CN104480319A - Preparation method of high-purity niobium ingot casting for radio frequency superconducting cavity - Google Patents
Preparation method of high-purity niobium ingot casting for radio frequency superconducting cavity Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-purity niobium ingot casting for a radio frequency superconducting cavity. The preparation method comprises performing vacuum electronic torch melting on a niobium batten for 3-7 times, thereby obtaining the high-purity niobium ingot casting; the specific electric energy of the vacuum electronic torch melting is 8-12 degrees per kilometer, and the vacuum degree of the vacuum electronic torch melting is not greater than 5*10<-3>Pa. The preparation method is reasonable in design, simple, simple and convenient to operate; the practical problems existing in the traditional niobium ingot casting production process can be effectively solved and the requirements on stabilized and large-scale production of the high-purity niobium ingot casting for the radio frequency superconducting cavity are met; the vacuum electronic torch melting is performed for 3-7 times, and by controlling the specific electric energy, the RRR value and the components of the prepared niobium ingot casting both conform to the requirements of the high-purity niobium ingot casting for the radio frequency superconducting cavity.
Description
Technical field
The invention belongs to High-purity Niobium ingot casting preparing technical field, be specifically related to a kind of preparation method of radio frequency superconducting cavity High-purity Niobium ingot casting.
Background technology
Radio frequency superconducting cavity is the key part making high-energy particle accelerator, and the metal niobium for the preparation of radio frequency superconducting cavity not only requires high purity, also exigent residual resistance rate (RRR).In recent years along with domestic, international going deep into high energy particle research, the research of high energy particle booster machinery and construction fast development, the demand for the preparation of the High-purity Niobium of radio frequency superconducting cavity is increasingly vigorous.RRR >=300 of service requirements ingot casting, require that chemical composition meets tantalum≤500ppm simultaneously; Silicon≤100ppm; Tungsten, molybdenum, titanium, zirconium, copper, chromium, nickel, iron all≤50ppm; Oxygen≤100ppm; Nitrogen≤50ppm, carbon≤20ppm, hydrogen≤10ppm.
But because the index request of RRR >=300 is very high, impurity element is to the reduction highly significant of RRR value.Traditional carbothermic method niobium bar foreign matter content is high, and after normal twice vacuum electron beam melting, the chemical composition of ingot casting and RRR value all do not reach the technical requirements of radio frequency superconducting cavity High-purity Niobium ingot casting.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of preparation method of radio frequency superconducting cavity High-purity Niobium ingot casting.The method is reasonable in design, method is simple, easy and simple to handle, effectively can solve the practical problems existing for traditional niobium ingot casting production technique, reach the requirement of stabilization, mass production radio frequency superconducting cavity High-purity Niobium ingot casting, adopt 3 ~ 7 vacuum electron beam meltings, by control ratio electric energy, the RRR value of the niobium ingot casting of preparation and composition all meet the requirement of radio frequency superconducting cavity High-purity Niobium ingot casting.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of radio frequency superconducting cavity High-purity Niobium ingot casting, and it is characterized in that, the method is: carry out 3 ~ 7 vacuum electron beam meltings to niobium lath, obtain High-purity Niobium ingot casting; The ratio electric energy of described vacuum electron beam melting is 8 degree/kg ~ 12 degree/kg, and vacuum tightness is not more than 5 × 10
-3pa; RRR>=300 of described High-purity Niobium ingot casting, in High-purity Niobium ingot casting, the mass content of impurity is: tantalum < 500ppm, silicon≤100ppm, tungsten < 50ppm, molybdenum < 50ppm, titanium≤1ppm, zirconium≤1ppm, copper≤1ppm, chromium≤1ppm, nickel≤1ppm, iron≤1ppm, oxygen≤10ppm, nitrogen < 10ppm, carbon < 10ppm, hydrogen < 1ppm.
The preparation method of above-mentioned a kind of radio frequency superconducting cavity High-purity Niobium ingot casting, is characterized in that, described niobium lath is the niobium lath that thermit reduction is produced.
The preparation method of above-mentioned a kind of radio frequency superconducting cavity High-purity Niobium ingot casting, it is characterized in that, in described niobium lath, the mass content of impurity is: tantalum≤420ppm, silicon≤100ppm, tungsten < 50ppm, molybdenum < 50ppm, titanium≤10ppm, zirconium≤10ppm, copper≤10ppm, chromium≤10ppm, nickel≤10ppm, iron≤10ppm, oxygen < 500ppm, nitrogen < 100ppm, carbon < 100ppm.
The preparation method of above-mentioned a kind of radio frequency superconducting cavity High-purity Niobium ingot casting, is characterized in that, describedly successively increases than the increase of electric energy with vacuum electron beam melting number of times.
The preparation method of above-mentioned a kind of radio frequency superconducting cavity High-purity Niobium ingot casting, is characterized in that, is stripped off the skin on the ingot casting surface of melting and remove 1mm ~ 3mm after each melting, then by clean for the ingot casting washed with de-ionized water after stripping off the skin.
The present invention compared with prior art has the following advantages:
1, the present invention is reasonable in design, method is simple, easy and simple to handle, effectively can solve the practical problems existing for traditional niobium ingot casting production technique, reach the requirement of stabilization, mass production radio frequency superconducting cavity High-purity Niobium ingot casting.
2, the present invention adopts 3 ~ 7 vacuum electron beam meltings, and by control ratio electric energy, the RRR value of the niobium ingot casting of preparation and composition all meet the requirement of radio frequency superconducting cavity High-purity Niobium ingot casting.
Below by embodiment, technical solution of the present invention is described in further detail.
Embodiment
Embodiment 1
The niobium lath adopting thermit reduction to produce does raw material, and obtain niobium ingot casting through 3 vacuum electron beam meltings, the vacuum tightness of 3 vacuum electron beam meltings is all not more than 4 × 10
-3pa, ratio electric energy 9 degree/kg, 9.5 degree/kg and the 10 degree/kg successively of 3 vacuum electron beam meltings, and stripped off the skin on the ingot casting surface of melting after each melting and remove 3mm, then by clean for the ingot casting washed with de-ionized water after stripping off the skin.In niobium lath used, the mass content of impurity is: tantalum is 30ppm, and silicon is 70ppm; Tungsten≤10ppm, molybdenum≤10ppm, titanium≤10ppm, zirconium≤10ppm, copper≤10ppm, chromium≤10ppm, nickel≤10ppm, iron≤10ppm, oxygen is 100ppm, and nitrogen is 40ppm, carbon≤10ppm.
After testing, RRR value is 420 to niobium ingot casting prepared by the present embodiment, and the mass content of impurity is: tantalum is 35ppm, silicon≤1ppm, tungsten≤1ppm, molybdenum≤1ppm, titanium≤1ppm, zirconium≤1ppm, copper≤1ppm, chromium≤1ppm, nickel≤1ppm, iron≤1ppm, oxygen is 6.5ppm, nitrogen≤5ppm, carbon≤3ppm, hydrogen <1ppm.The RRR value of the niobium ingot casting of preparation and composition all meet the requirement of radio frequency superconducting cavity High-purity Niobium ingot casting.
Embodiment 2
The niobium lath adopting thermit reduction to produce does raw material, and obtain niobium ingot casting through 5 vacuum electron beam meltings, the vacuum tightness of 5 vacuum electron beam meltings is all not more than 3 × 10
-3pa, the ratio electric energy of 5 vacuum electron beam meltings is 8 degree/kg, 9 degree/kg, 10 degree/kg, 10.5 degree/kg and 11 degree/kg successively, and is stripped off the skin on the ingot casting surface of melting after each melting and remove 2mm, then by clean for the ingot casting washed with de-ionized water after stripping off the skin.In niobium lath used, the mass content of impurity is: tantalum is 320ppm, and silicon is 100ppm; Tungsten is 33ppm, and molybdenum is 40ppm, titanium≤10ppm, zirconium≤10ppm, copper≤10ppm, chromium≤10ppm, nickel≤10ppm, iron≤10ppm, and oxygen is 180ppm, and nitrogen is 60ppm, and carbon is 35ppm.
After testing, RRR value is 380 to niobium ingot casting prepared by the present embodiment, and the mass content of impurity is: tantalum is 35ppm, tungsten is 28ppm, and molybdenum is 16ppm, silicon≤1ppm, titanium≤1ppm, zirconium≤1ppm, copper≤1ppm, chromium≤1ppm, nickel≤1ppm, iron≤1ppm, oxygen is 8ppm, nitrogen≤7ppm, carbon≤6ppm, hydrogen <1ppm.The RRR value of the niobium ingot casting of preparation and composition all meet the requirement of radio frequency superconducting cavity High-purity Niobium ingot casting.
Embodiment 3
The niobium lath adopting thermit reduction to produce does raw material, and obtain niobium ingot casting through 7 vacuum electron beam meltings, the vacuum tightness of 7 vacuum electron beam meltings is all not more than 5 × 10
-3pa, the ratio electric energy of 7 vacuum electron beam meltings is 8 degree/kg, 9 degree/kg, 10 degree/kg, 10.5 degree/kg, 11 degree/kg, 11.5 degree/kg and 12 degree/kg successively, and after each melting, the ingot casting surface of melting is stripped off the skin and remove 1mm, then by clean for the ingot casting washed with de-ionized water after stripping off the skin.In niobium lath used, the mass content of impurity is: tantalum is 420ppm, and silicon is 90ppm; Tungsten is 42ppm, and molybdenum is 35ppm, titanium≤10ppm, zirconium≤10ppm, copper≤10ppm, chromium≤10ppm, nickel≤10ppm, iron≤10ppm, and oxygen is 320ppm, and nitrogen is 80ppm, and carbon is 55ppm.
After testing, RRR value is 310 to niobium ingot casting prepared by the present embodiment, and the mass content of impurity is: tantalum is 345ppm, tungsten is 33ppm, and molybdenum is 25ppm, silicon≤1ppm, titanium≤1ppm, zirconium≤1ppm, copper≤1ppm, chromium≤1ppm, nickel≤1ppm, iron≤1ppm, oxygen is 10ppm, nitrogen≤8ppm, carbon≤9ppm, hydrogen <1ppm.The RRR value of the niobium ingot casting of preparation and composition all meet the requirement of radio frequency superconducting cavity High-purity Niobium ingot casting.
The above; it is only preferred embodiment of the present invention; not any restriction is done to the present invention, every above embodiment is done according to invention technical spirit any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.
Claims (5)
1. a radio frequency superconducting cavity preparation method for High-purity Niobium ingot casting, is characterized in that, the method is: carry out 3 ~ 7 vacuum electron beam meltings to niobium lath, obtain High-purity Niobium ingot casting; The ratio electric energy of described vacuum electron beam melting is 8 degree/kg ~ 12 degree/kg, and vacuum tightness is not more than 5 × 10
-3pa; RRR>=300 of described High-purity Niobium ingot casting, in High-purity Niobium ingot casting, the mass content of impurity is: tantalum < 500ppm, silicon≤100ppm, tungsten < 50ppm, molybdenum < 50ppm, titanium≤1ppm, zirconium≤1ppm, copper≤1ppm, chromium≤1ppm, nickel≤1ppm, iron≤1ppm, oxygen≤10ppm, nitrogen < 10ppm, carbon < 10ppm, hydrogen < 1ppm.
2. the preparation method of a kind of radio frequency superconducting cavity High-purity Niobium ingot casting according to claim 1, is characterized in that, described niobium lath is the niobium lath that thermit reduction is produced.
3. the preparation method of a kind of radio frequency superconducting cavity High-purity Niobium ingot casting according to claim 2, it is characterized in that, in described niobium lath, the mass content of impurity is: tantalum≤420ppm, silicon≤100ppm, tungsten < 50ppm, molybdenum < 50ppm, titanium≤10ppm, zirconium≤10ppm, copper≤10ppm, chromium≤10ppm, nickel≤10ppm, iron≤10ppm, oxygen < 500ppm, nitrogen < 100ppm, carbon < 100ppm.
4. the preparation method of a kind of radio frequency superconducting cavity High-purity Niobium ingot casting according to claim 1, is characterized in that, describedly successively increases than the increase of electric energy with vacuum electron beam melting number of times.
5. the preparation method of a kind of radio frequency superconducting cavity High-purity Niobium ingot casting according to claim 1, is characterized in that, is stripped off the skin on the ingot casting surface of melting and remove 1mm ~ 3mm after each melting, then by clean for the ingot casting washed with de-ionized water after stripping off the skin.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107470530A (en) * | 2017-08-28 | 2017-12-15 | 西北有色金属研究院 | A kind of forging method of radio frequency superconducting cavity High-purity Niobium ingot |
| CN110643875A (en) * | 2019-11-05 | 2020-01-03 | 青岛理工大学 | Smelting method for preparing fine-crystal pure niobium ingot |
| CN117887982A (en) * | 2024-03-18 | 2024-04-16 | 承德天大钒业有限责任公司 | High-purity niobium ingot and preparation method thereof |
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| CN110643875A (en) * | 2019-11-05 | 2020-01-03 | 青岛理工大学 | Smelting method for preparing fine-crystal pure niobium ingot |
| CN110643875B (en) * | 2019-11-05 | 2020-12-25 | 青岛理工大学 | Smelting method for preparing fine-crystal pure niobium ingot |
| WO2021088608A1 (en) * | 2019-11-05 | 2021-05-14 | 青岛理工大学 | Smelting method for preparing fine crystalline pure niobium ingot |
| CN117887982A (en) * | 2024-03-18 | 2024-04-16 | 承德天大钒业有限责任公司 | High-purity niobium ingot and preparation method thereof |
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