CN114368775A - Room temperature rapid preparation method of transition metal sulfide - Google Patents
Room temperature rapid preparation method of transition metal sulfide Download PDFInfo
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- CN114368775A CN114368775A CN202111564305.1A CN202111564305A CN114368775A CN 114368775 A CN114368775 A CN 114368775A CN 202111564305 A CN202111564305 A CN 202111564305A CN 114368775 A CN114368775 A CN 114368775A
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- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
- C01G1/12—Sulfides
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Abstract
The invention relates to a room-temperature rapid preparation method of transition metal sulfide, which mainly solves the problem that the traditional transition metal sulfide cannot be rapidly synthesized at room temperature. The invention dissolves solid elemental sulfur powder in the carbon disulfide solution to convert the elemental sulfur powder into a liquid phase, greatly improves the surface energy of sulfur and obviously improves the reaction activity of the sulfur. Meanwhile, nano-scale metal material particles with high surface energy and high reaction activity are used as precursors. By utilizing the synergistic effect of the liquid sulfur and the nano metal particles, the reaction driving force of elemental sulfur and transition metal elemental substances is effectively improved, the elemental sulfur can react with the nano-scale transition metal elemental particles under the induction of concentration gradient to quickly form transition metal sulfides, and the room-temperature quick preparation of the transition metal sulfides is realized.
Description
Technical Field
The invention relates to the field of energy storage material preparation and photoelectric information material synthesis, in particular to a room-temperature rapid preparation method of a transition metal sulfide.
Background
The transition metal sulfide is a novel material with two-dimensional layered structure characteristics, has excellent mechanical properties, thermal stability and semiconductor characteristics, shows unique optical and electrochemical properties, and has wide application in electrochemical energy storage, conversion and integrated circuits. At present, the preparation methods of transition metal sulfides are mainly chemical vapor deposition, hydrothermal, electrostatic spinning, lift-off, sol-gel methods. The chemical vapor deposition method is the most widely applied transition metal sulfide preparation method at present, and can accurately control the thickness and the crystal structure of a transition metal sulfide product through parameter regulation, but the method has high cost and large energy consumption, and limits the wide application of the method in industrial production; the hydrothermal method can realize low-cost rapid preparation of the transition metal sulfide, but the method generally needs more template materials, has high requirements on the temperature and pressure control precision of equipment and has certain potential safety hazard; the electrostatic spinning method can grow the transition metal sulfide with a network-shaped fiber staggered distribution structure, but has low yield and is not suitable for large-scale production; the stripping method can obtain high-quality single-layer transition metal sulfide, but the production efficiency is extremely low, and the stripping method cannot be applied to actual production; the sol-gel method can prepare the transition metal sulfide with the aerogel structure, but the used raw materials have higher cost and the preparation method is more complex, so the method is not suitable for industrial production. In addition, the above methods often require heating or pressurizing the raw materials, reducing production efficiency and increasing energy consumption. It can be seen that there is a gap in the current technology for the rapid preparation of transition metal sulfides at room temperature. Therefore, there is an urgent need to develop a new method for rapidly preparing transition metal sulfides at room temperature and atmospheric pressure to effectively overcome the above problems.
Disclosure of Invention
In order to solve the problems, the invention is based on the following two design ideas: (1) after the object is subjected to phase transformation from a solid phase to a liquid phase, the crystal structure of the object is remarkably changed, the surface energy is greatly improved, and the reactivity of the material can be remarkably improved; (2) after the material is subjected to size nanocrystallization, the specific surface area is increased, the surface energy is greatly improved, and the reaction activity is obviously improved. Based on the thought, the solid elemental sulfur powder is dissolved in the carbon disulfide solution, so that the elemental sulfur powder is converted into a liquid phase, the surface energy of sulfur is greatly improved, and the reaction activity of the sulfur is remarkably improved. Meanwhile, nano-scale metal material particles with high surface energy and high reaction activity are used as precursors. By utilizing the synergistic effect of the liquid sulfur and the nano metal particles, the reaction driving force of elemental sulfur and the transition metal elemental substance is effectively improved, the elemental sulfur can react with the nano metal elemental substance particles under the induction of concentration gradient to quickly form the transition metal sulfide, and the quick preparation of the transition metal sulfide at room temperature is realized.
Aiming at the problem that the existing room temperature rapid preparation technology of transition metal sulfide has a blank, the invention is to dissolve solid elemental sulfur powder into carbon disulfide solution based on the design idea of material phase change and material nanocrystallization, so that the elemental sulfur powder is converted into a liquid phase, thereby greatly improving the surface energy of sulfur and remarkably improving the reaction activity of sulfur. Meanwhile, nanoscale transition metal simple substance particles with high surface energy and high reaction activity are used as precursors. By utilizing the synergistic effect of the liquid sulfur and the nanoscale transition metal simple substance particles, the reaction driving force of the simple substance sulfur and the transition metal simple substance is effectively improved, the simple substance sulfur can react with the nanoscale transition metal simple substance particles under the induction of concentration gradient to quickly form the transition metal sulfide, and the quick preparation of the transition metal sulfide at room temperature is realized.
The basic technical scheme of the invention comprises the following specific steps:
firstly, placing sulfur powder in carbon disulfide liquid, and magnetically stirring at room temperature to obtain a uniformly mixed carbon disulfide solution of sulfur;
completely immersing transition metal powder with certain mass and nanometer scale in the obtained carbon disulfide solution of sulfur, and standing;
and thirdly, cleaning the obtained product by using carbon disulfide liquid, then placing the cleaned product in a vacuum drying box, and performing vacuum drying treatment at room temperature to completely remove the carbon disulfide liquid to obtain the transition metal sulfide powder.
In the step (1), the ratio of the sulfur powder to the carbon disulfide liquid is 0.5-50 g: 1 mL-1000 mL; the room temperature is 20 ℃, and the magnetic stirring time is 0.5-5 hours;
in the step (2), the mass ratio of the transition metal to the sulfur powder is 0.1-10: 0.5-50, transition metal is nickel, titanium, manganese, chromium, copper, cobalt, iron, tungsten, molybdenum or niobium, the particle size of the transition metal powder is 10-500 nm, and the standing time is 1-6 hours;
in the step (3), the vacuum drying treatment time is 1-12 hours.
The invention has the beneficial effects that: the invention relates to a room temperature rapid preparation method of transition metal sulfide, which dissolves solid elemental sulfur powder sulfur in a carbon disulfide solution to convert the sulfur powder sulfur into a liquid phase, greatly improves the surface energy of the sulfur, and obviously improves the reaction activity of the sulfur. Meanwhile, nano-scale metal material particles with high surface energy and high reaction activity are used as precursors. By utilizing the synergistic effect of the liquid sulfur and the nano metal particles, the reaction driving force of elemental sulfur and a metal elemental substance is effectively improved, the elemental sulfur can react with the nano metal elemental substance particles under the diffusion action to quickly form a transition metal sulfide, and the quick preparation of the transition metal sulfide at room temperature is realized. The invention has the following advantages:
1. the invention has wide application range, is suitable for various transition metal elements, and can meet the production requirements of various functional sulfide materials.
2. The invention realizes the room-temperature rapid preparation of the transition metal sulfide, has simple and efficient method, can effectively improve the production efficiency and reduce the production cost, and is suitable for industrial production.
3. The transition metal sulfide prepared by the method is nano-particles, has large surface area and high activity, and can more effectively exert the energy storage, catalysis and photoelectric properties of the transition metal sulfide material compared with the same transition metal sulfide material with the traditional scale.
Drawings
Fig. 1 shows the secondary electron morphology of the nano copper sulfide prepared by the first embodiment. It can be seen that the nano copper particles have been transformed into nano copper sulfide particles with lamellar structure characteristics, and the particles are uniformly distributed and do not agglomerate.
Fig. 2 is an X-ray diffraction line of the nano copper sulfide product prepared by the fourth embodiment. It can be seen that the typical characteristic peaks of the product are consistent with those of the standard card JCPDS No.79-232 of copper sulfide, indicating that the product is copper sulfide with high crystallinity.
Detailed Description
The invention discloses a room temperature rapid preparation method of transition metal sulfide, which is characterized in that solid elemental sulfur powder is dissolved in carbon disulfide solution to be converted into liquid phase, thereby greatly improving the surface energy of sulfur and remarkably improving the reaction activity of sulfur. Meanwhile, nano-scale metal material particles with high surface energy and high reaction activity are used as precursors. By utilizing the synergistic effect of the liquid sulfur and the nano metal particles, the reaction driving force of elemental sulfur and the transition metal elemental substance is effectively improved, the elemental sulfur can react with the nano metal elemental substance particles under the induction of concentration gradient to quickly form the transition metal sulfide, and the quick preparation of the transition metal sulfide at room temperature is realized.
The first embodiment is as follows: the room temperature fast transition metal sulfide preparing process includes the following steps:
firstly, 1g of sulfur powder is placed in 20mL of carbon disulfide liquid, and is magnetically stirred for 1 hour at room temperature (20 ℃) to obtain a uniformly mixed carbon disulfide solution of sulfur;
completely immersing 0.2g of nano copper powder with the particle size of 100nm into the obtained carbon disulfide solution of sulfur, and standing for 2 hours;
and thirdly, washing the obtained product by using 20mL of carbon disulfide liquid, then placing the washed product in a vacuum drying oven, and carrying out vacuum drying treatment for 2 hours at room temperature (20 ℃) to completely remove the carbon disulfide liquid, thereby obtaining the transition metal sulfide powder.
The beneficial effects of the embodiment are as follows: the invention relates to a room temperature rapid preparation method of transition metal sulfide, which dissolves solid elemental sulfur powder sulfur in a carbon disulfide solution to convert the sulfur powder sulfur into a liquid phase, greatly improves the surface energy of the sulfur, and obviously improves the reaction activity of the sulfur. Meanwhile, nano-scale metal material particles with high surface energy and high reaction activity are used as precursors. By utilizing the synergistic effect of the liquid sulfur and the nano metal particles, the reaction driving force of elemental sulfur and the transition metal elemental substance is effectively improved, the elemental sulfur can react with the nano metal elemental substance particles under the induction of concentration gradient to quickly form the transition metal sulfide, and the quick preparation of the transition metal sulfide at room temperature is realized.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: in the first step, the mass of the sulfur powder is 20g, the volume of the carbon disulfide liquid is 500mL, and the magnetic stirring time is 2 hours.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the metal used in the second step is cobalt, the mass is 5g, and the particle size is 60 nm.
The fourth concrete implementation mode: the present embodiment differs from the first to third embodiments in that: step three the volume of carbon disulfide used for cleaning was 50mL, and the vacuum drying treatment time was 12 hours.
Claims (5)
1. A room temperature rapid preparation method of transition metal sulfide is characterized by comprising the following steps: solid elemental sulfur powder is dissolved in carbon disulfide solution to be converted into liquid phase, so that the surface energy of sulfur is greatly improved, and the reaction activity of sulfur is obviously improved; meanwhile, nanoscale transition metal simple substance particles with high surface energy and high reaction activity are used as precursors, the synergistic effect of the liquid sulfur and the nanoscale transition metal simple substance particles is utilized, the reaction driving force of the simple substance sulfur and the transition metal simple substance is effectively improved, the simple substance sulfur and the nanoscale transition metal simple substance particles can react to quickly form transition metal sulfides under the induction of concentration gradient, and the rapid preparation of the transition metal sulfides at room temperature is realized.
2. The room-temperature rapid preparation method of a transition metal sulfide as claimed in claim 1, characterized by comprising the following steps:
(1) placing sulfur powder in carbon disulfide liquid, and magnetically stirring at room temperature to obtain a uniformly mixed carbon disulfide solution of sulfur;
(2) completely immersing transition metal powder with certain mass and nanometer scale in the obtained carbon disulfide solution of sulfur, and standing;
(3) and (3) cleaning the obtained product by using carbon disulfide liquid, then placing the cleaned product in a vacuum drying box, and carrying out vacuum drying treatment at room temperature to completely remove the carbon disulfide liquid to obtain the transition metal sulfide powder.
3. The room-temperature rapid preparation method of transition metal sulfide as claimed in claim 2, wherein in the step (1), the ratio of sulfur powder to carbon disulfide liquid is 0.5g to 50 g: 1 mL-1000 mL; the room temperature is 20 ℃, and the magnetic stirring time is 0.5-5 hours.
4. The room-temperature rapid preparation method of a transition metal sulfide as claimed in claim 2, wherein in the step (2), the mass ratio of the transition metal to the sulfur powder is 0.1-10: 0.5-50, transition metal is nickel, titanium, manganese, chromium, copper, cobalt, iron, tungsten, molybdenum or niobium, the grain diameter of the transition metal powder is 10-500 nm, and the standing time is 1-6 hours.
5. The room-temperature rapid preparation method of a transition metal sulfide as claimed in claim 2, wherein in the step (3), the vacuum drying treatment time is 1 to 12 hours.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1613750A (en) * | 2004-09-24 | 2005-05-11 | 武汉大学 | Preparation for metal sulfide |
| CN101597776A (en) * | 2009-07-07 | 2009-12-09 | 武汉大学 | A kind of metal sulfide M 1The metallurgical method of S |
| CN105776353A (en) * | 2016-03-29 | 2016-07-20 | 中国石油大学(北京) | Ironic sulfides and preparation method thereof |
| CN106972161A (en) * | 2017-04-05 | 2017-07-21 | 深圳市佩成科技有限责任公司 | A kind of preparation method of nitrogen-doped graphene/copper sulfide/hollow sulphur composite |
-
2021
- 2021-12-20 CN CN202111564305.1A patent/CN114368775A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1613750A (en) * | 2004-09-24 | 2005-05-11 | 武汉大学 | Preparation for metal sulfide |
| CN101597776A (en) * | 2009-07-07 | 2009-12-09 | 武汉大学 | A kind of metal sulfide M 1The metallurgical method of S |
| CN105776353A (en) * | 2016-03-29 | 2016-07-20 | 中国石油大学(北京) | Ironic sulfides and preparation method thereof |
| CN106972161A (en) * | 2017-04-05 | 2017-07-21 | 深圳市佩成科技有限责任公司 | A kind of preparation method of nitrogen-doped graphene/copper sulfide/hollow sulphur composite |
Non-Patent Citations (1)
| Title |
|---|
| MARKETA URBANOVA等: "Room-temperature sulfidation of copper nanoparticles with sulfur yielding covellite nanoparticles", 《COMPTES RENDUS CHIMIE》, pages 511 - 516 * |
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