CN107857240B - Method for producing niobium nitride powder - Google Patents
Method for producing niobium nitride powder Download PDFInfo
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- CN107857240B CN107857240B CN201711242474.7A CN201711242474A CN107857240B CN 107857240 B CN107857240 B CN 107857240B CN 201711242474 A CN201711242474 A CN 201711242474A CN 107857240 B CN107857240 B CN 107857240B
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- 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
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- C—CHEMISTRY; METALLURGY
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- 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
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for producing niobium nitride powder, which comprises the following steps of 1) uniformly mixing metal niobium powder and magnesium powder, putting the mixture into a vacuum reaction container, vacuumizing, carrying out first-stage heating, heating to a set temperature, then filling argon, carrying out heat preservation, then removing argon, filling high-purity nitrogen, carrying out second-stage heating, heating to a reaction temperature, carrying out reaction, and cooling to room temperature after the reaction is finished to obtain a reaction product; 2) crushing the reaction product obtained in the step 1), sieving, carrying out acid washing, washing with water until the solution is neutral after the acid washing is finished, and drying to obtain the niobium nitride powder. The invention reduces oxygen in the niobium powder by adopting magnesium powder, activates the surface activity of the niobium powder, and ensures that the niobium powder and nitrogen can fully react, and the nitrogen content of the prepared niobium nitride reaches more than 12 percent, and the impurity content is lower than 0.05 percent; the invention has the advantages of simple equipment, convenient operation and easy realization of industrial production.
Description
Technical Field
The invention belongs to the technical field of superconducting material preparation, and particularly relates to a production method of niobium nitride powder.
Background
Niobium nitride is a good superconducting material, and has a higher superconducting transition temperature (16.1K) and a narrower transition width (0.1K) compared with pure niobium; the niobium nitride has good stability at low temperature and high temperature, has good magnetic stability in a superconducting state, has a critical magnetic field of 25T at 4.2K, and is far higher than the critical magnetic field strength of niobium, so that the niobium nitride can be used as an alternative material of a radio frequency superconducting cavity.
At present, the preparation method of niobium nitride powder mainly comprises a direct method and a reduction method, wherein the direct method comprises the steps of sending crushed niobium metal into a nitriding furnace, introducing nitrogen or ammonia, directly heating to 700-; the reduction method is that carbon powder is added into the crushed niobium oxide powder, the mixture is sent into a reduction furnace after being fully mixed, then hydrogen and nitrogen are introduced, and the temperature is raised to 1200-1300 ℃ for reaction, so as to obtain the niobium nitride. However, because the metal niobium powder and the niobium oxide powder have low surface activity and do not completely react with nitrogen or ammonia gas, the prepared niobium nitride has low nitrogen content and high impurity content, and the performance of the niobium nitride is influenced; for example, in patent CN 1396111a, "a method for preparing cubic phase nano niobium nitride powder", niobium nitride is prepared by using niobium pentoxide as a raw material and by a reduction method, and the purity of the niobium nitride is about 95%, and the impurity content is relatively high.
Disclosure of Invention
The invention aims to provide a method for producing niobium nitride powder, which can effectively improve the purity of niobium nitride.
The production method of the niobium nitride powder comprises the following steps:
1) uniformly mixing metal niobium powder and magnesium powder, putting the mixture into a vacuum reaction container, vacuumizing, carrying out first-stage heating, heating to a set temperature, filling argon, carrying out heat preservation, then removing argon, filling high-purity nitrogen, carrying out second-stage heating, heating to a reaction temperature, carrying out reaction, and cooling to room temperature after the reaction is finished to obtain a reaction product;
2) crushing the reaction product obtained in the step 1), sieving, carrying out acid washing, washing with water until the solution is neutral after the acid washing is finished, and drying to obtain the niobium nitride powder.
In the step 1, the weight ratio of the niobium powder to the niobium powder is 100 (2-10); vacuumizing until the pressure is less than or equal to 0.1 Pa; the temperature rise temperature of the first stage is 700-750 ℃; the heat preservation time is 3-5 h; after nitrogen is filled, the nitrogen pressure is kept to be 0.02-0.16 MPa, and the temperature rise of the second section is 800-1200 ℃; the reaction time is 3-12 h.
In the step 2), the acid adopted in the acid washing process is one of hydrochloric acid, sulfuric acid and nitric acid, and the molar concentration of the acid is 3-5 mol/L; the mass volume ratio of the reaction product to the acid is 45 (10-15) kg/L.
The nitrogen content of the niobium nitride is more than or equal to 12.0 percent, and the purity of the niobium nitride is more than or equal to 99.95 percent.
The invention has the beneficial effects that:
the invention reduces oxygen in the niobium powder by adopting magnesium powder, activates the surface reaction activity of the niobium powder, and ensures that the niobium powder and nitrogen can fully react to prepare the niobium nitride, wherein the nitrogen content reaches more than 12 percent, and the impurity content is lower than 0.05 percent; secondly, the invention adopts a multi-stage heating mode, wherein the first stage heating is mainly used for enabling magnesium powder to activate the surface of niobium powder, the second stage heating is used for enabling the niobium powder to fully react with nitrogen, and the multi-stage heating mode can avoid the generation of impurities, thereby achieving the purpose of improving the purity of niobium nitride; thirdly, the equipment adopted by the invention is simple, the operation is convenient, and the industrial production is easy to realize.
Drawings
FIG. 1 is an X-ray diffraction pattern of niobium nitride produced in example 1;
FIG. 2 is an electron scanning spectrum of niobium nitride produced in example 1.
Detailed Description
Example 1
40kg of niobium powder and magnesium powder which accounts for 5 percent of the weight of the niobium powder are fully and uniformly mixed, the mixture is put into a closed reaction vessel which is internally lined with heat-resistant alloy materials and provided with an inert gas inlet and an inert gas outlet, the reaction vessel is vacuumized until the pressure is less than or equal to 0.1Pa, the reaction vessel is heated to 750 ℃, argon gas is filled, the temperature is kept constant for 3 hours, then the argon gas is pumped out, high-purity nitrogen gas with the purity of more than or equal to 99.999 percent is filled (the nitrogen gas purity is the same in the following examples), the reaction vessel is heated to 1200 ℃, the temperature is kept constant for 3 hours, the nitrogen. Crushing and sieving a reaction product, taking the reaction product, carrying out acid washing by using 10L hydrochloric acid with the concentration of 3mol/L, then washing by using water until the pH value of the solution is neutral, and drying to obtain niobium nitride powder, wherein the chemical components and the weight percentage of the prepared powder are shown in Table 1. The XRD of the prepared niobium nitride is shown in figure 1, and according to the comparison with the XRD standard card of the niobium nitride, the characteristic peaks shown in the figure are all the characteristic peaks of the niobium nitride, and no spectral line of the niobium, oxygen or other nitrides appears, which indicates that the purity of the obtained niobium nitride is higher; the micro-topography of the prepared niobium nitride is shown in figure 2, the product has uniform particle size distribution and no foreign matters, which shows that the product has high purity.
Example 2
The method comprises the steps of fully and uniformly mixing 40kg of niobium powder and magnesium powder accounting for 2% of the weight of the niobium powder, filling the mixture into a closed reaction vessel with an inert gas inlet and an inert gas outlet and a heat-resistant alloy material lining inside, vacuumizing until the pressure is less than or equal to 0.1Pa, heating to 700 ℃, filling argon, keeping the temperature constant for 4 hours, then removing the argon, filling high-purity nitrogen, heating to 1000 ℃, keeping the temperature constant for 5 hours, keeping the nitrogen pressure at 0.08MPa, and cooling to room temperature. And crushing and sieving the reaction product, taking the reaction product, carrying out acid washing by using 12L sulfuric acid with the equivalent concentration of 4mol/L, washing by using water until the pH value of the solution is neutral, and drying to obtain niobium nitride powder. The prepared powder was sampled and analyzed, and its chemical composition is shown in table 1.
Example 3
The method comprises the steps of fully and uniformly mixing 40kg of niobium powder and magnesium powder accounting for 10% of the weight of the niobium powder, filling the mixture into a closed reaction vessel with an inert gas inlet and an inert gas outlet and a heat-resistant alloy material lining inside, vacuumizing until the pressure is less than or equal to 0.1Pa, heating to 730 ℃, filling argon, keeping the temperature constant for 5 hours, then removing the argon, filling high-purity nitrogen, heating to 800 ℃, keeping the temperature constant for 12 hours, keeping the nitrogen pressure at 0.16MPa, and cooling to room temperature. And crushing and sieving the reaction product, taking the reaction product, carrying out acid washing by using 15L nitric acid with the concentration of 5mol/L, washing by using water until the pH value of the solution is neutral, and drying to obtain niobium nitride powder. The prepared powder was sampled and analyzed, and its chemical composition is shown in table 1.
TABLE 1 chemical composition of niobium powder and niobium nitride product (%)
From the results of the above examples, it can be seen that the niobium nitride powder prepared according to the method of the present invention has a high total nitrogen content, simple equipment, convenient operation, and easy realization of industrial production.
Claims (6)
1. A method for producing niobium nitride powder, comprising the steps of:
1) uniformly mixing metal niobium powder and magnesium powder, putting the mixture into a vacuum reaction container, vacuumizing, carrying out first-stage heating, heating to a set temperature, filling argon, carrying out heat preservation, then removing argon, filling high-purity nitrogen, carrying out second-stage heating, heating to a reaction temperature, carrying out reaction, and cooling to room temperature after the reaction is finished to obtain a reaction product;
2) crushing the reaction product obtained in the step 1), sieving, carrying out acid washing, washing with water until the solution is neutral after the acid washing is finished, and drying to obtain niobium nitride powder;
in the step 1), the temperature rise temperature of the first section is 700-750 ℃; the heat preservation time is 3-5 h; keeping the nitrogen pressure at 0.02-0.16 MPa after filling nitrogen; the temperature rise temperature of the second section is 800-1200 ℃; the reaction time is 3-12 h.
2. The method for producing the niobium nitride powder as claimed in claim 1, wherein the mass ratio of the niobium powder to the magnesium powder in step 1 is 100 (2-10).
3. The method for producing the niobium nitride powder as claimed in claim 1 or 2, wherein in the step 1), a vacuum is applied to a pressure of 0.1Pa or less.
4. The method for producing niobium nitride powder according to claim 1, wherein in the step 2), the acid used in the acid washing process is one of hydrochloric acid, sulfuric acid and nitric acid, and the molar concentration is 3 to 5 mol/L.
5. The method for producing the niobium nitride powder as claimed in claim 1, wherein the mass-to-volume ratio of the reaction product to the acid in the step 2) is 45 (10 to 15) kg/L.
6. The method for producing niobium nitride powder according to claim 1, wherein the produced niobium nitride has a nitrogen content of not less than 12.0% and a purity of not less than 99.95%.
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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***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***与信息技术研究所 | Preparation method of NbN thin film, SQUID device and preparation method of SQUID device |
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