CN111559756A - Light absorption enhanced spherical CuS submicron material and preparation method thereof - Google Patents
Light absorption enhanced spherical CuS submicron material and preparation method thereof Download PDFInfo
- Publication number
- CN111559756A CN111559756A CN202010501898.6A CN202010501898A CN111559756A CN 111559756 A CN111559756 A CN 111559756A CN 202010501898 A CN202010501898 A CN 202010501898A CN 111559756 A CN111559756 A CN 111559756A
- Authority
- CN
- China
- Prior art keywords
- cus
- spherical
- submicron
- deionized water
- submicron material
- 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
- C01G3/12—Sulfides
-
- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
Abstract
The invention discloses a light absorption enhanced spherical CuS submicron material and a preparation method thereof. The method comprises the steps of adding copper sulfate and sodium thiosulfate into deionized water, fully stirring, adding polyvinylpyrrolidone (PVP) and continuously stirring to completely dissolve the copper sulfate and the sodium thiosulfate, transferring the fully dissolved mixed solution into a reaction kettle with a polytetrafluoroethylene lining, heating and reacting for 8-12 hours at the constant temperature of 120-160 ℃, washing and centrifuging reaction products, and drying obtained dark brown precipitates to obtain the spherical CuS submicron material with enhanced light absorption. The method is simple to operate and suitable for industrial production, and the obtained spherical CuS submicron material is high in crystallinity, large in specific surface area and good in sunlight absorption performance, and can be used for efficient absorption and photothermal conversion utilization of solar energy.
Description
Technical Field
The invention belongs to the field of micro-nano functional material science, and particularly relates to a spherical CuS submicron material with enhanced light absorption and a preparation method thereof.
Background
Copper sulfide (CuS) is a p-type semiconductor material with a photonic band gap of about 1.2 to 2.0eV, and thus has good light absorption properties in both visible and near-infrared regions. The nano or micron CuS can show special optical, electrical and thermal properties due to the unique microstructure and size effect, and can be widely applied to the fields of light absorption, photo-thermal conversion, photocatalysis, solar cells and the like, so that the synthesis and performance research of the CuS micro-nano material also becomes one of the focuses of domestic and foreign material scientists.
The hydrothermal synthesis method is a synthesis method in which reactants are subjected to a chemical reaction in a fluid atmosphere such as an aqueous solution or steam under a high-temperature and high-pressure environment provided in a specific closed container (high-pressure reaction vessel); the nano particles prepared by the hydrothermal synthesis method have high purity and good crystal form, the whole preparation process is relatively simple, and the consumption cost is relatively low, so that the CuS nano material prepared by the hydrothermal synthesis method is greatly favored by researchers. Fang et al (J Fang, et al, Solar energy Materials and Solar Cells, 2018, 185: 456-; however, no surfactant is added during the reaction process, and the concentration used is relatively high, which leads to a certain agglomeration phenomenon of the prepared material, which may reduce the absorption capacity of the prepared material to sunlight. Therefore, the preparation method needs to be improved to prepare the spherical CuS micro-nano material with large specific surface area and uniform structure distribution for enhancing the sunlight absorption performance of the spherical CuS micro-nano material. Therefore, the method for preparing the spherical CuS micro-nano material which is more optimized, convenient to operate and low in energy consumption is very significant.
Disclosure of Invention
The invention aims to provide a spherical CuS submicron material with enhanced light absorption and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
a light absorption enhanced spherical CuS submicron material and a preparation method thereof are characterized by comprising the following steps:
(1) respectively weighing copper sulfate and sodium thiosulfate in a beaker, adding deionized water, fully stirring, then adding a certain amount of PVP, and continuously stirring to completely dissolve the PVP and the PVP;
(2) transferring the fully dissolved solution into a 100ml polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction at a certain temperature and for a certain time;
(3) and taking out the obtained precipitate, carrying out centrifugal separation, repeatedly washing and centrifuging by using deionized water, and then drying in a constant-temperature drying oven for 4-8 hours to obtain the spherical CuS submicron material.
Preferably, in the step (1), the molar weight ratio of the copper sulfate to the sodium thiosulfate is 1: 1, the molar volume ratio of copper sulfate to deionized water is 5 mmol: 60 mL.
Preferably, in the step (1), the mass-to-volume ratio of the added PVP to the deionized water is (0.25-0.75) g: 60 mL.
Preferably, in the step (2), the reaction temperature is 120-160 ℃, and the reaction time is 8-12 h.
Preferably, in step (3), the washing and centrifuging are: washing the reaction product with deionized water, centrifuging, and repeating the washing and centrifuging operations for 3-5 times.
Preferably, in the step (3), the drying temperature of the precipitate is 60-90 ℃.
Compared with the prior art, the spherical CuS submicron material with large specific surface area and uniform structure distribution is prepared by a simple hydrothermal reaction method, is used for improving the absorption performance of sunlight, provides a simple and feasible method for efficiently absorbing and utilizing solar energy, and has the following advantages:
(1) the preparation process of the spherical CuS material is simple, different amounts of submicron structural materials can be obtained by changing the addition amount of reactants and the size of a reaction container, and the method is suitable for industrial production.
(2) The crystallinity of the prepared CuS submicron material can be higher by controlling the time and the temperature of the hydrothermal reaction, and the material can have a larger specific surface area by changing the addition amount of the surfactant, so that the absorption performance of the material on sunlight is enhanced, and a greater possibility is provided for efficiently absorbing and converting and utilizing solar energy.
Drawings
FIG. 1 is an X-ray diffraction pattern of a CuS submicron material prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope picture of a CuS submicron material prepared in example 2 of the present invention;
FIG. 3 is a graph of the sum of N and CuS submicron materials prepared in example 2 of the present invention2Adsorption-desorption curves;
fig. 4 is a uv-vis-nir absorption spectrum curve of the CuS submicron material prepared in examples 1 and 2 of the present invention.
Detailed Description
The technical solution of the present invention is fully described in further detail by the following specific examples. The following examples are further illustrative of the present invention and do not limit the scope of the present invention.
Example 1
(1) Respectively weighing 1.25g of copper sulfate and 1.24g of sodium thiosulfate in a beaker, adding 60ml of deionized water, fully stirring, then adding 0.5g of PVP, and continuing stirring to completely dissolve the copper sulfate and the sodium thiosulfate;
(2) transferring the fully dissolved solution into a reaction kettle with a 100ml polytetrafluoroethylene lining, setting the temperature of a drying oven to be 120 ℃ for hydrothermal reaction, and setting the reaction time to be 12 h;
(3) after the reaction is finished, the precipitate is centrifugally washed by deionized water, is repeatedly centrifugally washed for 3 times, and is dried for 4 hours in a drying oven at the temperature of 90 ℃ to obtain a final product.
Referring to the attached figure 1, the X-ray diffraction spectrum of the CuS submicron material prepared by the method described in example 1, in the X-ray diffraction spectrum, the peak positions of the spectrum line in the X-ray diffraction spectrum correspond to all diffraction crystal faces of the JCPDS standard spectrum (06-0464) one by one, which indicates that the prepared sample is a CuS product of a hexagonal system, the diffraction peak is sharp and high, and the sample has high crystallinity.
Example 2
(1) Respectively weighing 1.25g of copper sulfate and 1.24g of sodium thiosulfate in a beaker, adding 60ml of deionized water, fully stirring, then adding 0.5g of PVP, and continuing stirring to completely dissolve the copper sulfate and the sodium thiosulfate;
(2) transferring the fully dissolved solution into a reaction kettle with a 100ml polytetrafluoroethylene lining, setting the temperature of a drying oven to be 160 ℃ for hydrothermal reaction, and setting the reaction time to be 12 h;
(3) after the reaction is finished, the precipitate is centrifugally washed by deionized water, is repeatedly centrifugally washed for 3 times, and is dried for 4 hours in a drying oven at the temperature of 90 ℃ to obtain a final product.
Referring to the attached figure 2, the SEM picture of the CuS submicron material prepared by the method described in example 2 shows that the obtained material has a spherical structure shape, the size of the spherical structure is about 1 μm, and the size distribution is relatively uniform.
N of CuS submicron Material produced as described in example 2, with reference to FIG. 32The specific surface area of the obtained spherical structure material is 34.93m according to an adsorption-desorption curve2The specific surface area of the CuS material is 20.90m compared with that of the CuS material prepared without adding a surfactant PVP2The specific surface area of the material is increased remarkably, and reaches 67.1%, and the larger specific surface area can provide more active sites for absorbing solar energy, so that the light absorption and utilization efficiency is improved.
Referring to fig. 4, uv-vis-nir absorption spectra of CuS submicron materials prepared as described in examples 1 and 2. It can be seen from the figure that the prepared material has good light absorption performance over the whole test wavelength band compared to deionized water, and the light absorption performance is enhanced as the reaction temperature is increased. At this time, the weighted solar energy absorption fractions of the materials obtained by integral calculation are 85.1% and 93.3%, respectively, and compared with the weighted solar energy absorption fractions of the CuS material prepared without adding the surfactant PVP, which are 77.8% and 82.4%, respectively, it can be known that the light absorption performance of the prepared CuS material is further enhanced after adding the surfactant PVP.
Example 3
(1) Respectively weighing 1.25g of copper sulfate and 1.24g of sodium thiosulfate in a beaker, adding 60ml of deionized water, fully stirring, then adding 0.25g of PVP, and continuing stirring to completely dissolve the copper sulfate and the sodium thiosulfate;
(2) transferring the fully dissolved solution into a reaction kettle with a 100ml polytetrafluoroethylene lining, setting the temperature of a drying oven to be 120 ℃ for hydrothermal reaction, and setting the reaction time to be 12 h;
(3) after the reaction is finished, the precipitate is centrifugally washed by deionized water, is repeatedly centrifugally washed for 3 times, and is dried for 4 hours in a drying oven at the temperature of 90 ℃ to obtain a final product.
The CuS submicron material obtained as described in example 3 was tested by XRD as a hexagonal CuS product and observed by SEM as a spherical submicron material.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (5)
1. A light absorption enhanced spherical CuS submicron material and a preparation method thereof are characterized in that the method comprises the following steps:
respectively weighing copper sulfate and sodium thiosulfate in a beaker, adding deionized water, fully stirring, then adding a certain amount of PVP, and continuously stirring to completely dissolve the PVP and the PVP;
transferring the fully dissolved solution into a reaction kettle with a 100ml polytetrafluoroethylene lining, setting the temperature of a drying oven to be 120-160 ℃ for hydrothermal reaction, and setting the reaction time to be 8-12 h;
(3) and taking out the obtained precipitate, carrying out centrifugal separation, repeatedly washing and centrifuging by using deionized water, and then drying in a constant-temperature drying oven for 4-8 hours to obtain the spherical CuS submicron material.
2. The method for preparing CuS submicron materials with spherical structures according to claim 1, wherein in the step (1), the molar weight ratio of copper sulfate to sodium thiosulfate is 1: 1, the molar volume ratio of copper sulfate to deionized water is 5 mmol: 60 mL.
3. The method for preparing the CuS submicron material with the spherical structure according to claim 1, wherein in the step (1), the mass-to-volume ratio of PVP to deionized water is (0.25-0.75) g: 60 mL.
4. The method for preparing the spherical-structured CuS submicron material according to claim 1, wherein in the step (3), the washing and centrifuging are: washing the reaction product with deionized water, centrifuging, and repeating the washing and centrifuging operations for 3-5 times;
in the step (3), the drying temperature of the precipitate is 60-90 ℃.
5. The spherical CuS submicron material with enhanced light absorption obtained by the preparation method of any one of claims 1 to 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010501898.6A CN111559756A (en) | 2020-06-04 | 2020-06-04 | Light absorption enhanced spherical CuS submicron material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010501898.6A CN111559756A (en) | 2020-06-04 | 2020-06-04 | Light absorption enhanced spherical CuS submicron material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111559756A true CN111559756A (en) | 2020-08-21 |
Family
ID=72073780
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010501898.6A Pending CN111559756A (en) | 2020-06-04 | 2020-06-04 | Light absorption enhanced spherical CuS submicron material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111559756A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113415819A (en) * | 2021-08-09 | 2021-09-21 | 陕西科技大学 | Cable-shaped multilevel-structure CuS micro-nano material and preparation method thereof |
| CN113428890A (en) * | 2021-08-09 | 2021-09-24 | 陕西科技大学 | Multilevel-structure CuS hollow sphere, preparation method and application thereof |
| CN114195182A (en) * | 2022-01-24 | 2022-03-18 | 长春大学 | Preparation method of soil additive component containing copper metal compound |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008056511A (en) * | 2006-08-30 | 2008-03-13 | Nagoya Institute Of Technology | Method for producing metal sulfide nanoparticle and photoelectric conversion element |
| CN101905900A (en) * | 2009-06-05 | 2010-12-08 | 河南大学 | Preparation method of hollow copper sulfide microspheres or microtubes |
| CN102502773A (en) * | 2011-11-23 | 2012-06-20 | 陕西科技大学 | Preparation method of annular self assembled copper sulfide hollow spheres |
| CN105016374A (en) * | 2015-08-14 | 2015-11-04 | 天津城建大学 | Method for preparing CuS micro-spheres of hierarchic structures |
-
2020
- 2020-06-04 CN CN202010501898.6A patent/CN111559756A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008056511A (en) * | 2006-08-30 | 2008-03-13 | Nagoya Institute Of Technology | Method for producing metal sulfide nanoparticle and photoelectric conversion element |
| CN101905900A (en) * | 2009-06-05 | 2010-12-08 | 河南大学 | Preparation method of hollow copper sulfide microspheres or microtubes |
| CN102502773A (en) * | 2011-11-23 | 2012-06-20 | 陕西科技大学 | Preparation method of annular self assembled copper sulfide hollow spheres |
| CN105016374A (en) * | 2015-08-14 | 2015-11-04 | 天津城建大学 | Method for preparing CuS micro-spheres of hierarchic structures |
Non-Patent Citations (3)
| Title |
|---|
| FANG, JF ET AL.: "Hydrothermal synthesis of nanostructured CuS for broadband efficient optical absorption and high-performance photo-thermal conversion", 《SOLAR ENERGY MATERIALS AND SOLAR CELLS》 * |
| ZHANG, YC ET AL.: "Shape-controlled synthesis of CuS nanocrystallites via a facile hydrothermal route", 《SOLID STATE COMMUNICATIONS》 * |
| 刘洋: "硫化铜及硫化亚铜作为锂离子电池负极材料的研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅱ辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113415819A (en) * | 2021-08-09 | 2021-09-21 | 陕西科技大学 | Cable-shaped multilevel-structure CuS micro-nano material and preparation method thereof |
| CN113428890A (en) * | 2021-08-09 | 2021-09-24 | 陕西科技大学 | Multilevel-structure CuS hollow sphere, preparation method and application thereof |
| CN113428890B (en) * | 2021-08-09 | 2022-08-09 | 陕西科技大学 | CuS hollow sphere with secondary structure, preparation method and application thereof |
| CN114195182A (en) * | 2022-01-24 | 2022-03-18 | 长春大学 | Preparation method of soil additive component containing copper metal compound |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111559756A (en) | Light absorption enhanced spherical CuS submicron material and preparation method thereof | |
| CN104821240B (en) | SnS2/MoS2 composite material one-step hydrothermal synthesizing method and application thereof | |
| CN105417507B (en) | A kind of preparation method and products obtained therefrom of azotized carbon nano particle | |
| CN102897724B (en) | Tin selenide nano-flowers and preparation method thereof | |
| CN102698728B (en) | Titanium dioxide nanotube/ graphene composite material and preparation method thereof | |
| CN110124692A (en) | A kind of preparation method of the zinc-cadmium sulfide solid solution of different-shape | |
| CN109999874A (en) | A kind of richness nitrogen azotized carbon nano pipe photochemical catalyst and preparation method and application | |
| CN101214932A (en) | Method for preparing nanometer tin selenide | |
| CN110605126A (en) | Cavity BiOCl @ CeO2Preparation method and application of nano composite material | |
| CN102935360A (en) | Method for preparing ZnWO4 nanorod photocatalysis material | |
| CN101759226A (en) | Binary sulfide CuXZn1-XS particle with efflorescent structure and preparation method thereof | |
| CN109748322A (en) | The synthetic method and application of α-MnS nanoparticle and α-MnS/rGO composite material | |
| CN108579773B (en) | A kind of perovskite-based composite nano materials and preparation method and purposes | |
| CN110713203A (en) | CuS/carbon black composite photothermal conversion material and preparation method thereof | |
| CN107265495A (en) | Non-template method prepares zinc sulphide microballoon | |
| CN114308073A (en) | Preparation method and application of composite catalyst | |
| CN107352521B (en) | A kind of threadiness phosphatization tin compound and preparation method thereof | |
| CN106430286A (en) | Method for preparing ZnO/g-C3N4 composite of core-shell structure | |
| CN106964388B (en) | A kind of wolframic acid stannous adulterates the preparation method of two-dimentional graphite phase carbon nitride composite photo-catalyst | |
| CN100534908C (en) | Process for preparing In2O3 nano-wire | |
| CN109761264A (en) | A kind of method of quick preparation water solubility CIS quantum dot/redox graphene composite material | |
| CN116393155A (en) | Carbocyclic doped g-C 3 N 4 Preparation method of heterojunction in basal plane and application of heterojunction in photo-reforming cellulose | |
| CN103145183A (en) | Three-dimensional TiO2 reticular nano-material, as well as preparation method and application thereof | |
| CN110563036A (en) | bismuth oxide nano material rich in oxygen vacancy and preparation method thereof | |
| CN109772241A (en) | A kind of nanoscale lignin-base microballoon and preparation method thereof |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200821 |
|
| RJ01 | Rejection of invention patent application after publication |