CN116120064A - Preparation method and application of accelerator irradiation target ceramic wafer - Google Patents
Preparation method and application of accelerator irradiation target ceramic wafer Download PDFInfo
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- CN116120064A CN116120064A CN202211534502.3A CN202211534502A CN116120064A CN 116120064 A CN116120064 A CN 116120064A CN 202211534502 A CN202211534502 A CN 202211534502A CN 116120064 A CN116120064 A CN 116120064A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 73
- 238000004062 sedimentation Methods 0.000 claims abstract description 49
- 238000001035 drying Methods 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000006228 supernatant Substances 0.000 claims abstract description 21
- 239000013049 sediment Substances 0.000 claims abstract description 20
- 238000005303 weighing Methods 0.000 claims abstract description 17
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 230000002093 peripheral effect Effects 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims description 27
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical group [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 23
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 23
- 229940075624 ytterbium oxide Drugs 0.000 claims description 23
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 10
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- ZCUFMDLYAMJYST-UHFFFAOYSA-N thorium dioxide Chemical compound O=[Th]=O ZCUFMDLYAMJYST-UHFFFAOYSA-N 0.000 claims description 5
- 229910003452 thorium oxide Inorganic materials 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 abstract description 11
- 239000000203 mixture Substances 0.000 abstract description 11
- 239000002245 particle Substances 0.000 abstract description 7
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 21
- 239000011224 oxide ceramic Substances 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 229910052691 Erbium Inorganic materials 0.000 description 4
- 229910052771 Terbium Inorganic materials 0.000 description 4
- 229910052745 lead Inorganic materials 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 238000000462 isostatic pressing Methods 0.000 description 3
- 229910052574 oxide ceramic Inorganic materials 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- 238000009827 uniform distribution Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The invention relates to a preparation method and application of an accelerator irradiation target ceramic wafer, comprising the following steps: measuring a dispersing agent, weighing powder, and dispersing the powder in the dispersing agent to obtain a uniform phase suspension; fully settling the homogeneous phase suspension to obtain a supernatant and a settled layer; removing supernatant, rinsing the sedimentation layer, and drying the rinsed sedimentation layer in the shade to obtain a dried sediment; performing peripheral correction on the shade-dried sediment; drying the mixture to obtain a dried product; and preparing the accelerator irradiation target ceramic wafer. The invention can realize high-density, large-size and uniform thin ceramic plates by a particle uniform sedimentation method without introducing other binders, and can prepare a complete ceramic plate with uniform density and low porosity by utilizing the particle size, loose density and dispersion solvent of powder, so that the ceramic plate can be used as an accelerator irradiation target making piece, and can meet the irradiation requirements of density, porosity and the like.
Description
Technical Field
The invention belongs to the field of ceramic preparation, and particularly relates to a preparation method and application of an accelerator irradiation target ceramic wafer.
Background
The ceramic powder is sintered to manufacture the ceramic sheet after demolding by isostatic pressing, but when manufacturing a thin ceramic sheet with high thickness uniformity requirement, the ceramic sheet is molded by adopting an isostatic pressing mode, and the thickness uniformity of the sheet cannot meet the index requirement due to non-uniform pressure in the isostatic pressing process.
Currently, solid targets commonly used for producing medical isotopes using accelerators are classified into metal-coated and metal/oxide ceramic target pieces. Wherein the oxide ceramic target plate needs different size and thickness according to the requirements of the target raw material, the reaction mechanism and the irradiation condition. Typically thin ceramic plates having a thickness of no more than 10mm.
The conventional thin ceramic plates are usually prepared by sintering, hot pressing, vapor deposition, wet preparation and the like, but the conditions of smaller preparation size and uneven preparation are usually encountered. In order to overcome the problems, various binders and additives are required to be added to realize uniform distribution of materials, and ceramic sheets with uniform distribution are prepared by high-pressure pressing and high-temperature sintering, wherein the thickness of the ceramic sheets is not less than 10mm. The similar method is as follows: publication No. CN102822115, "Corrosion resistant Member for semiconductor manufacturing apparatus and method for producing the same", requires sintering at a high temperature of 1500℃and sintering aid selected from the group consisting of Mg, ca and Sr, and hot pressing under an inert atmosphere, and is complicated in production method and difficult to realize. Publication No. CN104177085, a molybdenum-based temperature-stable microwave dielectric ceramic and a preparation method thereof. Wet preparation typically uses spin coating to prepare oxide ceramic films of uniform thickness, but also requires the addition of binders or precursors to achieve uniform distribution of the ceramic sheets, similar methods are seen in: publication No. CN101293770, "A Nb composite metal oxide dielectric ceramic film and method for preparing same", uses Nb 2 O 5 And (3) hydrolyzing after reacting with hot alkali, reacting the obtained gel with citric acid to obtain Nb-citric acid solution, and polymerizing, concentrating and esterifying the Nb-citric acid solution with other metal-citric acid solutions to obtain precursor liquid. The precursor solution is spin-coated on a clean substrate with a certain rotating speed, the spin-coating and treatment process is repeated as required after the drying at 120 ℃ and the pretreatment at 400-500 ℃, and finally the film is prepared by heat treatment at 500-900 ℃ for 0.5-1 hour, and the process flow is complex and the popularization difficulty is high depending on a spin-coating instrument.
Disclosure of Invention
Aiming at the problems, the preparation method of the accelerator irradiation target piece ceramic wafer comprises the following steps:
dispersing: measuring a dispersing agent, weighing powder, and dispersing the powder in the dispersing agent to obtain a uniform phase suspension;
sedimentation: fully settling the uniform phase suspension to obtain a supernatant and a settled layer;
and (5) drying in the shade: removing the supernatant, rinsing the sedimentation layer, and drying the rinsed sedimentation layer in the shade to obtain a dried sediment;
and (3) correction: performing peripheral correction or cutting on the shade-dried sediment;
sintering: covering the corrected top surface and bottom surface of the dried sediment with a covering sheet, and drying the sediment after applying fixed pressure on the covering sheet to obtain a dried object;
preparing an accelerator irradiation target piece ceramic plate: and taking out the dried object, and removing the pressure on the covering sheet to obtain the accelerator irradiation target ceramic sheet.
The further technical preferable scheme is as follows: the powder is ytterbium oxide or thorium oxide with granularity not more than 150 meshes.
The further technical preferable scheme is as follows: the loose density of the powder is not more than 3g/cm 3 。
The further technical preferable scheme is as follows: in the sedimentation step, the sedimentation speed is not more than 5mm/min.
The further technical preferable scheme is as follows: the dispersing agent is a solution with the density not less than 60% of the bulk density of the powder, and is selected from one of deionized water, saline solution and organic solution.
The further technical preferable scheme is as follows: the method for preparing the accelerator irradiation target ceramic wafer according to claim 5, wherein the organic solution is ethanol, diethyl ether, carbon tetrachloride, ethylene glycol or the like.
The further technical preferable scheme is as follows: when the dispersing agent is a saline solution, deionized water is selected to rinse the sedimentation layer until the pH value of the water phase is 5-7; when the dispersing agent is an organic solution, any one of ethanol, diethyl ether, carbon tetrachloride and ethylene glycol is selected to rinse the sedimentation layer, and the organic solvent attached to the surface of the sedimentation layer is washed off.
The further technical preferable scheme is as follows: the covering sheet is selected from any one of a highly polished metal sheet or a ceramic sheet, and in the sintering step, the sintering temperature is 500-700 ℃.
An accelerator irradiation target ceramic wafer and application thereof in accelerator irradiation.
The invention has the beneficial effects that: 1. the powder granularity of the ceramic manufactured by the method is not more than 150 meshes, the loose density is not more than 3g/cm < 3 >, the diameter is not less than 50mm, and the thickness is not more than 5mm, so that the manufacture of large-size uniform thin metal oxide ceramic sheets can be realized;
2. the invention can realize high-density, large-size and uniform thin ceramic plates by a particle uniform sedimentation method under the condition of not introducing other binders.
3. The invention can prepare the ceramic sheet with uniform density, low porosity and integrity by using the powder particle size, bulk density and dispersion solvent without high temperature and high pressure.
4. The ceramic plate manufactured by the method can be used as an accelerator irradiation target making piece, and can meet the irradiation requirements of density, porosity and the like.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
the preparation of the accelerator irradiation target piece ceramic wafer comprises the following steps:
weighing: weighing ytterbium oxide powder for standby, wherein the ytterbium oxide powder contains 0.001% of each of oxides of Tb, dy, ho, lu, Y, fe, ni, zn and Pb, 0.01% of each of oxides of Er, tm, si and Ca, and under the condition of no addition of a binder and a sintering aid, selecting powder with granularity not more than 150 meshes and bulk density not more than 3g/cm < 3 >;
dispersing: weighing 20ml of aqueous solution, dispersing ytterbium oxide powder in the aqueous solution, and fully and uniformly mixing the ytterbium oxide powder and the aqueous solution through electromagnetic stirring to form uniform phase turbid liquid;
sedimentation: fully settling the suspension to obtain a supernatant and a settled layer; transferring the turbid liquid into a container with a diameter of 10cm and a detachable bottom, horizontally placing the container, uniformly settling the powder in the solution on the filter paper, and ensuring the settling speed of the powder to be not more than 5mm/min during settling.
And (5) drying in the shade: after powder sedimentation is completed, a sedimentation layer and supernatant are obtained, the supernatant is removed to obtain a sedimentation layer, and the sedimentation layer is placed in a dryer for drying in the shade to obtain a dried sediment;
and (3) correction: performing peripheral correction or cutting on the shade-dried sediment;
sintering: the powder sheet is clamped by two stainless steel sheets with the diameter not smaller than 10cm, two clamping blocks are added outside the powder sheet, the pressure not smaller than 0.1Mpa is provided, and the powder sheet is put into an oven for secondary drying. Drying, putting into a high-temperature furnace preheated at 700 ℃ for uniform sintering for 1 hour, and slowly cooling to room temperature. The ytterbium oxide ceramic flake with the size not less than 8 cm, the thickness of 5mm, the density of about 8.6g/cm < 3 > -8.7g/cm < 3 >, which is equivalent to 94% -95% of the theoretical density and the porosity of less than 10% is obtained.
Preparing an accelerator irradiation target piece ceramic plate: and taking out the dried object, slowly and uniformly removing the pressure on the covering sheet to obtain the accelerator irradiation target ceramic wafer.
The invention combines the wet preparation and static pressure sintering technology, and can realize the manufacture of large-size uniform thin metal oxide ceramic flakes by only utilizing proper powder granularity and loose packing density; in addition, the invention can prepare the high-density, large-size and uniform thin ceramic sheet by a particle uniform sedimentation method without introducing other binders, and the preparation method is simple and convenient to popularize.
Example 2:
the preparation of the accelerator irradiation target piece ceramic wafer comprises the following steps:
weighing: weighing thorium oxide powder for standby, and selecting powder with granularity not more than 150 meshes and loose packing density not more than 3g/cm < 3 > under the condition of no addition of a binder and a sintering aid;
dispersing: weighing 50ml of aqueous solution, dispersing ytterbium oxide powder in the aqueous solution, and fully and uniformly mixing the ytterbium oxide powder with the aqueous solution through electromagnetic stirring to form uniform phase turbid liquid;
sedimentation: fully settling the suspension to obtain a supernatant and a settled layer; transferring the turbid liquid into a container with a diameter of 10cm and a detachable bottom, horizontally placing the container, uniformly settling the powder in the solution on the filter paper, and ensuring the settling speed of the powder to be not more than 5mm/min during settling.
And (5) drying in the shade: after powder sedimentation is completed, a sedimentation layer and supernatant are obtained, the supernatant is removed to obtain a sedimentation layer, and the sedimentation layer is placed in air or a dryer for drying in the shade to obtain a dried sediment;
and (3) correction: performing peripheral correction or cutting on the shade-dried sediment;
sintering: the powder sheet is clamped by two stainless steel sheets with the diameter not smaller than 10cm, two clamping blocks are added outside the powder sheet, the pressure not smaller than 0.1Mpa is provided, and the powder sheet is put into an oven for secondary drying. And after drying, placing the mixture into a high-temperature furnace with the temperature of 700 ℃ and preheating, uniformly sintering the mixture for 1 hour, and slowly cooling the mixture to room temperature. The thorium oxide ceramic flake with the size not less than 8 cm, the thickness of 5mm, the density of about 8.6g/cm3-8.7g/cm3 and the porosity of less than 10 percent is obtained, which is equivalent to 94-95 percent of the theoretical density.
Preparing an accelerator irradiation target piece ceramic plate: and taking out the dried object, slowly and uniformly removing the pressure on the covering sheet to obtain the accelerator irradiation target ceramic wafer.
According to the invention, thorium oxide powder is used as a raw material, and a ceramic sheet with uniform density, low porosity and integrity can be prepared by combining a wet preparation method and a sintering preparation method without high-temperature and high-pressure conditions.
Example 3:
the preparation of the accelerator irradiation target piece ceramic wafer comprises the following steps:
weighing: weighing ytterbium oxide powder for standby, wherein the ytterbium oxide powder contains 0.001% of each of oxides of Tb, dy, ho, lu, Y, fe, ni, zn and Pb, 0.01% of each of oxides of Er, tm, si and Ca, and under the condition of no addition of a binder and a sintering aid, selecting powder with granularity not more than 150 meshes and bulk density not more than 3g/cm < 3 >;
dispersing: measuring 50ml of ethanol of the organic solution, dispersing ytterbium oxide powder in the organic solution, and fully and uniformly mixing the ytterbium oxide powder and the organic solution through electromagnetic stirring to form uniform-phase turbid liquid;
sedimentation: fully settling the suspension to obtain a supernatant and a settled layer; introducing the suspension of the dispersed powder into a container which is placed in advance and has a detachable bottom and is larger than the filter paper with the diameter of more than 1.5mm of the ceramic wafer to be prepared, horizontally placing the container, uniformly settling the powder in the solution on the filter paper, and adding macromolecular organic solute during the settling period to ensure that the settling speed is not more than 5mm/min.
And (5) drying in the shade: after powder sedimentation is completed, a sedimentation layer and supernatant are obtained, the supernatant is removed to obtain the sedimentation layer, diethyl ether is used for rinsing the sedimentation layer, and ethanol solution attached to the surface is washed off;
the sedimentation layer is placed in air or a dryer for drying in the shade, and the process of cleaning the organic solvent by using ethanol, diethyl ether or carbon tetrachloride and the subsequent drying in the shade are carried out in a fume hood; when the amount of the organic solvent is large, the solvent is recovered as necessary. Obtaining a shade-dried sediment;
and (3) correction: performing peripheral correction or cutting on the shade-dried sediment;
sintering: the powder sheet is clamped by two stainless steel sheets with the diameter not smaller than 10cm, two clamping blocks are added outside the powder sheet, the pressure not smaller than 0.1Mpa is provided, and the powder sheet is put into an oven for secondary drying. And after drying, placing the mixture into a high-temperature furnace with the temperature of 700 ℃ and preheating, uniformly sintering the mixture for 1 hour, and slowly cooling the mixture to room temperature. The ytterbium oxide ceramic flake with the size not less than 8 cm, the thickness of 5mm, the density of about 8.6g/cm < 3 > -8.7g/cm < 3 >, which is equivalent to 94% -95% of the theoretical density and the porosity of less than 10% is obtained.
Preparing an accelerator irradiation target piece ceramic plate: and taking out the dried object, slowly and uniformly removing the pressure on the covering sheet to obtain the accelerator irradiation target ceramic wafer.
Example 4:
the preparation of the accelerator irradiation target piece ceramic wafer comprises the following steps:
weighing: weighing ytterbium oxide powder for standby, wherein the ytterbium oxide powder contains 0.001% of each of oxides of Tb, dy, ho, lu, Y, fe, ni, zn and Pb, 0.01% of each of oxides of Er, tm, si and Ca, and the granularity is not more than 150 meshes and the bulk density is not more than 3g/cm under the condition of no addition of binder and sintering aid 3 Is a powder of (2);
dispersing: weighing 30ml of 2mol/L hydrochloric acid solution, dispersing ytterbium oxide powder in the salt solution, and fully and uniformly mixing the ytterbium oxide powder with the salt solution through electromagnetic stirring to form uniform phase turbid liquid;
sedimentation: fully settling the suspension to obtain a supernatant and a settled layer; introducing the suspension of the dispersed powder into a container which is placed in advance and has a detachable bottom and is larger than the filter paper with the diameter of more than 1.5mm of the ceramic wafer to be prepared, horizontally placing the container, uniformly settling the powder in the solution on the filter paper, and adding macromolecular organic solute during the settling period to ensure that the settling speed is not more than 5mm/min.
And (5) drying in the shade: after powder sedimentation is completed, a sedimentation layer and supernatant are obtained, the supernatant is removed to obtain the sedimentation layer, and deionized water is used for rinsing the sedimentation layer until the process requirement is met;
drying the sedimentation layer in the air or a dryer in the shade to obtain a shade-dried sediment;
and (3) correction: performing peripheral correction or cutting on the shade-dried sediment;
sintering: clamping the powder sheet with two stainless steel sheets with diameter not smaller than 10cm, and adding two clamping blocks to provide a powder sheet with diameter not smaller thanAnd (3) placing the mixture into an oven under the pressure of 0.1Mpa for secondary drying. And after drying, placing the mixture into a high-temperature furnace with the temperature of 700 ℃ and preheating, uniformly sintering the mixture for 1 hour, and slowly cooling the mixture to room temperature. The obtained product has a size of not less than 8 cm, a thickness of 5mm, and a density of about 8.6g/cm 3 －8.7g/cm 3 The ceramic sheet is equivalent to 94% -95% of theoretical density, and the porosity is less than 10%.
Preparing an accelerator irradiation target piece ceramic plate: and taking out the dried object, slowly and uniformly removing the pressure on the covering sheet to obtain the accelerator irradiation target ceramic wafer.
The powder granularity of the ceramic manufactured by the method is not more than 150 meshes, the loose density is not more than 3g/cm < 3 >, the diameter is not less than 50mm, and the thickness is not more than 5mm, so that the manufacture of large-size uniform thin metal oxide ceramic sheets can be realized;
the invention can realize high-density, large-size and uniform thin ceramic plates by a particle uniform sedimentation method under the condition of not introducing other binders.
The invention can prepare the ceramic sheet with uniform density, low porosity and integrity by using the powder particle size, bulk density and dispersion solvent without high temperature and high pressure.
The ceramic plate manufactured by the method can be used as an accelerator irradiation target making piece, and can meet the irradiation requirements of density, porosity and the like.
Example 5:
the preparation of the accelerator irradiation target piece ceramic wafer comprises the following steps:
weighing: weighing ytterbium oxide powder for standby, wherein the ytterbium oxide powder contains 0.001% of each of oxides of Tb, dy, ho, lu, Y, fe, ni, zn and Pb, 0.01% of each of oxides of Er, tm, si and Ca, and under the condition of no addition of a binder and a sintering aid, selecting powder with granularity not more than 150 meshes and bulk density not more than 3g/cm < 3 >;
dispersing: weighing 50ml of aqueous solution, dispersing ytterbium oxide powder in the aqueous solution, and fully and uniformly mixing the ytterbium oxide powder with the aqueous solution through electromagnetic stirring to form uniform phase turbid liquid;
sedimentation: fully settling the suspension to obtain a supernatant and a settled layer; transferring the turbid liquid into a container with a diameter of 10cm and a detachable bottom, horizontally placing the container, uniformly settling the powder in the solution on the filter paper, and ensuring the settling speed of the powder to be not more than 5mm/min during settling.
And (5) drying in the shade: after powder sedimentation is completed, a sedimentation layer and supernatant are obtained, the supernatant is removed to obtain a sedimentation layer, and the sedimentation layer is placed in a dryer for drying in the shade to obtain a dried sediment;
and (3) correction: performing peripheral correction or cutting on the shade-dried sediment;
sintering: the powder sheet is clamped by two stainless steel sheets with the diameter not smaller than 10cm, two clamping blocks are added outside the powder sheet, the pressure not smaller than 0.1Mpa is provided, and the powder sheet is put into an oven for secondary drying. Drying, putting into a preheated high-temperature furnace at 500 ℃ for uniform sintering for 1 hour, and slowly cooling to room temperature. The ytterbium oxide ceramic flake with the size not less than 8 cm, the thickness of 5mm, the density of about 8.6g/cm < 3 > -8.7g/cm < 3 >, which is equivalent to 94% -95% of the theoretical density and the porosity of less than 10% is obtained.
Preparing an accelerator irradiation target piece ceramic plate: and taking out the dried object, slowly and uniformly removing the pressure on the covering sheet to obtain the accelerator irradiation target ceramic wafer.
It should be noted that the terms "first," "second," and the like herein are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate in order to describe the embodiments of the present application described herein.
Although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the accelerator irradiation target piece ceramic wafer is characterized by comprising the following steps of:
dispersing: measuring a dispersing agent, weighing powder, and dispersing the powder in the dispersing agent to obtain a uniform phase suspension;
sedimentation: fully settling the uniform phase suspension to obtain a supernatant and a settled layer;
and (5) drying in the shade: removing the supernatant, rinsing the sedimentation layer, and drying the rinsed sedimentation layer in the shade to obtain a dried sediment;
and (3) correction: performing peripheral correction or cutting on the shade-dried sediment;
sintering: covering the corrected top surface and bottom surface of the dried sediment with a covering sheet, and drying the sediment after applying fixed pressure on the covering sheet to obtain a dried object;
preparing an accelerator irradiation target piece ceramic plate: and taking out the dried object, and removing the pressure on the covering sheet to obtain the accelerator irradiation target ceramic sheet.
2. The method for preparing the accelerator irradiation target ceramic wafer according to claim 1, wherein the powder is ytterbium oxide or thorium oxide with the granularity not more than 150 meshes.
3. The method for producing an accelerator irradiation target ceramic wafer according to claim 2, wherein the bulk density of the powder is not more than 3g/cm 3 。
4. A method of producing an accelerator irradiation target ceramic wafer according to claim 3, wherein in the sedimentation step, the sedimentation velocity is not more than 5mm/min.
5. The method for preparing the accelerator irradiation target ceramic wafer according to claim 4, wherein the dispersing agent is a solution with a density not less than 60% of the bulk density of the powder, and the dispersing agent is one selected from deionized water, a saline solution and an organic solution.
6. The method for preparing the accelerator irradiation target ceramic wafer according to claim 5, wherein the organic solution is one selected from ethanol, diethyl ether, carbon tetrachloride and ethylene glycol.
7. The method for preparing the accelerator irradiation target ceramic wafer according to claim 6, wherein when the dispersing agent is a saline solution, deionized water is selected to rinse the sedimentation layer until the pH value of the water phase is 5-7; when the dispersing agent is an organic solution, any one of ethanol, diethyl ether, carbon tetrachloride and ethylene glycol is selected to rinse the sedimentation layer, and the organic solvent attached to the surface of the sedimentation layer is washed off.
8. The method for producing an accelerator irradiation target ceramic wafer according to claim 7, wherein the cover sheet is selected from any one of a highly polished metal sheet and a ceramic sheet, and the sintering temperature in the sintering step is 500 to 700 ℃.
9. An accelerator irradiation target ceramic wafer prepared according to the method of any one of claims 1 to 9.
10. Use of an accelerator irradiation target ceramic wafer according to claim 9 in accelerator irradiation.
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