
c. the temperature of the molybdenum-niobium alloy target 5 reaches 80-90 ℃, and a heat insulation layer 6 is placed on the upper side of the target mold frame 4;
d. And placing the explosive 7 on the upper side of the heat insulation layer 6 within 2-3 min, inserting the detonator 8 into the middle of the explosive 7, and detonating. It can be understood by those skilled in the art that the molybdenum-niobium alloy target 5 can be produced by performing the above steps in one step, and it should be noted that if the temperature in the step c does not reach the required 80 ℃, the irradiation time can be properly prolonged to make the temperature of the molybdenum-niobium alloy target 5 reach 80-90 ℃; if the temperature is too high, the thickness of the heat insulating layer 6 may be increased. The temperature of the molybdenum-niobium alloy target 5 can be measured by a thermometer or an electronic thermometer.
Preferably, the heat collection coating 3 in the step b in the device is formed by mixing vanadium extraction tailings and an adhesive at the temperature of 80-90 ℃, wherein the vanadium extraction tailings account for 60-70% of the total mass of the vanadium extraction tailings and the adhesive, and the particle size of the vanadium extraction tailings is smaller than 74um; the adhesive is prepared from polyethylene glycol, polyoxymethylene, acrylic ester, polymethyl methacrylate and sodium styrene sulfonate, wherein the mass percentage of the adhesive is 70 percent to 20 percent to 8 percent to 1 percent in sequence; the preparation of the adhesive needs to be heated to 70-100 ℃; the vanadium extraction tailings contain TFe32.8％,TiO212.9％,V2O52.08％,MnO7.84％,SiO214.4％,Al2O33.2％,GaO2.5％,MgO3.57％,Cr2O32.24％, and the balance of unavoidable impurities. It will be appreciated by those skilled in the art that the composition content and manufacturing requirements of the heat collecting coating 3 in step b are further preferred by the present process in order to achieve the final product quality of the present process.
Preferably, in the above device, after the upper side of the gypsum board 2 is coated with the heat collecting coating 3, the gypsum board can be placed under the sun for a period of time, then the target mold frame 4 with the molybdenum-niobium alloy target 5 inside is placed on the upper side of the gypsum board 2, and then the gypsum board is placed under the sun for irradiation. It will be appreciated by those skilled in the art that in order to uniformly heat up the molybdenum-niobium alloy target 5, it is further preferable that the method comprises the steps of first passing the upper heat collecting coating 3 of the gypsum board 2 through sunlight for a period of time and then placing the target mold frame 4 having the molybdenum-niobium alloy target 5 inside on the upper side thereof.
Preferably, in the above-mentioned apparatus, hot water may be added to the step b to mix with the heat collecting coating 3 and then it is applied to the upper side of the gypsum board 2. It will be appreciated by those skilled in the art that the present device is designed to closely attach the heat collecting coating 3 to the gypsum board 2 while uniformly distributing the heat collecting coating 3 on the gypsum board 2, and further preferably to add hot water to mix with the heat collecting coating 3 before applying it to the upper side of the gypsum board 2.
Preferably, in the step b, the gap between the molybdenum-niobium alloy target 5 and the target mold frame 4 is 0.5-1 mm. It will be appreciated by those skilled in the art that in order to prevent the molybdenum-niobium alloy target 5 from being convenient, the gap between the molybdenum-niobium alloy target 5 and the target mold frame 4 is preferably 0.5-1 mm.
Example 1
(1) Preparing a heat collection coating: ball milling is carried out on the existing vanadium extraction tailings or the vanadium extraction tailings subjected to reduction iron removal, and the particle size is smaller than 74 microns. Mixing with adhesive, extracting vanadium tailings: the adhesive=65%:35% and is mixed by heating at 85-95 ℃, wherein the mass ratio of polyethylene glycol to polyoxymethylene to acrylic ester to polymethyl methacrylate to sodium styrene sulfonate is 70%:20%:8%:1%, the main component of the vanadium extraction tailings is TFe32.8％,TiO212.9％,V2O52.08％,MnO7.84％,SiO214.4％,Al2O33.2％,GaO2.5％,MgO3.57％,Cr2O32.24％,, and the adhesive is prepared by heating at 70-100 ℃, and is properly mixed with hot water for coating on the gypsum board 2 for the convenience of coating, and the thickness is 3mm.
(2) The sand bed 1 was tamped onto a flat ground surface as shown in fig. 1 and a plasterboard 2 coated with a 3mm thick heat collecting coating 3 was placed. After the sunshine irradiates for 15min, a target material mold frame 4 device with a molybdenum-niobium alloy target material 5 is placed, a 1mm heat collecting coating 3 is coated on the upper side, the sunshine irradiates for 15min again, the temperature reaches about 80-90 ℃, an explosive 7 and a detonator 8 are prepared, an ultralow heat conduction PI film is placed on the target material within 3min, the explosive 7 is placed, the detonator 8 is inserted in the middle of the explosive 7, and the detonation is performed.
(3) And the preheated molybdenum-niobium alloy target 5 is subjected to explosive compaction to obtain the 3 molybdenum-niobium alloy target 5 with the density reaching 9.92g/cm, and the target has no cracks.
Example 2
(1) Preparing a heat collection coating: ball milling is carried out on the existing vanadium extraction tailings or the vanadium extraction tailings subjected to reduction iron removal, and the particle size is smaller than 74 microns. Mixing with adhesive, extracting vanadium tailings: the adhesive=60%:40% and is mixed by heating at 80-90 ℃, wherein the mass ratio of polyethylene glycol to polyoxymethylene to acrylic ester to polymethyl methacrylate to sodium styrene sulfonate is 70%:20%:8%:1%, the main component of the vanadium extraction tailings is TFe32.8％,TiO212.9％,V2O52.08％,MnO7.84％,SiO214.4％,Al2O33.2％,GaO2.5％,MgO3.57％,Cr2O32.24％,, and the adhesive is prepared by heating at 70-100 ℃, and is properly mixed with hot water for coating on the gypsum board 2 for the convenience of coating, and the thickness is 4mm.
(2) The sand bed 1 was compacted on a flat ground surface as shown in fig. 1 and a plasterboard 2 coated with a heat collecting coating 3 of 4mm thickness was put on. After the sunshine irradiates for 15min, a target material die frame 4 device with a molybdenum-niobium alloy target material 5 is placed, the upper side is coated with heat collecting coating material with the thickness of 1.5mm, the sunshine irradiates for 15min again, the temperature can reach about 80-90 ℃, an explosive 7 and a detonator 8 are prepared, an ultralow heat conduction PI film is placed on the target material within 3min, the explosive 7 is placed, the detonator 8 is inserted into the middle part of the explosive 7, and the detonation is performed.
(3) And the preheated molybdenum-niobium alloy target 5 is subjected to explosive compaction to obtain the 3 molybdenum-niobium alloy target 5 with the density reaching 9.90g/cm, and the target has no cracks.
Example 3
(1) Preparing a heat collection coating: ball milling is carried out on the existing vanadium extraction tailings or the vanadium extraction tailings subjected to reduction iron removal, and the particle size is smaller than 74 microns. Mixing with adhesive, extracting vanadium tailings: the adhesive=70%:30% and is mixed by heating at 85-100 ℃, wherein the mass ratio of polyethylene glycol to polyoxymethylene to acrylic ester to polymethyl methacrylate to sodium styrene sulfonate is 70%:20%:8%:1%, the main component of the vanadium extraction tailings is TFe32.8％,TiO212.9％,V2O52.08％,MnO7.84％,SiO214.4％,Al2O33.2％,GaO2.5％,MgO3.57％,Cr2O32.24％,, and the adhesive is prepared by heating at 70-100 ℃, and is properly mixed with hot water for coating convenience, and is coated on the gypsum board 2 with the thickness of 5mm.
(2) The sand bed 1 was compacted on a flat ground surface as shown in fig. 1 and a plasterboard 2 coated with a heat collecting coating 3 of 5mm thickness was put on. After the sunshine irradiates for 15min, a target material mold frame 4 device with a molybdenum-niobium alloy target material 5 is placed, a heat collecting coating with the thickness of 1.5mm is coated, the sunshine irradiates for 15min again, the temperature can reach about 80-90 ℃, an explosive 7 and a detonator 8 are prepared, an ultralow heat conduction PI film is placed on the target material within 3min, the explosive 7 is arranged, and the detonator 8 is inserted in the middle of the explosive 7 for detonation.
(3) And the preheated molybdenum-niobium alloy target 5 is subjected to explosive compaction to obtain the molybdenum-niobium alloy target 5 with the density reaching 9.94g/cm 3, and the target has no cracks.
Claims (4)
1. The preparation method of the high-density molybdenum-niobium alloy target material comprises the steps of using a preparation device comprising a gypsum board (2), a target material mould frame (4), a heat insulation layer (6), explosives (7) and detonators (8), wherein a heat collection coating (3) is arranged on the upper side of the gypsum board (2); the novel composite explosive material is characterized by further comprising a sand base (1), wherein the sand base (1), a gypsum board (2), a target material mold frame (4), a heat insulation layer (6) and an explosive (7) are sequentially arranged from bottom to top, and a detonator (8) is inserted into the middle of the explosive (7); the heat insulation layer (6) is made of an ultralow heat conduction PI film; the thickness of the heat-collecting coating (3) is 3-5 mm; the thickness of the gypsum board (2) is 15-20 mm; the explosive (7) is a No. 2 rock emulsion explosive (7) with the thickness of: 0.33-0.44 mm;
The method is characterized by comprising the following operation steps:
a. tamping the sand foundation (1) on a flat ground (9);
b. a gypsum board (2) is placed on the upper side of a sand base (1), a heat collecting coating (3) is coated on the upper side of the gypsum board (2), a target material mould frame (4) internally provided with a molybdenum-niobium alloy target material (5) is placed on the upper side of the gypsum board (2), and the gypsum board is placed for irradiation under sunlight;
c. the temperature of the molybdenum-niobium alloy target (5) reaches 80-90 ℃, and a heat insulation layer (6) is placed on the upper side of the target mold frame (4);
d. Placing an explosive (7) on the upper side of the heat insulation layer (6) within 2-3min, inserting a detonator (8) into the middle of the explosive (7), and detonating;
The heat collection coating (3) in the step b is formed by mixing vanadium extraction tailings and an adhesive at the temperature of 80-90 ℃, wherein the vanadium extraction tailings account for 60-70% of the total mass of the vanadium extraction tailings and the adhesive, and the particle size of the vanadium extraction tailings is smaller than 74um; the adhesive is prepared from polyethylene glycol, polyoxymethylene, acrylic acid ester, polymethyl methacrylate and sodium styrene sulfonate, wherein the mass percentage of the adhesive is 70 percent to 20 percent to 8 percent to 1 percent; the preparation of the adhesive needs to be heated to 70-100 ℃; the vanadium extraction tailings contain TFe 32.8％,TiO2 12.9％,V2O5 2.08％, MnO 7.84％,SiO2 14.4％,Al2O3 3.2％,GaO 2.5％,MgO 3.57％,Cr2O3 2.24％, and the balance of unavoidable impurities.
2. The method for preparing the high-density molybdenum-niobium alloy target material according to claim 1, which is characterized in that: in the step b, after the upper side of the gypsum board (2) is coated with the heat-collecting coating (3), the gypsum board is placed under the sun for a period of time, a target material mold frame (4) internally provided with a molybdenum-niobium alloy target material (5) is placed on the upper side of the gypsum board (2), and then the gypsum board is placed under the sun for irradiation; b, adding hot water and mixing with the heat-collecting coating (3) and then coating the mixture on the upper side of the gypsum board (2); in the step b, the clearance between the molybdenum-niobium alloy target (5) and the target mould frame (4) is 0.5-1 mm.
3. The method for preparing the high-density molybdenum-niobium alloy target material according to claim 1, which is characterized in that: a heat collection coating (3) is further arranged between the heat insulation layer (6) and the target material die frame (4); the target material die frame (4) is formed by splicing a plurality of panels.
4. The method for preparing the high-density molybdenum-niobium alloy target material according to claim 1, which is characterized in that: and a heat collection coating (3) is arranged on the side wall of the target material mold frame (4).
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| CN108977744A (en) * | 2018-09-12 | 2018-12-11 | 河北工业大学 | A kind of method that plasma spraying tailings in vanadium extraction prepares photothermal conversion coating |
| CN112475290A (en) * | 2020-11-16 | 2021-03-12 | 福州大学 | Powder compacting device and method based on metal foil gasification |
| CN114834080A (en) * | 2022-04-14 | 2022-08-02 | 安徽理工大学 | Spherical explosive shock wave compactor |
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