CN114715930A - Synthesizing CuS by aerosol condensation and chemical deposition: method for manufacturing Ho diluted magnetic semiconductor - Google Patents
Synthesizing CuS by aerosol condensation and chemical deposition: method for manufacturing Ho diluted magnetic semiconductor Download PDFInfo
- Publication number
- CN114715930A CN114715930A CN202210285059.4A CN202210285059A CN114715930A CN 114715930 A CN114715930 A CN 114715930A CN 202210285059 A CN202210285059 A CN 202210285059A CN 114715930 A CN114715930 A CN 114715930A
- Authority
- CN
- China
- Prior art keywords
- ions
- cus
- magnetic semiconductor
- diluted magnetic
- aerosol
- 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.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/006—Compounds containing, besides copper, two or more other elements, with the exception of oxygen or hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/12—Sulfides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/40—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials of magnetic semiconductor materials, e.g. CdCr2S4
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
-
- 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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Abstract
The invention relates to a method for synthesizing CuS by aerosol condensation and chemical deposition: a method for manufacturing a Ho diluted magnetic semiconductor belongs to the technical field of diluted magnetic semiconductor material preparation, and comprises the following steps: generating mixed gas fog of Cu ions and Ho ions by using a mixed solution of Cu ions and Ho ions under the action of an ultrasonic atomization machine, then reacting with hydrogen sulfide gas in a circulating water environment under the driving of a gas driving device, and precipitating in a collection bottle to obtain Ho-doped CuS-based diluted magnetic semiconductor nanoparticles CuS: and Ho. The preparation method is simple, the cost is low, the requirement of batch production can be met, and the obtained Ho-doped CuS-based diluted magnetic semiconductor has room-temperature ferromagnetism.
Description
Technical Field
The invention belongs to the technical field of diluted magnetic semiconductor material preparation, and particularly relates to a method for synthesizing a Ho-doped CuS-based diluted magnetic semiconductor with room-temperature ferromagnetism by adopting aerosol condensation chemical deposition.
Background
The diluted magnetic semiconductor has magnetic properties and semiconductor characteristics, and simultaneously utilizes two degrees of freedom of electrons, namely electron spin and charge, so that the spintronics of two subjects combining magnetism and microelectronics is developed on the basis. In order to make spintronic devices function in practical applications, diluted magnetic semiconductors with room-temperature ferromagnetism must be prepared, and therefore, the search for new materials with room-temperature ferromagnetism becomes the central work of diluted magnetic semiconductor research.
In the long-term research on the preparation of diluted magnetic semiconductors, a number of methods have been developed: molecular beam epitaxy, metal organic chemical vapor deposition, ion implantation, pulsed laser deposition, sol-gel methods, and the like. The methods described above have various features and can be applied to the field of diluted magnetic semiconductors. However, each method has its limitations and still cannot meet the needs of research.
At present, the magnetic property of the CuS nano material is small, and it has been reported that a transition metal Ni ion is doped into a CuS nano particle by using a simple wet chemical coprecipitation method, and a transition from diamagnetism to paramagnetism is obtained, and a diluted magnetic semiconductor having room-temperature ferromagnetism is not obtained after doping. For details, see Subramanyam K, Sreelekha N, Reddy D A, et al chemical synthesis, structural, optical, magnetic characteristics and enhanced visual light activity catalysis of Ni doped CuS nanoparticles [ J ] Solid State Sciences,2017,65:68-78 doping with rare earth ions is a means to effectively change the magnetic properties, which can adjust the electronic structure of the host compound, further increasing the functionality of the material.
The invention utilizes an aerosol condensation chemical deposition method to prepare Ho-doped CuS nano particles and explores the synthesis of diluted magnetic semiconductor materials. Successfully synthesizes the Ho-doped CuS-based diluted magnetic semiconductor material with room-temperature ferromagnetism.
Disclosure of Invention
The invention aims to provide a method for synthesizing a Ho-doped CuS-based diluted magnetic semiconductor by using aerosol condensation chemical deposition. By means of proper raw material proportion and proper synthesis temperature regulation, Ho is effectively doped into CuS nano particles, and the Ho-doped CuS nano particles are diluted magnetic semiconductors with room-temperature ferromagnetism.
The technical scheme adopted by the invention is as follows:
an aerosol condensation chemical deposition synthesis CuS: the method for manufacturing the Ho diluted magnetic semiconductor comprises the following steps:
(1) the sodium sulfide solution and the hydrochloric acid solution generate chemical reaction to provide sufficient hydrogen sulfide gas;
(2) generating mixed aerosol of Cu ions and Ho ions by the mixed solution of Cu ions and Ho ions under the action of an ultrasonic atomizer;
(3) and (3) reacting hydrogen sulfide gas with the mixed gas fog of the Cu ions and the Ho ions in the environment of circulating water under the driving of a gas driving device, and precipitating in a collecting bottle to obtain the Ho-doped CuS-based diluted magnetic semiconductor nanoparticles CuS: Ho.
Preferably, the sodium sulfide solution in the step (1) is Na2S·9H2The mass ratio of O to water is 1: 2-4, preparing a solution; the hydrochloric acid solution is prepared by mixing HCl and water according to a mass ratio of 1: 1-3 of a prepared solution; na (Na)2The molar ratio of S to HCl is 1: 2.
preferably, the molar ratio of the Cu ions to the Ho ions in the mixed solution of Cu ions and Ho ions in the step (2) is 1: 0.001 to 0.15; the mixed aerosol of Cu ions and Ho ions is mixed aerosol of copper acetate and holmium acetate.
Preferably, the environmental temperature of the circulating water in the step (3) is 20-40 ℃; the gas driving device is an air pump.
Has the advantages that:
compared with the prior art, the method for synthesizing the Ho-doped CuS-based diluted magnetic semiconductor by the aerosol condensation chemical deposition method has the advantages that magnetic ions are more easily doped into a main body crystal lattice, so that the magnetism of the CuS is changed. By the method, the obtained Ho-doped CuS-based diluted magnetic semiconductor has room-temperature ferromagnetism, and meets the requirements of some fields on diluted magnetic semiconductor 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 a Ho-doped CuS-based diluted magnetic semiconductor synthesized by an aerosol condensation chemical deposition method. In FIG. 1, 1 is a sodium sulfide solution; 2 is hydrochloric acid solution; 3 is an air valve switch; 4 is hydrogen sulfide gas; 5 is a suck-back prevention bottle; 6 is an ultrasonic atomizer; 7 is a mixed solution of Ho ions and Cu ions; 8 is mixture aerial fog of Ho ions and Cu ions; 9 is circulating water; 10 is a collecting bottle; 11 is an ultrasonic machine; 12 is a circulating water machine; 13 is waste gas; 14 is a suck-back prevention bottle; 15 is sodium hydroxide solution; 16 is an anti-suck back bottle; 17 is a gas driving device; 18 is a separating funnel; 19 is a three-necked bottle; 20 is a flow dividing head; 21 is a condenser; and 22 is a tail gas bottle.
FIG. 2 is a graph comparing the X-ray diffraction patterns of the diluted magnetic semiconductor of CuS: Ho with different doping concentrations synthesized in example 1.
FIG. 3 is a graph of M-H comparison of different concentrations of CuS: Ho diluted magnetic semiconductors synthesized in example 1.
Detailed Description
The examples are provided to illustrate the present invention more specifically, and the present invention is not limited to the examples.
Example 1
The detailed process for synthesizing the Ho-doped CuS-based diluted magnetic semiconductor by the aerosol condensation chemical deposition method comprises the following steps:
(1) in the following steps of 1: selectively weighing medicines according to the required molar ratio range of 0.001-0.15 of copper acetate and holmium acetate, adding holmium acetate, copper acetate and 0.001-0.01 g of polyvinylpyrrolidone into 0.5-2L of deionized ultrapure water, and uniformly stirring on a stirring table for 3-5 hours to prepare a Ho ion and Cu ion mixed solution 7;
(2) the assembled aerosol condensation chemical deposition device is shown in figure 1, a separating funnel 18 filled with a sodium sulfide solution 1 is inserted into one neck opening of a three-neck bottle 19 filled with a hydrochloric acid solution 2, an air valve switch 3 is placed on one neck opening, the air valve switch 3, an anti-suck-back bottle 5 and a side opening of a flow dividing head 20 are sequentially connected, the flow dividing head 20 is arranged at the lower opening, a condenser 21, a collecting bottle 10, an anti-suck-back bottle 14, a tail gas treatment bottle 22, an anti-suck-back bottle 16 and an air driving device 17 are sequentially connected, the collecting bottle 10 is arranged in an ultrasonic machine 11, an ultrasonic atomizer 6 is connected with the upper opening of the flow dividing head 20, and a water circulating machine 12 is connected with the condenser 21. Synthesizing CuS, namely Ho nano particles, wherein the synthesis environment temperature is 20-40 ℃;
(3) and pouring the supernatant part of the fully reacted liquid into a waste liquid barrel, putting the precursor into a centrifugal machine, alternately centrifuging for five times by using water and ethanol, wherein the rotating speed of the centrifugal machine is 8000-10000 rpm, and the centrifuging time is 3-5 min, then putting the centrifuged sample into a freeze drying box, drying for 24-48 h to obtain the CuS: Ho diluted magnetic semiconductor, and testing the sample by using energy dispersion X-ray spectrum, X-ray diffraction and hysteresis loop.
The specific reaction parameters and results selected in this example are as follows:
pure CuS nanoparticles were prepared using this method by weighing 10mmol copper acetate and 0.002g polyvinylpyrrolidone and adding to 1L deionized ultrapure water. Selecting copper acetate and holmium acetate according to molar ratios of 1:0.02, 1:0.04, 1:0.06, 1:0.08 and 1:0.1, weighing 10mmol of copper acetate and holmium acetate according to the corresponding molar ratio, weighing 5 parts of 0.002g of polyvinylpyrrolidone, respectively adding 1L of deionized ultrapure water, preparing mixed solutions of Cu ions and Ho ions with different doping ratios, and synthesizing pure CuS nanoparticles and CuS: Ho nanoparticles under the condition of circulating water at 30 ℃. The synthesized samples were subjected to energy dispersive X-ray spectroscopy and the resulting doping contents were 0 at.%, 0.11 at.%, 0.19 at.%, 0.31 at.%, 0.40 at.%, and 0.54 at.%, respectively. To synthesisHo nanoparticles are subjected to an X-ray diffraction spectrum test, and a diffraction peak is obviously shifted along with the increase of doping concentration, so that Ho is successfully doped into the CuS nanoparticles, and the result is shown in figure 2. The resultant samples were tested for hysteresis at room temperature to give better hysteresis, the results are shown in fig. 3. The saturation magnetization of the doping contents 0 at.%, 0.11 at.%, 0.19 at.%, 0.31 at.%, 0.40 at.% and 0.54 at.% was 0.00229emu g-1、0.00248emu g-1、0.00268emu g-1、0.00322emu g-1、0.00443emu g-1And 0.00301emu g-1The saturation magnetization value tends to increase first and then decrease. The sample passes a magnetic test, and the Ho doped CuS nanoparticle diluted magnetic semiconductor is proved to retain stronger ferromagnetism compared with pure CuS nanoparticles. Successfully prepares the Ho-doped CuS nano-particle diluted magnetic semiconductor with room-temperature ferromagnetism.
Claims (4)
1. An aerosol condensation chemical deposition synthesis CuS: the method for manufacturing the Ho diluted magnetic semiconductor comprises the following steps:
(1) the sodium sulfide solution and the hydrochloric acid solution generate chemical reaction to provide sufficient hydrogen sulfide gas;
(2) generating mixed aerosol of Cu ions and Ho ions by the mixed solution of Cu ions and Ho ions under the action of an ultrasonic atomizer;
(3) and (3) reacting hydrogen sulfide gas with the mixed gas fog of the Cu ions and the Ho ions in the environment of circulating water under the driving of a gas driving device, and precipitating in a collecting bottle to obtain the Ho-doped CuS-based diluted magnetic semiconductor nanoparticles CuS: Ho.
2. The aerosol condensation cvd synthetic CuS of claim 1: the method for preparing the Ho diluted magnetic semiconductor is characterized in that the sodium sulfide solution in the step (1) is Na2S·9H2The mass ratio of O to water is 1: 2-4; the hydrochloric acid solution is prepared by mixing HCl and water according to a mass ratio of 1: 1-3 of a prepared solution; na (Na)2The molar ratio of S to HCl is 1: 2.
3. the aerosol condensation cvd synthetic CuS of claim 1: the method for preparing the Ho diluted magnetic semiconductor is characterized in that the molar ratio of the Cu ions to the Ho ions in the mixed solution of the Cu ions and the Ho ions in the step (2) is 1: 0.001 to 0.15; the mixed aerosol of Cu ions and Ho ions is mixed aerosol of copper acetate and holmium acetate.
4. The aerosol condensation cvd synthetic CuS of claim 1: the method for the Ho diluted magnetic semiconductor is characterized in that the environmental temperature of the circulating water in the step (3) is 20-40 ℃; the gas driving device is an air pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210285059.4A CN114715930A (en) | 2022-03-22 | 2022-03-22 | Synthesizing CuS by aerosol condensation and chemical deposition: method for manufacturing Ho diluted magnetic semiconductor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210285059.4A CN114715930A (en) | 2022-03-22 | 2022-03-22 | Synthesizing CuS by aerosol condensation and chemical deposition: method for manufacturing Ho diluted magnetic semiconductor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114715930A true CN114715930A (en) | 2022-07-08 |
Family
ID=82239646
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210285059.4A Pending CN114715930A (en) | 2022-03-22 | 2022-03-22 | Synthesizing CuS by aerosol condensation and chemical deposition: method for manufacturing Ho diluted magnetic semiconductor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114715930A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3865744A (en) * | 1971-04-02 | 1975-02-11 | Alan James Parker | Method of producing copper and composition therefor |
| CN103449506A (en) * | 2013-09-05 | 2013-12-18 | 吉林大学 | Preparation method of yttrium-doped cadmium sulfide diluted magnetic semiconductor nanomaterial |
| CN104200947A (en) * | 2014-08-11 | 2014-12-10 | 华南理工大学 | Nano-structure-controllable diluted magnetic semiconductor material and preparation method and device thereof |
| CN111269014A (en) * | 2020-01-20 | 2020-06-12 | 昆明理工大学 | Cu-S-based composite thermoelectric material and preparation method thereof |
| CN113136579A (en) * | 2021-04-26 | 2021-07-20 | 王水平 | Method and device for recovering copper from waste circuit board etching solution and regenerating etching solution |
-
2022
- 2022-03-22 CN CN202210285059.4A patent/CN114715930A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3865744A (en) * | 1971-04-02 | 1975-02-11 | Alan James Parker | Method of producing copper and composition therefor |
| CN103449506A (en) * | 2013-09-05 | 2013-12-18 | 吉林大学 | Preparation method of yttrium-doped cadmium sulfide diluted magnetic semiconductor nanomaterial |
| CN104200947A (en) * | 2014-08-11 | 2014-12-10 | 华南理工大学 | Nano-structure-controllable diluted magnetic semiconductor material and preparation method and device thereof |
| CN111269014A (en) * | 2020-01-20 | 2020-06-12 | 昆明理工大学 | Cu-S-based composite thermoelectric material and preparation method thereof |
| CN113136579A (en) * | 2021-04-26 | 2021-07-20 | 王水平 | Method and device for recovering copper from waste circuit board etching solution and regenerating etching solution |
Non-Patent Citations (1)
| Title |
|---|
| QI ZHAO等: "Magnetic and optical properties of two-dimensional SnS2 nanosheets doped with Ho ions", 《APPLIED SURFACE SCIENCE》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wu et al. | Controlled synthesis of magnetic iron oxides@ SnO 2 quasi-hollow core–shell heterostructures: formation mechanism, and enhanced photocatalytic activity | |
| CN106583750B (en) | A method of preparing boron nitride nanosheet/metal nano particle composite material | |
| Tang et al. | Room temperature ferromagnetism in hydrothermally grown Ni and Cu co-doped ZnO nanorods | |
| Cui et al. | Formation of FeMoO 4 hollow microspheres via a chemical conversion-induced Ostwald ripening process | |
| Soofivand et al. | Simple and facile synthesis of Ag2CrO4 and Ag2Cr2O7 micro/nanostructures using a silver precursor | |
| Baranowska-Korczyc et al. | Facile synthesis of core/shell ZnO/ZnS nanofibers by electrospinning and gas-phase sulfidation for biosensor applications | |
| Guo et al. | Complex doping chemistry owing to Mn incorporation in nanocrystalline anatase TiO 2 powders | |
| Hao et al. | Novel magnetic behavior of Mn-doped ZnO hierarchical hollow spheres | |
| CN114715930A (en) | Synthesizing CuS by aerosol condensation and chemical deposition: method for manufacturing Ho diluted magnetic semiconductor | |
| CN101774628B (en) | Preparation method of water-soluble metal sulfide semiconductor nanoparticle | |
| CN105314672A (en) | Method for preparing cobalt-doped zinc oxide nanorods through sol-gel | |
| Sedighi et al. | Fabricant and characterization of SrWO4 and novel silver-doped SrWO4 using co-precipitation method: Their photocatalytic performances for methyl orange degradation | |
| WO2020073926A1 (en) | Preparation method for quantum dots | |
| Zhang et al. | Fluctuant magnetism in metal oxide nanocrystals capped with surfactants | |
| Li et al. | Hyperbranched hierarchical nanoarchitectures of ZnOHF: synthesis, characterization, growth mechanism and their gas sensing property | |
| CN111807333B (en) | Preparation method of three-dimensional cuprous selenide nanocrystalline superlattice | |
| CN102154705B (en) | Preparation method of indium antimonide nanocrystal | |
| Mozafari et al. | Effects of heat treatment on physical, microstructural and optical characteristics of PbS luminescent nanocrystals | |
| CN111777093B (en) | Preparation method of short rod-shaped nano copper sulfide material | |
| CN100393920C (en) | Method for preparing single crystal ZnO based rare magnetism semi-conducting nanometer rod blended by magnetic metal ion | |
| CN107720711A (en) | The more thorn-like magnetic telluride nickel nano wires of functional gold and preparation, application | |
| Vladut et al. | Thermal investigations of the Sn–Zn–O gels obtained by sol–gel method | |
| CN110015691B (en) | Method for preparing nano-scale barium molybdate particles | |
| CN102097206A (en) | Low temperature growth method for wurtzite zinc sulfide base diluted magnetic semiconductor nanorod | |
| CN106243583A (en) | Amorphous carbon/CNT Kynoar high-dielectric composite material is modified on surface |
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 | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20220708 |