CN115466841A - Preparation method of high-purity niobium sheet for irradiation supervision neutron detection - Google Patents
Preparation method of high-purity niobium sheet for irradiation supervision neutron detection Download PDFInfo
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- CN115466841A CN115466841A CN202211116321.9A CN202211116321A CN115466841A CN 115466841 A CN115466841 A CN 115466841A CN 202211116321 A CN202211116321 A CN 202211116321A CN 115466841 A CN115466841 A CN 115466841A
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- niobium sheet
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- purity niobium
- sheet
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- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 38
- 239000010955 niobium Substances 0.000 title claims abstract description 38
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000001514 detection method Methods 0.000 title claims description 14
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 16
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000003723 Smelting Methods 0.000 claims abstract description 12
- 238000000605 extraction Methods 0.000 claims abstract description 12
- 238000005096 rolling process Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 9
- 238000010894 electron beam technology Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims abstract description 4
- 230000009467 reduction Effects 0.000 claims abstract description 4
- 238000007670 refining Methods 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 239000010937 tungsten Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000011265 semifinished product Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052785 arsenic Inorganic materials 0.000 claims description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000003344 environmental pollutant Substances 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 3
- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 claims description 3
- 239000012074 organic phase Substances 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 231100000719 pollutant Toxicity 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000008346 aqueous phase Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000005253 cladding Methods 0.000 abstract 2
- 230000001276 controlling effect Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/22—Remelting metals with heating by wave energy or particle radiation
- C22B9/228—Remelting metals with heating by wave energy or particle radiation by particle radiation, e.g. electron beams
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T3/00—Measuring neutron radiation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- General Physics & Mathematics (AREA)
- High Energy & Nuclear Physics (AREA)
- Molecular Biology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Toxicology (AREA)
- Plasma & Fusion (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a niobium sheet preparation technology field, which comprises the following steps: firstly, strictly selecting ores, and carrying out acid washing and anti-niobium extraction for multiple times by utilizing extraction equipment; secondly, carrying out aluminothermic reduction and horizontal electron beams, and controlling the content of impurity elements; thirdly, carrying out vacuum electron beam refining purification, and controlling the smelting speed, the smelting vacuum degree and the smelting power; fourthly, performing secondary pollution control on the whole process; and fifthly, rolling by adopting a pack rolling and cladding rolling process by taking the semi-finished high-purity niobium sheet as a cladding material. In the preparation process, the content of the residual elements except the tantalum element is strictly controlled, and the thickness of the niobium sheet is controlled, so that the finally prepared high-purity niobium sheet can accurately detect the 1.0MeV fast neutron.
Description
Technical Field
The invention relates to the technical field of niobium sheet preparation, in particular to a preparation method of a high-purity niobium sheet for irradiation supervision neutron detection.
Background
The irradiation supervision of ferrite materials of a reactor pressure vessel of a nuclear power station is an important measure for ensuring the safe operation of the reactor pressure vessel in a design life, the irradiation supervision of the reactor pressure vessel aims at monitoring the reactor core area of the reactor pressure vessel, namely the maximum fluence rate irradiation area of the reactor pressure vessel, the material performance change caused by neutron irradiation and thermal environment of ferrite parent metals and weld metals, and irradiation supervision data plays an important role in the safety assessment and the subsequent life extension assessment in the life after the operation of the nuclear power station;
the neutron detection materials recommended by the U.S. NRC regulatory code RG1.190 have the following 8 types: np-237, U-238, ni, fe, cu, ti, nb, and Co. The Np-237 and U-238 high-purity materials are in short supply and are limited in transportation, the current fast neutron detection materials of the nuclear power plant only use niobium, and high-purity niobium sheets suitable for neutron detection in irradiation supervision need to be prepared.
Disclosure of Invention
The invention aims to provide a preparation method of a high-purity niobium sheet for neutron detection in irradiation supervision, which aims to solve the preparation problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a high-purity niobium sheet for irradiation supervision neutron detection comprises the following steps:
firstly, selecting ores, and carrying out acid washing and anti-niobium extraction for multiple times by utilizing extraction equipment;
secondly, carrying out aluminothermic reduction and horizontal electron beams, and controlling the content of impurity elements;
thirdly, carrying out vacuum electron beam refining purification, and controlling the smelting speed, the smelting vacuum degree and the smelting power;
fourthly, performing secondary pollution control on the whole process, wherein the secondary pollution control comprises the cleaning of all items in the production and manufacturing process, so that secondary pollutants are not introduced in each manufacturing stage;
and fifthly, preparing a semi-finished product of the high-purity niobium sheet, and rolling by adopting the semi-finished product as a coating material through a stack rolling and coating rolling process to finally obtain the finished product of the high-purity niobium sheet.
Preferably, in the first step, ores are selected to control the content of harmful elements such as tungsten, phosphorus, arsenic and antimony in the ore raw materials.
Preferably, in the first step, in the extraction process, according to the difference of distribution coefficients of tantalum, tungsten, molybdenum and niobium, the hydrofluoric acid and sulfuric acid are decomposed in the acid washing process, and the high-purity fluoroniobium acid solution is obtained by extraction through organic phases such as sec-octanol, and the like, and then the high-purity niobium oxide is prepared by ammonia gas or ammonia water precipitation, washing, drying and roasting.
Preferably, in the second step, the tantalum content is controlled to be below 5ppm.
Preferably, in the fourth step, the whole process is ensured not to generate pollution of impurity elements.
Preferably, in the fifth step, the thickness of the high-purity niobium sheet is controlled not to exceed 0.020mm.
Preferably, the content of residual elements other than tantalum is controlled during the preparation process.
Preferably, the tantalum element content is less than 5ppm.
Compared with the prior art, the invention has the beneficial effects that:
1. in the preparation process, the content of the residual elements except the tantalum element is strictly controlled, and the thickness of the niobium sheet is controlled, so that the finally prepared high-purity niobium sheet can accurately detect the 1.0MeV fast neutron.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
The invention provides a technical scheme that: a preparation method of a high-purity niobium sheet for irradiation supervision neutron detection comprises the following steps:
strictly selecting ores, performing acid washing and anti-niobium extraction for multiple times by using extraction equipment, and selecting the ores to control the content of harmful elements such as tungsten, phosphorus, arsenic and antimony in the ore raw materials; in the extraction process, according to different distribution coefficients of tantalum, tungsten, molybdenum and niobium, in the pickling process, hydrofluoric acid and sulfuric acid are decomposed in water phase, and are extracted by organic phases such as sec-octanol and the like to obtain high-purity fluoroniobate solution, and then the high-purity niobium oxide is prepared by ammonia gas or ammonia water precipitation, washing, drying and roasting;
secondly, carrying out aluminothermic reduction and horizontal electron beams, and controlling the content of impurity elements, wherein the content of tantalum is controlled to be below 5ppm;
thirdly, carrying out vacuum electron beam refining purification, and controlling the smelting speed, the smelting vacuum degree and the smelting power to further improve the purity of the material;
fourthly, performing secondary pollution control on the whole process, wherein the whole process is required to be free from the pollution of impurity elements, and the secondary pollution control comprises the cleaning of all items in the production and manufacturing process, so that secondary pollutants are not introduced in each manufacturing stage, and the purity and the tantalum content of the high-purity niobium sheet finished product are ensured to meet the requirements;
fifthly, rolling by adopting a semi-finished high-purity niobium sheet as a coating material through a stack rolling and coating rolling process, wherein the thickness of the high-purity niobium sheet is required to be controlled not to exceed 0.020mm;
in the preparation process, the content of residual elements except tantalum is strictly controlled, and the content of the tantalum is less than 5ppm;
in the preparation process, the content of the residual elements except the tantalum element is strictly controlled, and the thickness of the niobium sheet is controlled, so that the finally prepared high-purity niobium sheet can accurately detect the 1.0MeV fast neutron.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A preparation method of a high-purity niobium sheet for irradiation supervision neutron detection is characterized by comprising the following steps:
firstly, selecting ores, and carrying out acid washing and anti-niobium extraction for multiple times by utilizing extraction equipment;
secondly, carrying out aluminothermic reduction and horizontal electron beams, and controlling the content of impurity elements;
thirdly, carrying out vacuum electron beam refining purification, and controlling the smelting speed, the smelting vacuum degree and the smelting power;
fourthly, performing secondary pollution control on the whole process, wherein the secondary pollution control comprises the cleaning of all items in the production and manufacturing process, so that secondary pollutants are not introduced in each manufacturing stage;
and fifthly, preparing a semi-finished product of the high-purity niobium sheet, and rolling by adopting the semi-finished product as a coating material through a stack rolling and coating rolling process to finally obtain the finished product of the high-purity niobium sheet.
2. The method for preparing a high-purity niobium sheet for irradiation supervision neutron detection according to claim 1, wherein in the first step, ores are selected to control the contents of harmful elements such as tungsten, phosphorus, arsenic and antimony in ore raw materials.
3. The method for preparing a high-purity niobium sheet for irradiation supervision neutron detection according to claim 1, wherein in the first step, according to the difference of distribution coefficients of tantalum, tungsten, molybdenum and niobium, the acid cleaning process is performed by decomposing with hydrofluoric acid and sulfuric acid aqueous phases, and performing extraction with organic phases such as sec-octanol to obtain a high-purity fluoroniobate solution, and then the high-purity niobium oxide is prepared by ammonia gas or ammonia water precipitation, washing, drying and roasting.
4. The method of claim 1, wherein in the second step, the tantalum content is controlled to be less than 5ppm.
5. The method for preparing a high-purity niobium sheet for irradiation monitoring neutron detection according to claim 1, wherein in the fourth step, the whole process is ensured not to generate impurity element pollution.
6. The method of claim 1, wherein in the fifth step, the thickness of the high-purity niobium sheet is controlled to be not more than 0.020mm.
7. The method of claim 1, wherein the content of residual elements other than tantalum is controlled during the preparation process.
8. The preparation method of a high-purity niobium sheet for irradiation monitoring neutron detection according to claim 8, wherein the content of tantalum is less than 5ppm.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210384999 | 2022-04-13 | ||
| CN2022103849999 | 2022-04-13 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115466841A true CN115466841A (en) | 2022-12-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211116321.9A Pending CN115466841A (en) | 2022-04-13 | 2022-09-14 | Preparation method of high-purity niobium sheet for irradiation supervision neutron detection |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115466841A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594611A (en) * | 2004-06-24 | 2005-03-16 | 株洲硬质合金集团有限公司 | Niobium purifying method |
| CN102978649A (en) * | 2012-12-14 | 2013-03-20 | 中国铝业股份有限公司 | Preparation method of high-purity gallium oxide |
| CN106929697A (en) * | 2017-04-18 | 2017-07-07 | 江苏圣亚有色金属材料有限公司 | A kind of purifying technique of pure niobium |
| CN112845590A (en) * | 2021-03-10 | 2021-05-28 | 宁夏东方钽业股份有限公司 | Metal foil and preparation method thereof |
-
2022
- 2022-09-14 CN CN202211116321.9A patent/CN115466841A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594611A (en) * | 2004-06-24 | 2005-03-16 | 株洲硬质合金集团有限公司 | Niobium purifying method |
| CN102978649A (en) * | 2012-12-14 | 2013-03-20 | 中国铝业股份有限公司 | Preparation method of high-purity gallium oxide |
| CN106929697A (en) * | 2017-04-18 | 2017-07-07 | 江苏圣亚有色金属材料有限公司 | A kind of purifying technique of pure niobium |
| CN112845590A (en) * | 2021-03-10 | 2021-05-28 | 宁夏东方钽业股份有限公司 | Metal foil and preparation method thereof |
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Address after: 753099 Yejin Road, Dawukou, Shizuishan City, Ningxia Hui Autonomous Region Applicant after: NINGXIA ORIENT TANTALUM INDUSTRY Co.,Ltd. Applicant after: Shanghai Nuclear Engineering Research and Design Institute Co.,Ltd. Address before: 753099 Yejin Road, Dawukou, Shizuishan City, Ningxia Hui Autonomous Region Applicant before: NINGXIA ORIENT TANTALUM INDUSTRY Co.,Ltd. Applicant before: SHANGHAI NUCLEAR ENGINEERING RESEARCH & DESIGN INSTITUTE Co.,Ltd. |