CN107857240A - The production method of niobium nitride powder - Google Patents
The production method of niobium nitride powder Download PDFInfo
- Publication number
- CN107857240A CN107857240A CN201711242474.7A CN201711242474A CN107857240A CN 107857240 A CN107857240 A CN 107857240A CN 201711242474 A CN201711242474 A CN 201711242474A CN 107857240 A CN107857240 A CN 107857240A
- Authority
- CN
- China
- Prior art keywords
- niobium
- niobium nitride
- production method
- nitride powder
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
- C01B21/0617—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with vanadium, niobium or tantalum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of production method of niobium nitride powder, comprise the following steps, 1) after metal niobium powder is well mixed with magnesium powder, it is put into vacuum reaction container, after vacuumizing, carries out first paragraph heating, after being warming up to design temperature, argon gas is filled with, and be incubated, then argon gas is extracted, is filled with high pure nitrogen, carries out second segment heating, after being warming up to reaction temperature, reacted, after the completion of reaction, room temperature is cooled to, obtains reaction product；2) reaction product obtained in step 1) is crushed, after sieving, carries out pickling, after the completion of pickling, it is neutral to be rinsed with water to solution, after then being dried, produces niobium nitride powder.The present invention reduces the oxygen in niobium powder by using magnesium powder, intensifies niobium powder surface-active, niobium powder is fully reacted with nitrogen, the niobium nitride of preparation, and nitrogen content has reached more than 12%, and impurity content is less than 0.05%；The equipment that the present invention uses is simple, easy to operate, it is easy to accomplish industrialized production.
Description
Technical field
The invention belongs to superconductor preparing technical field, and in particular to the production method of niobium nitride powder.
Background technology
Niobium nitride is a kind of good superconductor, and compared with pure niobium, niobium nitride has higher superconducting transition temperature
(16.1K) and narrower width of transition (0.1K)；Also there is good stability at low temperatures and high temperatures, niobium nitride is under superconducting state
Also good magnetic stability, in 4.2K, critical magnetic field is 25T, far above the critical magnetic field strength of niobium in itself, it can thus be appreciated that
Niobium nitride can be as the candidate materials of radio frequency superconducting cavity.
At present, the preparation method of niobium nitride powder mainly has direct method and reducing process, and direct method is by the metal niobium of crushing
It is sent into nitriding furnace, is passed through nitrogen or ammonia, is directly warming up to 700-1000 DEG C and is reacted, niobium nitride is prepared；Reduction
Method is to add powdered carbon in the niobium oxide powder of crushing, it is sent into after being sufficiently mixed in reduction furnace, then passes to hydrogen and nitrogen,
It is warming up to 1200-1300 DEG C to react, obtains niobium nitride.But because metal niobium powder and niobium oxide powder surface-active are relatively low,
It is incomplete with nitrogen or ammonia reaction, thus the nitrogen content of the niobium nitride prepared is relatively low, impurity content is higher, influences its performance；
In patent CN 1396111A " a kind of method for preparing nano cubic niobium nitride powder ", by using niobium pentaoxide as original
Material, niobium nitride is arrived by prepared by reducing process, 95% or so, impurity content is higher for the purity of its niobium nitride.
The content of the invention
It is an object of the invention to provide a kind of production method for the niobium nitride powder for effectively improving niobium nitride purity.
The production method of this niobium nitride powder of the present invention, comprises the following steps：
1) after metal niobium powder is well mixed with magnesium powder, it is put into vacuum reaction container, after vacuumizing, carries out first paragraph liter
Temperature, after being warming up to design temperature, argon gas is filled with, and is incubated, then extract argon gas, be filled with high pure nitrogen, carry out second segment
Heating, after being warming up to reaction temperature, is reacted, after the completion of reaction, is cooled to room temperature, obtains reaction product；
2) reaction product obtained in step 1) is crushed, after sieving, carries out pickling, after the completion of pickling, rushed with water
Solution is washed till as neutrality, after then being dried, produces niobium nitride powder.
In the step 1, niobium powder is 100 with niobium powder weight ratio:(2-10)；It is evacuated to pressure≤0.1Pa；First paragraph liter
Temperature is 700~750 DEG C；Soaking time is 3~5h；It is 0.02~0.16MPa that nitrogen pressure should be kept by, which being filled with after nitrogen,
Two sections of warming temperatures are 800~1200 DEG C；Reaction time is 3~12h.
In the step 2), acid is one kind in hydrochloric acid, sulfuric acid, nitric acid used by acid cleaning process, and its molar concentration is 3
~5mol/L；The mass volume ratio of reaction product and acid is 45:(10~15) kg/L.
Nitrogen content >=12.0% of the niobium nitride, purity >=99.95% of niobium nitride.
Beneficial effects of the present invention：
The present invention reduces the oxygen in niobium powder, intensifies niobium powder surface reaction activity, make niobium powder and nitrogen by using magnesium powder
Can fully it react, the niobium nitride being prepared, nitrogen content has reached more than 12%, and impurity content is less than 0.05%；Secondly, originally
Invention employs the form of multistage heating, and first paragraph heats up primarily to enabling magnesium powder to activate niobium powder surface, second segment liter
Temperature is that multistage heating mode can avoid the generation of impurity in order that niobium powder fully reacts with nitrogen, so as to reach raising niobium nitride
The purpose of purity；Again, the equipment that the present invention uses is simple, easy to operate, it is easy to accomplish industrialized production.
Brief description of the drawings
The X-ray diffracting spectrum for the niobium nitride that Fig. 1 embodiments 1 are produced；
The electron scanning collection of illustrative plates for the niobium nitride that Fig. 2 embodiments 1 are produced.
Embodiment
Embodiment 1
5% magnesium powder of 40kg niobiums powder and niobium powder weight is sufficiently mixed uniformly, is incorporated with the close of inert gas import and export
In the reaction vessel of the inside lining heat-resisting alloy material closed, after being evacuated to pressure≤0.1Pa, 750 DEG C are warming up to, is filled with argon
Gas, constant temperature 3 hours, then extracts argon gas, and being re-filled with the high pure nitrogen of purity >=99.999%, (nitrogen gas purity following examples are all
It is identical), it is warming up to 1200 DEG C of constant temperature 3 hours, and keep nitrogen pressure to be then cooled to room temperature in 0.02Mpa.By reaction product
Broken, sieving, takes reaction product, and the hydrochloric acid 10L for being 3mol/L with concentration carries out pickling, then after being washed to solution pH value as neutrality
Drying, obtains niobium nitride powder, the dust sampling of preparation is analyzed, its chemical composition and percentage by weight are shown in Table 1.Prepared
The XRD of niobium nitride according to the XRD standard cards of niobium nitride as shown in figure 1, contrast, the characteristic peak occurred in figure is niobium nitride
Characteristic peak, there is not the spectral line of raw material niobium, oxygen or other nitride, illustrate that the niobium nitride purity of acquisition is higher；Prepared
The microscopic appearance figure of niobium nitride, as shown in Fig. 2 the Granularity Distribution is uniform, without foreign matter, show product purity height.
Embodiment 2
2% magnesium powder of 40kg niobiums powder and niobium powder weight is sufficiently mixed uniformly, is incorporated with the close of inert gas import and export
In the reaction vessels of the inside lining heat-resisting alloy material closed, 700 DEG C are warming up to after being evacuated to pressure≤0.1Pa, is filled with argon gas,
Constant temperature 4 hours, then extracts argon gas, is re-filled with high pure nitrogen, is warming up to 1000 DEG C of constant temperature 5 hours, and keeps nitrogen pressure to exist
0.08Mpa, then it is cooled to room temperature.Reaction product is crushed, sieving, take reaction product, the sulphur for being 4mol/L with equivalent concentration
Sour 12L carries out pickling, then is washed to solution pH value to be dried after neutrality, obtains niobium nitride powder.To the dust sampling point of preparation
Analysis, its chemical composition are shown in Table 1.
Embodiment 3
10% magnesium powder of 40kg niobiums powder and niobium powder weight is sufficiently mixed uniformly, is incorporated with inert gas import and export
In the reaction vessel of closed inside lining heat-resisting alloy material, 730 DEG C are warming up to after being evacuated to pressure≤0.1Pa, is filled with argon
Gas, constant temperature 5 hours, then extracts argon gas, is re-filled with high pure nitrogen, is warming up to 800 DEG C of constant temperature 12 hours, and keeps nitrogen pressure
In 0.16Mpa, room temperature is then cooled to.Reaction product is crushed, sieving, take reaction product, the nitric acid for being 5mol/L with concentration
15L carries out pickling, then is washed to solution pH value to be dried after neutrality, obtains niobium nitride powder.The dust sampling of preparation is analyzed,
Its chemical composition is shown in Table 1.
The chemical composition (%) of the niobium powder of table 1 and niobium nitride product
The total nitrogen content for the niobium nitride powder produced according to the inventive method is can be seen that from the result of above example
Height, equipment is simple, easy to operate, it is easy to accomplish industrialized production.
Claims (10)
1. a kind of production method of niobium nitride powder, comprises the following steps：
1) after metal niobium powder is well mixed with magnesium powder, it is put into vacuum reaction container, after vacuumizing, carries out first paragraph heating,
After being warming up to design temperature, argon gas is filled with, and is incubated, then extracts argon gas, is filled with high pure nitrogen, carries out second segment liter
Temperature, after being warming up to reaction temperature, reacted, after the completion of reaction, be cooled to room temperature, obtain reaction product；
2) reaction product obtained in step 1) is crushed, after sieving, carry out pickling, after the completion of pickling, with water rinse to
Solution is neutrality, after then being dried, produces niobium nitride powder.
2. the production method of niobium nitride powder according to claim 1, it is characterised in that in the step 1, niobium powder and magnesium
The mass ratio of powder is 100:(2-10).
3. the production method of niobium nitride powder according to claim 1 or 2, it is characterised in that in the step 1), take out true
It is empty to pressure≤0.1Pa.
4. the production method of niobium nitride powder according to claim 1 or 2, it is characterised in that in the step 1), first
Section warming temperature is 700 DEG C -750 DEG C；Soaking time is 3~5h.
5. the production method of niobium nitride powder according to claim 1 or 2, it is characterised in that in the step 1), be filled with
It is 0.02~0.16MPa that nitrogen pressure should be kept after nitrogen.
6. the production method of niobium nitride powder according to claim 1 or 2, it is characterised in that in the step 1), second
Section warming temperature is 800~1200 DEG C.
7. the production method of niobium nitride powder according to claim 1 or 2, it is characterised in that in the step 1), reaction
Time is 3~12h.
8. the production method of niobium nitride powder according to claim 1, it is characterised in that in the step 2), pickling work
Acid is one kind in hydrochloric acid, sulfuric acid, nitric acid used by skill, and its molar concentration is 3~5mol/L.
9. the production method of the niobium nitride powder according to claim 1 or 8, it is characterised in that in the step 2), reaction
The mass volume ratio of product and acid is 45:(10-15)kg/L.
10. the production method of niobium nitride powder according to claim 1, it is characterised in that the nitridation being prepared
Nitrogen content >=12.0% of niobium, purity >=99.95% of niobium nitride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711242474.7A CN107857240B (en) | 2017-11-30 | 2017-11-30 | Method for producing niobium nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711242474.7A CN107857240B (en) | 2017-11-30 | 2017-11-30 | Method for producing niobium nitride powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107857240A true CN107857240A (en) | 2018-03-30 |
| CN107857240B CN107857240B (en) | 2021-03-30 |
Family
ID=61704363
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711242474.7A Active CN107857240B (en) | 2017-11-30 | 2017-11-30 | Method for producing niobium nitride powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107857240B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60169176A (en) * | 1984-02-13 | 1985-09-02 | Rikagaku Kenkyusho | Formation of nbn thin film |
| US5284639A (en) * | 1991-06-27 | 1994-02-08 | Teledyne Industries, Inc. | Method for the preparation of niobium nitride |
| CN1224529A (en) * | 1997-02-28 | 1999-07-28 | 昭和电工株式会社 | Capacitor |
| CN1426334A (en) * | 2000-03-01 | 2003-06-25 | 卡伯特公司 | Nitrided valve metals and processes for making same |
| CN1699147A (en) * | 2005-05-24 | 2005-11-23 | 株洲硬质合金集团有限公司 | Ultra-fine high-nitrogen tantalum nitride powder and its preparation method |
| CN105449094A (en) * | 2015-12-29 | 2016-03-30 | 中国科学院上海微系统与信息技术研究所 | Preparation method of NbN thin film, SQUID device and preparation method of SQUID device |
-
2017
- 2017-11-30 CN CN201711242474.7A patent/CN107857240B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60169176A (en) * | 1984-02-13 | 1985-09-02 | Rikagaku Kenkyusho | Formation of nbn thin film |
| US5284639A (en) * | 1991-06-27 | 1994-02-08 | Teledyne Industries, Inc. | Method for the preparation of niobium nitride |
| CN1224529A (en) * | 1997-02-28 | 1999-07-28 | 昭和电工株式会社 | Capacitor |
| CN1426334A (en) * | 2000-03-01 | 2003-06-25 | 卡伯特公司 | Nitrided valve metals and processes for making same |
| CN1699147A (en) * | 2005-05-24 | 2005-11-23 | 株洲硬质合金集团有限公司 | Ultra-fine high-nitrogen tantalum nitride powder and its preparation method |
| CN105449094A (en) * | 2015-12-29 | 2016-03-30 | 中国科学院上海微系统与信息技术研究所 | Preparation method of NbN thin film, SQUID device and preparation method of SQUID device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107857240B (en) | 2021-03-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108328635B (en) | Method for preparing alumina aerogel | |
| CN103130506B (en) | Method for preparing superfine titanium carbonitride | |
| CN101642812A (en) | Molybdenum-yttrium alloy wire preparation method | |
| CN104894641B (en) | It is a kind of high fine and close（LaxCa1‑x）B6Polycrystalline cathode material and preparation method thereof | |
| CN110204341B (en) | (Hf, Ta, Nb, Ti) B2High-entropy ceramic powder and preparation method thereof | |
| CN103014345B (en) | The production method of VN alloy | |
| CN110422883A (en) | A method of FeAs powder is prepared using mechanical alloying | |
| CN103011098B (en) | Production method for increasing content of nitrogen in vanadium-nitrogen alloy | |
| CN104726758A (en) | Method for preparing vanadium-nitrogen alloy by matching of ammonium metavanadate and vanadium pentoxide | |
| CN104451758A (en) | Method for preparing titanium carbide by performing molten salt electrolysis on high titanium slags | |
| CN107857240A (en) | The production method of niobium nitride powder | |
| CN114334423A (en) | Iron-based nitride soft magnetic material and preparation method thereof | |
| CN106829978B (en) | A method of preparing fayalite | |
| CN104532034A (en) | Preparation method for low-oxygen vanadium-nitrogen alloy | |
| CN114822976B (en) | Preparation method of iron-arsenic compound and iron-based superconductor | |
| CN102938270A (en) | Method for preparing and conducting cold high pressure densifying on Cu wrapped Ba0.6K0.4Fe2As2 superconducting wire | |
| CN110817813B (en) | Preparation method of nanocrystalline vanadium nitride powder | |
| CN106866152B (en) | A kind of YB4The preparation method of block | |
| CN106336220B (en) | High-density MgB2Method for producing superconductor | |
| CN106348288B (en) | A kind of purification process technique of compound probability diamond graphite stem | |
| CN100415640C (en) | Ultra-fine high-nitrogen tantalum nitride powder and its preparation method | |
| GB2617006A (en) | Expanded graphite and preparation method therefor | |
| CN106782897A (en) | A kind of method that high-temperature sintering process prepares yttrium niobium copper superconductor | |
| CN102259882B (en) | Preparation method of high-purity YB4 powder body | |
| CN113564344A (en) | Method for reducing pyrolusite by gas |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |