CN110357157B - Method for preparing nano niobium oxide by niobium ceramic chromatography process - Google Patents
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- CN110357157B CN110357157B CN201910598712.0A CN201910598712A CN110357157B CN 110357157 B CN110357157 B CN 110357157B CN 201910598712 A CN201910598712 A CN 201910598712A CN 110357157 B CN110357157 B CN 110357157B
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- 229910052758 niobium Inorganic materials 0.000 title claims abstract description 122
- 239000010955 niobium Substances 0.000 title claims abstract description 122
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 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 title claims abstract description 81
- 229910000484 niobium oxide Inorganic materials 0.000 title claims abstract description 80
- 239000000919 ceramic Substances 0.000 title claims abstract description 47
- 238000004587 chromatography analysis Methods 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000001035 drying Methods 0.000 claims abstract description 41
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000007873 sieving Methods 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 238000004806 packaging method and process Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract 2
- 239000007788 liquid Substances 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 26
- 239000002002 slurry Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000005070 sampling Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000003990 capacitor Substances 0.000 abstract description 3
- -1 targets Substances 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- MAKKVCWGJXNRMD-UHFFFAOYSA-N niobium(5+);oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] MAKKVCWGJXNRMD-UHFFFAOYSA-N 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 239000013077 target material Substances 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a method for preparing nano niobium oxide by a niobium ceramic chromatography process, which comprises the following steps: step S1 blending, step S2 chromatography preparation, step S3 drying, step S4 sieving, step S5 calcining, step S6 sieving, step S7 crushing, step S8 size mixing, step S9 dispersing, step S10 quick drying, step S11 air flow classification and step 12 packaging. The product has the characteristics of uniform particle size distribution, wide particle size range and good fluidity, can well meet the requirements of niobium oxide coating, targets, capacitors and batteries, and is highly praised by the requirements of users.
Description
Technical Field
The invention relates to the technical field of new rare metal material production, in particular to a method for preparing nano niobium oxide by a niobium ceramic chromatography process.
Background
Niobium oxide is a basic material for producing a niobium-coated material (target material). Niobium pentoxide (nb2O5) target is used as a material for sputtering coating in the fields of electrochromic films of optical interference filters, gas sensors and the like, and is a single-body ultrafine niobium oxide which is an important coating material of plasma displays and is widely used in the fields of ceramic capacitors, batteries and the like. However, with the development of high-tech materials, the demand of the fields such as target materials, capacitors and batteries on niobium oxide is higher and higher, and especially higher standards are provided for particle size, particle size distribution and fluidity.
Disclosure of Invention
The invention aims to solve the problems and designs a method for preparing nano niobium oxide by a niobium ceramic chromatography process.
The technical scheme of the invention is that the method for preparing the nano niobium oxide by the niobium ceramic chromatography process comprises the following steps: blending in step S1, preparing chromatography in step S2, drying in step S3, sieving in step S4, calcining in step S5, sieving in step S6, crushing in step S7, size mixing in step S8, dispersing in step S9, quick drying in step S10, airflow classification in step S11 and packaging in step 12;
step S1, putting the niobium liquid into a blending tank, determining pure water to be added before blending according to different acidity and concentration of the niobium liquid, and controlling the concentration of the niobium liquid to be 90-100 g/L and the acidity to be 3.3-5.0N;
step S2, the niobium liquid is stirred fully and blended, and then is slowly added into the niobium-based ceramic filter to form chromatography;
step S3, the niobium-based ceramic chromatographic filter which is sleeved with the niobium-based ceramic tray and is filled with niobium liquid is sent into a drying chamber together for low-temperature time-controlled chromatography and drying;
step S4, collecting niobium materials falling into the niobium-based ceramic tray after chromatography and drying, putting the niobium materials into a niobium crucible, sending the niobium crucible into an oven, controlling the temperature of the oven at 180-200 ℃, drying the niobium materials until the niobium materials are slightly twisted into powder by hands, crushing the powder and sieving the powder with a 60-mesh sieve;
step S5, loading the sieved niobium oxide into a niobium crucible, and calcining the niobium oxide in a calciner at a temperature range within a time range and a temperature range, wherein the calcining temperature is controlled at 600 ℃;
step S6, cooling the calcined niobium oxide and screening the cooled calcined niobium oxide through a 120-mesh classifying screen;
step S7, crushing the graded niobium oxide, thinning and crushing;
step S8: preparing the refined and crushed niobium oxide into slurry by pure water according to a certain proportion;
step S9, preparing niobium oxide into slurry for ultrasonic dispersion;
step S10, timely feeding the dispersed niobium oxide slurry into a quick drying furnace for quick drying;
step S11, classifying the dried niobium oxide airflow to obtain a nano niobium oxide product;
step S12: and after sampling and analyzing to be qualified, weighing, packaging and warehousing.
In the step S1, the concentration of the niobium solution is 100g/L, and the acidity is 5.5N.
In the step S1, the concentration of the niobium solution is 80g/L, and the acidity is 4.5N.
In the step S1, the concentration of the niobium solution is 90g/L, and the acidity is 5N.
And (8) after the chromatography and drying in the step S4 are finished, cleaning the outer wall of the niobium-based ceramic chromatography filter by using a clean brush.
And (4) putting the niobium oxide sieved in the step S5 into a niobium crucible, and calcining the niobium oxide in a calciner at 200 ℃ for 2 hours, 400 ℃ for 2 hours, 600 ℃ for 4 hours and 800 ℃ for 4 hours in different time intervals.
And in the step S8, pure water is mixed into niobium oxide slurry according to the liquid-solid ratio of 5: 1.
And in the step S9, sending the mixture into an ultrasonic disperser to carry out ultrasonic dispersion for 20 minutes.
And step S10, feeding the dispersed niobium oxide slurry into a rapid drying furnace to be rapidly dried for 30 minutes.
The method for preparing the nano niobium oxide by the niobium ceramic chromatography process, which is prepared by the technical scheme of the invention, well solves the problems of the niobium oxide such as particle size, particle size distribution and fluidity. The product has the characteristics of uniform particle size distribution, wide particle size range and good fluidity, can well meet the requirements of niobium oxide coating, targets, capacitors and batteries, and is highly praised by the requirements of users.
Detailed Description
The invention specifically describes a method for preparing high-purity niobium oxide by filtering a niobium ceramic membrane, which comprises the following steps:
the first embodiment is as follows:
1. the analysis shows that the concentration of the niobium liquid is 100g/L, and the acidity is 5.5N. According to the technological requirements, the total content of niobium oxide in a barrel (tank) of oxide is controlled to be 20Kg, and pure water is added to adjust the acidity of the niobium liquid to be 5.0N by calculation.
2. And after the niobium liquid is fully stirred and blended for 5 minutes, slowly adding the niobium liquid into the niobium-based ceramic chromatographic filter sleeved with the niobium-based ceramic tray.
3. And (3) conveying the niobium-based ceramic chromatographic filter which is filled with the niobium liquid and is sleeved with the niobium-based ceramic tray into a drying chamber for carrying out low-temperature time control chromatographic drying for 24 hours until the niobium liquid is chromatographed, and separating the niobium oxide hydrate from the outer wall of the niobium-based ceramic chromatographic filter.
4. And after the chromatography and the drying are finished, cleaning the outer wall of the niobium-based ceramic chromatography filter by using a clean brush, collecting niobium materials falling into a niobium-based ceramic tray, combining the niobium materials, putting the niobium materials into a niobium crucible, sending the niobium crucible into an oven, controlling the temperature of the oven at 180-200 ℃, drying the niobium crucible until the niobium materials are slightly twisted into powder by hand, cooling the powder, and crushing the powder into a 60-mesh sieve.
5. The sieved niobium oxide is filled into a niobium crucible and sent to a calcining furnace to be calcined at 200 ℃ for 2 hours, 400 ℃ for 2 hours, 600 ℃ for 4 hours and 800 ℃ for 4 hours in different time intervals.
6. Cooling the calcined niobium oxide, and sieving the cooled niobium oxide by a 120-mesh grading sieve.
7. And crushing and refining the graded niobium oxide, mixing the crushed niobium oxide with pure water according to the liquid-solid ratio of 5:1 to obtain niobium oxide slurry, and sending the niobium oxide slurry into an ultrasonic dispersion machine for ultrasonic dispersion for 20 minutes.
8. And (4) timely feeding the dispersed niobium oxide slurry into a quick drying furnace for quick drying for 30 minutes.
9. And (3) feeding the dried niobium oxide into an airflow classifier, and performing airflow classification to obtain a nano niobium oxide product.
10. And after sampling and analyzing to be qualified, weighing, packaging and warehousing.
Example two:
1. the analysis shows that the concentration of the niobium liquid is 80g/L, and the acidity is 4.5N. According to the technological requirements, the total content of niobium oxide in a barrel (tank) of oxide is controlled to be 18Kg, and pure water is added to make the acidity of niobium liquid to be 4.0N by calculation.
2. And after the niobium liquid is fully stirred and blended for 5 minutes, slowly adding the niobium liquid into the niobium-based ceramic chromatographic filter sleeved with the niobium-based ceramic tray.
3. And (3) conveying the niobium-based ceramic chromatographic filter which is filled with the niobium liquid and is sleeved with the niobium-based ceramic tray into a drying chamber for carrying out low-temperature time control chromatographic drying for 24 hours until the niobium liquid is chromatographed, and separating the niobium oxide hydrate from the outer wall of the niobium-based ceramic chromatographic filter.
4. After the chromatography and the drying are finished, cleaning the outer wall of the niobium-based ceramic chromatography filter by using a clean brush, collecting niobium materials falling into a niobium-based ceramic tray, combining the niobium materials, putting the niobium materials into a niobium crucible, sending the niobium crucible into an oven, controlling the temperature of the oven at 180-200 ℃, drying the niobium crucible until the niobium materials are slightly twisted into powder by hands,
after cooling, the mixture is crushed and sieved by a 60-mesh sieve.
5. The sieved niobium oxide is filled into a niobium crucible and sent to a calcining furnace to be calcined at 200 ℃ for 2 hours, 400 ℃ for 2 hours, 600 ℃ for 4 hours and 800 ℃ for 4 hours in different time intervals.
6. Cooling the calcined niobium oxide, and sieving the cooled niobium oxide by a 120-mesh grading sieve.
7. And crushing and refining the graded niobium oxide again, mixing the niobium oxide slurry with pure water according to the liquid-solid ratio of 5:1, and sending the niobium oxide slurry into an ultrasonic dispersion machine for ultrasonic dispersion for 15 minutes.
8. And (4) timely feeding the dispersed niobium oxide slurry into a quick drying furnace for quick drying for 25 minutes.
9. And (3) feeding the dried niobium oxide into an airflow classifier, and performing airflow classification to obtain a nano niobium oxide product.
10. And after sampling and analyzing to be qualified, weighing, packaging and warehousing.
Example three:
1. the analysis shows that the concentration of the niobium liquid is 90g/L, and the acidity is 5N. According to the technological requirements, the total content of niobium oxide in a barrel (tank) of oxide is controlled to be 20Kg, and pure water is added by calculation until the acidity of niobium liquid is 4.5N.
2. And after the niobium liquid is fully stirred and blended for 5 minutes, slowly adding the niobium liquid into the niobium-based ceramic chromatographic filter sleeved with the niobium-based ceramic tray.
3. And (3) conveying the niobium-based ceramic chromatographic filter which is filled with the niobium liquid and is sleeved with the niobium-based ceramic tray into a drying chamber for carrying out low-temperature time control chromatographic drying for 24 hours until the niobium liquid is chromatographed, and separating the niobium oxide hydrate from the outer wall of the niobium-based ceramic chromatographic filter.
4. After the chromatography and the drying are finished, cleaning the outer wall of the niobium-based ceramic chromatography filter by using a clean brush, collecting niobium materials falling into a niobium-based ceramic tray, combining the niobium materials, putting the niobium materials into a niobium crucible, sending the niobium crucible into an oven, controlling the temperature of the oven at 180-200 ℃, drying the niobium crucible until the niobium materials are slightly twisted into powder by hands,
after cooling, the mixture is crushed and sieved by a 60-mesh sieve.
5. The sieved niobium oxide is filled into a niobium crucible and sent to a calcining furnace to be calcined at 200 ℃ for 2 hours, 400 ℃ for 2 hours, 600 ℃ for 4 hours and 800 ℃ for 4 hours in different intervals.
6. Cooling the calcined niobium oxide, and sieving the cooled niobium oxide by a 120-mesh grading sieve.
7. And crushing and refining the graded niobium oxide, mixing the niobium oxide slurry with pure water according to the liquid-solid ratio of 5:1 to obtain niobium oxide slurry, and sending the niobium oxide slurry into an ultrasonic dispersion machine to carry out ultrasonic dispersion for 20 minutes.
8. And (4) timely feeding the dispersed niobium oxide slurry into a quick drying furnace for quick drying for 30 minutes.
9. And (3) feeding the dried niobium oxide into an airflow classifier, and performing airflow classification to obtain a nano niobium oxide product.
10. And after sampling and analyzing to be qualified, weighing, packaging and warehousing.
Claims (8)
1. A method for preparing nano niobium oxide by a niobium ceramic chromatography process is characterized by comprising the following steps: blending in step S1, preparing chromatography in step S2, drying in step S3, sieving in step S4, calcining in step S5, sieving in step S6, crushing in step S7, size mixing in step S8, dispersing in step S9, quick drying in step S10, airflow classification in step S11 and packaging in step 12;
step S1, putting the niobium liquid into a blending tank, determining pure water to be added before blending according to different acidity and concentration of the niobium liquid, and controlling the concentration of the niobium liquid to be 80-100 g/L and the acidity to be 3.3-5.0N;
step S2, after fully stirring and blending the niobium liquid, slowly adding the niobium liquid into a niobium-based ceramic filter for chromatography preparation;
step S3, the niobium-based ceramic chromatographic filter which is sleeved with the niobium-based ceramic tray and is filled with niobium liquid is sent into a drying chamber together for low-temperature time-controlled chromatography and drying;
step S4, collecting niobium materials falling into the niobium-based ceramic tray after chromatography and drying, putting the niobium materials into a niobium crucible, sending the niobium crucible into an oven, controlling the temperature of the oven at 180-200 ℃, drying the niobium materials until the niobium materials are slightly twisted into powder by hands, crushing the powder and sieving the powder with a 60-mesh sieve;
step S5, putting the sieved niobium oxide into a niobium crucible, and calcining the niobium oxide in a calciner at the temperature of 200 ℃ for 2 hours, 400 ℃ for 2 hours, 600 ℃ for 4 hours and 800 ℃ for 4 hours in different time intervals;
step S6, cooling the calcined niobium oxide and screening the cooled calcined niobium oxide through a 120-mesh classifying screen;
step S7, crushing the graded niobium oxide, thinning and crushing;
step S8, preparing the refined and crushed niobium oxide into slurry by pure water according to a certain proportion;
step S9, preparing niobium oxide into slurry for ultrasonic dispersion;
step S10, timely feeding the dispersed niobium oxide slurry into a quick drying furnace for quick drying;
step S11, classifying the dried niobium oxide airflow to obtain a nano niobium oxide product;
step S12: and after sampling and analyzing to be qualified, weighing, packaging and warehousing.
2. The method for preparing nano niobium oxide through niobium ceramic chromatography process as claimed in claim 1, wherein the niobium solution concentration in step S1 is 100g/L, and the acidity is 5.5N.
3. The method for preparing nano niobium oxide through niobium ceramic chromatography process as claimed in claim 1, wherein the niobium solution concentration in step S1 is 80g/L, and the acidity is 4.5N.
4. The method for preparing nano niobium oxide through niobium ceramic chromatography process as claimed in claim 1, wherein the niobium solution concentration in step S1 is 90g/L, and the acidity is 5N.
5. The method for preparing nano niobium oxide through niobium ceramic chromatography process as claimed in claim 1, wherein after the step S4 of chromatography and drying, the outer wall of the niobium-based ceramic chromatography filter is cleaned by a clean brush.
6. The method for preparing nano niobium oxide through niobium ceramic chromatography process as claimed in claim 1, wherein the pure water in step S8 is mixed into niobium oxide slurry according to the ratio of liquid to solid of 5: 1.
7. The method for preparing nano niobium oxide through niobium ceramic chromatography process as claimed in claim 1, wherein in step S9, the material is sent to an ultrasonic disperser to be subjected to ultrasonic dispersion for 20 minutes.
8. The method for preparing nano niobium oxide through niobium ceramic chromatography process as claimed in claim 1, wherein step S10 is to feed the dispersed niobium oxide slurry into a rapid drying oven for rapid drying for 30 minutes in time.
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Citations (4)
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CN102897836A (en) * | 2012-10-23 | 2013-01-30 | 九江有色金属冶炼有限公司 | Preparation method of ultrafine niobium oxide |
CN103864146A (en) * | 2012-12-12 | 2014-06-18 | 毛华军 | Preparation method for niobium oxide nanotube |
CN104495929A (en) * | 2014-12-26 | 2015-04-08 | 宁夏东方钽业股份有限公司 | Low-valent niobium oxide powder and preparation method thereof |
CN106865614A (en) * | 2017-03-24 | 2017-06-20 | 广东广晟稀有金属光电新材料有限公司 | A kind of specific surface area is 7m2/ g~8m2The preparation method of the niobium oxide of/g |
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CA2615772A1 (en) * | 2005-07-28 | 2007-02-08 | Indiana University Research & Technology Corporation | Niobium oxide compositions, nanostructures, bioactive forms and uses thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN102897836A (en) * | 2012-10-23 | 2013-01-30 | 九江有色金属冶炼有限公司 | Preparation method of ultrafine niobium oxide |
CN103864146A (en) * | 2012-12-12 | 2014-06-18 | 毛华军 | Preparation method for niobium oxide nanotube |
CN104495929A (en) * | 2014-12-26 | 2015-04-08 | 宁夏东方钽业股份有限公司 | Low-valent niobium oxide powder and preparation method thereof |
CN106865614A (en) * | 2017-03-24 | 2017-06-20 | 广东广晟稀有金属光电新材料有限公司 | A kind of specific surface area is 7m2/ g~8m2The preparation method of the niobium oxide of/g |
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