CN108063249B - Preparation method of high-purity copper nitride nanocrystal - Google Patents
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- CN108063249B CN108063249B CN201711275090.5A CN201711275090A CN108063249B CN 108063249 B CN108063249 B CN 108063249B CN 201711275090 A CN201711275090 A CN 201711275090A CN 108063249 B CN108063249 B CN 108063249B
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Abstract
The invention discloses a preparation method of a high-purity copper nitride nanocrystal, which is characterized by comprising the following steps: in an oxygen-free, water-free and inert gas environment, nano Cu is added2And uniformly mixing the O and the urea according to the molar ratio of 1:1.5-4, pouring the mixture into a sealed container for sealing, transferring the sealed container into a heating device filled with inert gas, heating to the temperature of 150-. The invention adopts nano Cu2O and urea are directly subjected to solid-state reaction, a solvent is not required to be provided for a reaction site, a product is not required to be separated from the solvent, and other subsequent treatments are not required, so that the solid copper nitride nanocrystal with the purity of more than 98.5 percent is directly obtained, and the purity is greatly improved.
Description
Technical Field
The invention relates to the technical field of new energy, in particular to a preparation method of a high-purity copper nitride nanocrystal.
Background
Copper nitride (Cu)3N) is a semiconductor, considered to be a promising material, widely used in solar conversion catalytic applications, Huisgen cycloaddition and electrochemical oxygen reduction reactions, resistive random access memory chips and optical storage devices, etc. Meanwhile, due to the huge demand for electrochemical power sources with higher energy density, new electrode materials for improving performance are sought, and the research of Lithium Ion Batteries (LIBs) is rapidly ongoing. The nano-structured metal oxide has good electrochemical performance and is considered to be a promising high-performance material of an anode material. In addition to metal oxides, the advent of metal nitrides has also raised widespread interest in the area of anodes for high performance lithium ion and sodium ion batteries.
Binary metal nitrides, e.g. VN, CrN, Zn3N2，Fe3N，Co3N, and Cu3N reacts electrochemically with Li to form Li3A matrix of N metal nanoparticles. In 2003, Tarascon and colleagues reported that it still had 300mAh/g at 224mA/g currentThe capacity of (c). Meanwhile, for submicron copper nitride particles, no further report on lithium storage is currently available. Although copper nitride has attracted a wide range of attention in the electrochemical field, the synthetic methods for preparing copper nitride nanoparticles remain limited.
In the past, copper nitride synthesis methods have included: ammonolysis of molecular precursors, reaction of copper or copper oxide at high temperature, and decomposition of copper nitride precursors. However, these methods require the use of very high reaction temperatures (generally greater than 240 ℃), and although researchers have made considerable efforts in the synthesis of solution routes that do not require high temperatures and pressures, there are also methoxy copper and benzylamine reduction methods that produce copper nitride at low temperatures, but with insufficient purity, as can be seen in fig. 1, the resulting product has a very limited purity, approximately 80-90%, compared to the characteristic peaks in the standard copper nitride pattern. The Chinese patent with publication No. CN102211763 discloses a preparation method of copper nitride nanocrystals, primary amine reduction and octadecene are required to be used as solvents, primary amine and copper nitrate are solid at normal temperature, the solubility of the primary amine and the copper nitrate in an organic solvent is very low, the two substances can hardly be removed by various methods, the XRD pattern of the patent shows that the synthesis effect is very unsatisfactory, and the product purity is low until characteristic peaks hardly appear. The preparation of high purity copper nitride nanocrystals remains a significant challenge.
Disclosure of Invention
The present invention aims at solving the above background technology deficiencies and providing a method for preparing copper nitride nanocrystals with high purity and without the need of separation and purification of the product.
The technical scheme of the invention is as follows: a preparation method of high-purity copper nitride nanocrystals is characterized by comprising the following steps: in an oxygen-free, water-free and inert gas environment, nano Cu is added2And uniformly mixing the O and the urea according to the molar ratio of 1:1.5-4, pouring the mixture into a sealed container for sealing, transferring the sealed container into a heating device filled with inert gas, heating to the temperature of 150-. In the scheme, the inert gas is argon or nitrogen, the heating device is preferably a heating furnace, and the heating furnace is sealedThe stainless steel hydrothermal kettle is preferably selected as the container, and the proper molar ratio and heating temperature in the scheme are favorable for the urea to remove the nano Cu2And (3) carrying out high-speed reduction on the O to obtain a product with the purity as high as 98.59-99.79%.
Preferably, the steps are as follows:
a. in a glove box, under the environment of no oxygen, no water and argon, nano Cu is added2Mixing O and urea uniformly according to a molar ratio of 1:1.5-4, and pouring into a stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle to a heating furnace filled with argon, heating to 150-210 ℃, keeping the temperature for 6-18h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, and drying to obtain the copper nitride nanocrystal.
Further, the nano Cu2The molar ratio of O to urea is 1: 2-3.
Furthermore, the heating rate of the stainless steel hydrothermal kettle is 1-5 ℃/min.
Furthermore, the heating rate of the stainless steel hydrothermal kettle is 3-5 ℃/min.
Furthermore, the stainless steel hot kettle is heated to 190 ℃ at 170 ℃ and then is kept at the constant temperature for 8-12 h.
Further, the method comprises the following steps:
a. in a glove box, under the environment of no oxygen, no water and argon, nano Cu is added2Mixing O and urea uniformly according to a molar ratio of 1:2-3, and pouring into a stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle out of the glove box to a heating furnace filled with argon, heating to 170-190 ℃ at a heating rate of 3-5 ℃/min, keeping the temperature for 8-12h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, and drying to obtain the copper nitride nanocrystal. In the scheme, the temperature rise at a proper rate is favorable for the urea to remove the nano Cu2And O is reduced at a high speed, and the purity of the obtained product is as high as 99.45-99.79%.
Further, the method comprises the following steps:
a. in a glove box, under the environment of no oxygen, no water and argon, nano Cu is added2Mixing O and urea uniformly according to a molar ratio of 1:2, and pouring into a stainless steel hydrothermal kettle;
b. stainless steel to be sealed completelyAnd (3) moving the hydrothermal kettle out of the glove box to a heating furnace filled with argon, heating to 190 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 8h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, and drying to obtain the copper nitride nanocrystal. In the scheme, the nano Cu is favorably mixed with urea at the molar ratio of 1:2 and the reaction temperature of 190 DEG C2And (4) completely reducing O to obtain the product with the purity as high as 99.79%.
In the present invention, nano Cu2O and urea are both in powder state and analytically pure, and finally the stainless steel hydrothermal kettle (sealing device) is opened, so that the product is in a slightly moist powder state because the urea is in a closed inert gas environment for the nano Cu2O is reduced to obtain copper nitride and CO2、H2O and a small amount of impurities, and drying to obtain the copper nitride nano crystal with the purity of more than 98.5 percent.
The invention has the beneficial effects that:
1. nano Cu2O and urea are directly subjected to solid-state reaction, a solvent is not required to provide a reaction site, a product is not required to be separated from the solvent, and other subsequent treatments are not required, so that the solid copper nitride nanocrystal with the purity of more than 98% is directly obtained, and the purity is greatly improved.
2. The source of the reactant is wide, no solvent is needed, the reaction temperature is 150-210 ℃, and the whole preparation method is efficient, economical, environment-friendly and energy-saving.
Drawings
FIG. 1 is an XRD pattern of copper nitride nanocrystals prepared in the prior art
FIG. 2 is an XRD pattern of copper nitride nanocrystals prepared in accordance with the present invention
FIG. 3 is an SEM image of copper nitride nanocrystals prepared in the present invention
Detailed Description
The invention is described in further detail below with reference to the figures and the specific embodiments.
Example 1
The preparation method of the copper nitride nanocrystal comprises the following steps:
a. in a glove box O2＜0.1ppm、H2O is less than 0.1ppm, under the argon atmosphere, the nano Cu is added2O (0.30g) and urea (0.252g) are evenly mixed according to the mol ratio of 1:2 and poured into a specificationIn a 50ml stainless steel water heating kettle (with polytetrafluoroethylene as a lining), a bottle cap is screwed tightly to seal the stainless steel water heating kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle to a tubular heating furnace filled with argon, heating to 190 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 8h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, drying at 40 ℃, and drying in vacuum to obtain copper nitride nanocrystals, and determining the purity of the copper nitride nanocrystals.
Example 2
The preparation method of the copper nitride nanocrystal comprises the following steps:
a. in a glove box O2＜0.1ppm、H2O is less than 0.1ppm, under the argon atmosphere, the nano Cu is added2Mixing O (0.15g) and urea (0.126g) uniformly according to a molar ratio of 1:2, pouring the mixture into a stainless steel hydrothermal kettle (lining polytetrafluoroethylene) with the specification of 50ml, and screwing a bottle cap to seal the stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle to a tubular heating furnace filled with argon, heating to 170 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 8h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, drying at 40 ℃ in vacuum to obtain copper nitride nanocrystals, and measuring the purity of the copper nitride nanocrystals.
Example 3
The preparation method of the copper nitride nanocrystal comprises the following steps:
a. in a glove box O2＜0.1ppm、H2O is less than 0.1ppm, under the argon atmosphere, the nano Cu is added2Mixing O (0.30g) and urea (0.315g) uniformly according to a molar ratio of 1:2.5, pouring the mixture into a stainless steel hydrothermal kettle (lining polytetrafluoroethylene) with the specification of 50ml, and screwing a bottle cap to seal the stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle to a tubular heating furnace filled with argon, heating to 180 ℃ at a heating rate of 4 ℃/min, keeping the temperature for 10 hours, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, drying at 40 ℃ in vacuum to obtain copper nitride nanocrystals, and measuring the purity of the copper nitride nanocrystals.
Example 4
The preparation method of the copper nitride nanocrystal comprises the following steps:
a. in a glove box O2＜0.1ppm、H2O is less than 0.1ppm, under the argon atmosphere, the nano Cu is added2Mixing O (0.30g) and urea (0.277g) uniformly according to a molar ratio of 1:2.2, pouring the mixture into a stainless steel hydrothermal kettle (lining polytetrafluoroethylene) with the specification of 50ml, and screwing a bottle cap to seal the stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle to a tubular heating furnace filled with argon, heating to 185 ℃ at a heating rate of 3 ℃/min, keeping the temperature for 12h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, drying at 40 ℃ in vacuum to obtain copper nitride nanocrystals, and measuring the purity of the copper nitride nanocrystals.
Example 5
The preparation method of the copper nitride nanocrystal comprises the following steps:
a. in a glove box O2＜0.1ppm、H2O is less than 0.1ppm, under the argon atmosphere, the nano Cu is added2Mixing O (0.30g) and urea (0.378g) uniformly according to a molar ratio of 1:3, pouring the mixture into a stainless steel hydrothermal kettle (lined with polytetrafluoroethylene) with the specification of 50ml, and screwing a bottle cap to seal the stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle to a tubular heating furnace filled with argon, heating to 175 ℃ at a heating rate of 3 ℃/min, keeping the temperature for 12h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, drying at 40 ℃ in vacuum to obtain copper nitride nanocrystals, and measuring the purity of the copper nitride nanocrystals.
Example 6
The preparation method of the copper nitride nanocrystal comprises the following steps:
a. in a glove box O2＜0.1ppm、H2O is less than 0.1ppm, under the argon atmosphere, the nano Cu is added2Mixing O (0.30g) and urea (0.189g) uniformly according to a molar ratio of 1:1.5, pouring the mixture into a stainless steel hydrothermal kettle (lining polytetrafluoroethylene) with the specification of 50ml, and screwing a bottle cap to seal the stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle to a tubular heating furnace filled with argon, heating to 160 ℃ at a heating rate of 1 ℃/min, keeping the temperature for 14h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, drying at 45 ℃ in vacuum to obtain copper nitride nanocrystals, and measuring the purity of the copper nitride nanocrystals.
Example 7
The preparation method of the copper nitride nanocrystal comprises the following steps:
a. in a glove box O2＜0.1ppm、H2O is less than 0.1ppm, under the argon atmosphere, the nano Cu is added2Mixing O (0.30g) and urea (0.227g) uniformly according to a molar ratio of 1:1.8, pouring the mixture into a stainless steel hydrothermal kettle (lining polytetrafluoroethylene) with the specification of 50ml, and screwing a bottle cap to seal the stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle to a tubular heating furnace filled with argon, heating to 200 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 6h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, drying at 45 ℃ in vacuum to obtain copper nitride nanocrystals, and measuring the purity of the copper nitride nanocrystals.
Example 8
The preparation method of the copper nitride nanocrystal comprises the following steps:
a. in a glove box O2＜0.1ppm、H2O is less than 0.1ppm, under the argon atmosphere, the nano Cu is added2Mixing O (0.30g) and urea (0.441g) uniformly according to a molar ratio of 1:3.5, pouring the mixture into a stainless steel hydrothermal kettle (lining polytetrafluoroethylene) with the specification of 50ml, and screwing a bottle cap to seal the stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle to a tubular heating furnace filled with argon, heating to 150 ℃ at a heating rate of 1.5 ℃/min, keeping the temperature for 14h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, drying at 50 ℃ in vacuum to obtain copper nitride nanocrystals, and determining the purity of the copper nitride nanocrystals.
Example 9
The preparation method of the copper nitride nanocrystal comprises the following steps:
a. in a glove box O2＜0.1ppm、H2O is less than 0.1ppm, under the argon atmosphere, the nano Cu is added2Uniformly mixing O (0.30g) and urea (0.479g) according to a molar ratio of 1:3.8, pouring the mixture into a stainless steel hydrothermal kettle (lining polytetrafluoroethylene) with the specification of 50ml, and screwing a bottle cap to seal the stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle to a tubular heating furnace filled with argon, heating to 210 ℃ at a heating rate of 2 ℃/min, keeping the temperature for 18h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, drying at 50 ℃ in vacuum to obtain copper nitride nanocrystals, and measuring the purity of the copper nitride nanocrystals.
Example 10
The preparation method of the copper nitride nanocrystal comprises the following steps:
a. in a glove box O2＜0.1ppm、H2O is less than 0.1ppm, under the argon atmosphere, the nano Cu is added2Mixing O (0.30g) and urea (0.504g) uniformly according to a molar ratio of 1:4, pouring the mixture into a stainless steel hydrothermal kettle (lining polytetrafluoroethylene) with the specification of 50ml, and screwing a bottle cap to seal the stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle to a tubular heating furnace filled with argon, heating to 205 ℃ at a heating rate of 1 ℃/min, keeping the temperature for 15h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, drying at 50 ℃ in vacuum to obtain copper nitride nanocrystals, and measuring the purity of the copper nitride nanocrystals.
The purities of the copper nitride nanocrystals obtained in examples 1 to 10 are shown in table 1 below, and it can be seen from table 1 that the purities of the obtained products are as high as 98.59 to 99.79%.
TABLE 1 purity of copper nitride nanocrystals obtained in examples 1-10
The XRD spectrum of the product copper nitride particles obtained in the above examples is shown in fig. 2, and it can be seen from fig. 2 that the baseline is stable and the characteristic peak is distinct, thus proving that high-purity copper nitride particles are successfully synthesized.
Scanning electron microscope images of the copper nitride particles obtained in the above examples at different magnifications are shown in fig. 3. As can be seen from fig. 3, the sample has a high degree of uniformity in morphology and a cubic structure. The particles crystallized well and were of uniform size and were distributed in the 2 μm range.
Claims (6)
1. A preparation method of high-purity copper nitride nanocrystals is characterized by comprising the following steps:
a. in a glove box, under the environment of no oxygen, no water and argon, nano Cu is added2Mixing O and urea according to the mol ratio of 1:2-3Pouring the mixture into a stainless steel hydrothermal kettle after uniform mixing;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle to a heating furnace filled with argon, heating to 150-210 ℃, keeping the temperature for 6-18h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, and drying to obtain the copper nitride nanocrystal.
2. The method for preparing high-purity copper nitride nanocrystals according to claim 1, wherein the stainless steel hydrothermal reactor is heated at a temperature-rising rate of 1 to 5 ℃/min.
3. The method for preparing high-purity copper nitride nanocrystals according to claim 2, wherein the temperature rise rate of the stainless steel hydrothermal reactor is 3-5 ℃/min.
4. The method for preparing high-purity copper nitride nanocrystals according to claim 2, wherein the stainless steel is heated in a hot kettle to 190 ℃ and then kept at the temperature for 8-12 h.
5. The method for preparing high-purity copper nitride nanocrystals according to claim 1, comprising the steps of:
a. in a glove box, under the environment of no oxygen, no water and argon, nano Cu is added2Mixing O and urea uniformly according to a molar ratio of 1:2-3, and pouring into a stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle out of the glove box to a heating furnace filled with argon, heating to 170-190 ℃ at a heating rate of 3-5 ℃/min, keeping the temperature for 8-12h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, and drying in vacuum at 40-50 ℃ to obtain the copper nitride nanocrystal.
6. The method for preparing high-purity copper nitride nanocrystals according to claim 5, comprising the steps of:
a. in a glove box, under the environment of no oxygen, no water and argon, nano Cu is added2Mixing O and urea uniformly according to a molar ratio of 1:2, and pouring into a stainless steel hydrothermal kettle;
b. and (3) moving the completely sealed stainless steel hydrothermal kettle out of the glove box to a heating furnace filled with argon, heating to 190 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 8h, cooling to room temperature, opening the stainless steel hydrothermal kettle, taking out the product, and drying in vacuum at 40 ℃ to obtain the copper nitride nanocrystal.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257836A (en) * | 1998-12-23 | 2000-06-28 | 中国科学院物理研究所 | Process for synthesizing nm-class GaN material |
| CN1733600A (en) * | 2005-07-22 | 2006-02-15 | 西安交通大学 | Method for solid-phase double decomposition to synthesize nanometer aluminium nitride |
| CN102211763A (en) * | 2011-04-14 | 2011-10-12 | 中国科学院长春应用化学研究所 | Method for preparing copper nitride nano crystalline |
| CN102491290A (en) * | 2011-12-12 | 2012-06-13 | 沈阳化工大学 | Method for preparing copper nitride powder |
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| CN102139920B (en) * | 2010-01-28 | 2012-12-05 | 中国科学院青岛生物能源与过程研究所 | Preparation method for nanoscale transition metal nitride/carbon composite material |
| US10118833B2 (en) * | 2014-10-02 | 2018-11-06 | Cornell University | Dimensionally focused nanoparticle synthesis methodology |
| CN106672921B (en) * | 2016-12-26 | 2019-01-15 | 华中科技大学 | A kind of preparation method of two-dimensional metallic compound-material |
| CN107324396B (en) * | 2017-06-06 | 2019-05-31 | 江苏大学 | A kind of preparation method based on iron oxide doped graphite phase carbon nitride composite material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257836A (en) * | 1998-12-23 | 2000-06-28 | 中国科学院物理研究所 | Process for synthesizing nm-class GaN material |
| CN1733600A (en) * | 2005-07-22 | 2006-02-15 | 西安交通大学 | Method for solid-phase double decomposition to synthesize nanometer aluminium nitride |
| CN102211763A (en) * | 2011-04-14 | 2011-10-12 | 中国科学院长春应用化学研究所 | Method for preparing copper nitride nano crystalline |
| CN102491290A (en) * | 2011-12-12 | 2012-06-13 | 沈阳化工大学 | Method for preparing copper nitride powder |
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