CN114671454A - Method for synthesizing novel phase chalcocite-H copper sulfide ferromagnetic material at high temperature and high pressure - Google Patents
Method for synthesizing novel phase chalcocite-H copper sulfide ferromagnetic material at high temperature and high pressure Download PDFInfo
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- CN114671454A CN114671454A CN202210285040.XA CN202210285040A CN114671454A CN 114671454 A CN114671454 A CN 114671454A CN 202210285040 A CN202210285040 A CN 202210285040A CN 114671454 A CN114671454 A CN 114671454A
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- C01G3/12—Sulfides
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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Abstract
The invention discloses a method for synthesizing a new-phase chalcocite-H copper sulfide ferromagnetic material at high temperature and high pressure, which belongs to the technical field of preparation of ferromagnetic materials, and comprises the steps of firstly assembling a pressure maintaining device, arranging a sample raw material (6), a sample cavity (5), a hard alloy mold (10), mold steel (4) and a heating resistance wire (3) in a cavity of the pressure maintaining device from a high-temperature end to a low-temperature end in sequence, then placing the assembled pressure maintaining device in a common double-face top press, pressurizing for 2-4 GPa, heating to 300-500 ℃, maintaining the pressure and keeping the temperature for 60-100 minutes, cooling to 20-30 ℃, relieving the pressure to 0GPa, removing hard alloy punches (9) at two ends, and cleaning the surface of a sample to obtain the new-phase chalcocite-H copper sulfide ferromagnetic material. The preparation method is simple, has low cost and can meet the requirement of batch production.
Description
Technical Field
The invention belongs to the technical field of ferromagnetic material preparation, and particularly relates to a method for synthesizing a new phase Chalcocite-H (Chalcocite-H) copper sulfide ferromagnetic material under extreme conditions of high temperature and high pressure.
Background
Copper sulfide is a multifunctional material integrating a plurality of excellent properties, and with the development of nanotechnology, the copper sulfide nanometer material has better photoelectric property, catalytic capability, high conductivity and high electric energy property than the traditional material due to quantum size effect, surface effect and macroscopic quantum tunnel effect, so that the copper sulfide has wide application in many fields.
At present, the copper sulfide nano material has small magnetism, and most means for changing the magnetism are focused on doping magnetic atoms, synthesizing magnetic composite materials and the like. The high-temperature and high-pressure technology is an important means for changing the magnetism of the material, and the atomic position, the atomic distance and the electronic structure of atoms of a unit cell are changed through regulating and controlling the temperature and the pressure, so that the material is subjected to phase change, and the magnetism of the material is further changed. The high-temperature and high-pressure technology plays an important role in exploring new materials, is a novel way for researching the phase change mechanism of a substance, can enable the substance to have a new structure and performance under extreme conditions, and expands the application field of the material.
The invention uses the aerosol condensation chemical deposition method to synthesize the copper sulfide nano-particles as the raw material, and explores the synthesis of the ferromagnetic material. The new phase Chalcocite-H copper sulfide ferromagnetic material is successfully synthesized under high temperature and high pressure.
Disclosure of Invention
The invention aims to provide a method for synthesizing a new phase Chalcocite-H copper sulfide ferromagnetic material at high pressure and high temperature. The phase change of the copper sulfide is directionally induced by the regulation and control of proper pressure and proper synthesis temperature, and the new phase Chalcocite-H copper sulfide has stronger ferromagnetism.
The technical scheme adopted by the invention is as follows:
a method for synthesizing a new-phase chalcocite-H copper sulphide ferromagnetic material at high temperature and high pressure adopts a high-temperature and high-pressure method to synthesize a new-phase chalcocite-H copper sulphide ferromagnetic material, firstly, a pressure maintaining device is assembled according to the following steps, so that a sample raw material 6, a sample cavity 5, a hard alloy mould 10, mould steel 4 and a heating resistance wire 3 are sequentially arranged in a cavity of the pressure maintaining device from a high-temperature end to a low-temperature end:
1) placing the hard alloy die 10 into die steel 4 to form a high-pressure die, and placing the thermocouple probe 2 into a hole position of the high-pressure die;
2) placing the hard alloy punch 9 at the left end into a high-pressure die to enable the punch to be close to the thermocouple probe 2;
3) a sample raw material 6 is placed in a sample cavity 5, and a hard alloy punch 9 at the right end is placed in a high-pressure die;
4) the outermost layer of the high-pressure die is wrapped with a heating resistance wire 3.
And then, placing the assembled pressure maintaining device in a common double-sided pressing machine, pressurizing for 2-4 GPa, heating to 300-500 ℃, maintaining the pressure and the temperature for 60-100 minutes, cooling to 20-30 ℃, releasing the pressure to 0GPa, removing the hard alloy punches 9 at two ends, and cleaning the surface of the sample to obtain the new-phase chalcocite-H copper sulfide ferromagnetic material.
Preferably, the cemented carbide mold 10 is a YG8 cemented carbide mold.
Preferably, the sample raw material 6 is a copper sulfide nanoparticle initial raw material synthesized by an aerosol condensation chemical deposition method, and is prepared by the following method: sufficient hydrogen sulfide gas reacts with the copper acetate gas mist in the environment of circulating water bath, and copper sulfide nano-particle initial raw materials are generated through precipitation.
Has the advantages that: the invention provides a method for synthesizing a new phase Chalcocite-H copper sulphide ferromagnetic material at high pressure and high temperature, compared with the prior art, the magnetism of copper sulphide is easier to be greatly changed, and the new phase Chalcocite-H copper sulphide ferromagnetic material is easier to obtain by the method, thereby meeting the requirements of some fields on ferromagnetic materials. The preparation method is simple, has low cost, and can meet the requirement of batch production.
Drawings
FIG. 1 is a schematic diagram of the assembly of a new phase Chalcocite-H copper sulfide ferromagnetic material synthesized at high temperature and high pressure.
FIG. 2 is an X-ray diffraction pattern of the copper sulfide nanoparticle starting material synthesized in example 1.
FIG. 3 is a M-H diagram of the copper sulfide nanoparticle starting material synthesized in example 1.
FIG. 4 is an X-ray diffraction pattern of the new phase Chalcocite-H copper sulfide ferromagnetic material synthesized in example 1.
FIG. 5 is an M-H plot of the new phase Chalcocite-H copper sulfide ferromagnetic material synthesized in example 1.
Detailed Description
The examples are merely to illustrate the present invention more specifically, and the present invention is not limited to the examples.
Example 1:
sufficient hydrogen sulfide gas meets copper acetate gas fog under the condition of circulating water bath with the ambient temperature of 20-40 ℃ to generate copper sulfide nano-particle initial raw material. The synthesized copper sulfide nanoparticles were subjected to X-ray diffraction and hysteresis loop tests, and the results are shown in fig. 2 and 3.
The pressurizer was assembled as shown in FIG. 1. The synthesis pressure was 3GPa and the temperature was 400 ℃. In the synthesis chamber, a sample material 6 (i.e. copper sulphide nanoparticle starting material) is placed in a high temperature end sample chamber 5, the sample chamber 5 is placed in the center of a cemented carbide mold 10, and mold steel 4 is arranged around the cemented carbide 10. And simultaneously applying pressure to two ends of the hard alloy punch 9, setting a required temperature value, keeping the pressure for 100 minutes, and then cooling and releasing the pressure. And removing pressure transmission media at two ends of the sample, cleaning the surface of the sample, and then testing the sample by XRD and a magnetic hysteresis loop. The X-ray diffraction pattern of the Chalcocite-H copper sulfide synthesized under the conditions is compared with that of the copper sulfide nano-particles, the diffraction peaks are obviously different, phase change is generated, and the corresponding PDF card is not included in the crystallography database, so that the Chalcocite-H copper sulfide is a new phase, and the result is shown in a figure 4. The sample was passed through the magnetic test at room temperature and gave a better hysteresis loop, the result of which is shown in FIG. 5. The new phase Chalcocite-H copper sulfide ferromagnetic material is proved to retain stronger ferromagnetism relative to the copper sulfide nanoparticle initial raw material.
Claims (3)
1. A method for synthesizing a new-phase Chalcocite-H copper sulphide ferromagnetic material at high temperature and high pressure comprises the steps of synthesizing the new-phase Chalcocite-H copper sulphide of a stronger ferromagnetic material by adopting a high-temperature and high-pressure method, firstly assembling a pressure maintaining device according to the following steps, and sequentially arranging a sample raw material (6), a sample cavity (5), a hard alloy mold (10), mold steel (4) and a heating resistance wire (3) from a high-temperature end to a low-temperature end in a cavity of the pressure maintaining device:
1) placing the hard alloy die (10) into die steel (4) to form a high-pressure die, and placing the thermocouple probe (2) into a hole position of the high-pressure die;
2) placing a hard alloy punch (9) at the left end into a high-pressure die to enable the punch to be close to the thermocouple probe (2);
3) a sample raw material (6) is placed in a sample cavity (5), and a hard alloy punch head (9) at the right end is placed in a high-pressure die;
4) the outermost layer of the high-pressure die is wrapped with a heating resistance wire (3);
and then, placing the assembled pressure maintaining device in a common double-sided pressing machine, pressurizing for 2-4 GPa, heating to 300-500 ℃, maintaining the pressure and the temperature for 60-100 minutes, cooling to 20-30 ℃, relieving the pressure to 0GPa, removing hard alloy punches (9) at two ends, and cleaning the surface of the sample to obtain the new-phase Chalcocite-H copper sulfide ferromagnetic material.
2. A method for high temperature high pressure synthesis of a new phase chalcocite-H copper sulphide ferromagnetic material according to claim 1, characterized in that the cemented carbide mould (10) is a YG8 cemented carbide mould.
3. The method for synthesizing a new-phase chalcocite-H copper sulfide ferromagnetic material at high temperature and high pressure according to claim 1, wherein the sample raw material (6) is a raw material of copper sulfide nanoparticles synthesized by aerosol condensation chemical deposition method, and is prepared by the following method: sufficient hydrogen sulfide gas reacts with the copper acetate aerial fog in the environment of circulating water bath, and copper sulfide nanoparticle initial raw materials are generated through precipitation.
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| CN202210285040.XA CN114671454B (en) | 2022-03-22 | 2022-03-22 | Method for synthesizing new-phase chalcocite-H copper sulfide ferromagnetic material at high temperature and high pressure |
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| CN202210285040.XA CN114671454B (en) | 2022-03-22 | 2022-03-22 | Method for synthesizing new-phase chalcocite-H copper sulfide ferromagnetic material at high temperature and high pressure |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR983408A (en) * | 1943-08-13 | 1951-06-22 | Process for obtaining pure cuprous sulphides | |
| CN102616830A (en) * | 2012-04-11 | 2012-08-01 | 吉林大学 | Preparation method of rock-salt mine structure Co-doped CdS diluted magnetic semiconductor nanoparticles |
| CN111620696A (en) * | 2020-06-09 | 2020-09-04 | 吉林大学 | Preparation method of high-hardness ferromagnetic alpha-MnB |
| CN111829849A (en) * | 2020-07-24 | 2020-10-27 | 中国科学院地球化学研究所 | Method for directly synthesizing high-purity and high-density chalcopyrite block material by solid-phase reaction |
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- 2022-03-22 CN CN202210285040.XA patent/CN114671454B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR983408A (en) * | 1943-08-13 | 1951-06-22 | Process for obtaining pure cuprous sulphides | |
| CN102616830A (en) * | 2012-04-11 | 2012-08-01 | 吉林大学 | Preparation method of rock-salt mine structure Co-doped CdS diluted magnetic semiconductor nanoparticles |
| CN111620696A (en) * | 2020-06-09 | 2020-09-04 | 吉林大学 | Preparation method of high-hardness ferromagnetic alpha-MnB |
| CN111829849A (en) * | 2020-07-24 | 2020-10-27 | 中国科学院地球化学研究所 | Method for directly synthesizing high-purity and high-density chalcopyrite block material by solid-phase reaction |
Non-Patent Citations (2)
| Title |
|---|
| CHAOJUN FANG等: ""How Ferric Salt Enhances the First-Stage Acidic Leaching of Chalcocite: Performance of Intermediate Crystallite"", 《JOM》 * |
| 陈海英 等: ""铜纳米材料的制备、应用及安全性研究进展"", 《化工新型材料》 * |
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