CN103373741A - Method for preparing copper, zinc, tin and sulphur powder - Google Patents
Method for preparing copper, zinc, tin and sulphur powder Download PDFInfo
- Publication number
- CN103373741A CN103373741A CN 201210118674 CN201210118674A CN103373741A CN 103373741 A CN103373741 A CN 103373741A CN 201210118674 CN201210118674 CN 201210118674 CN 201210118674 A CN201210118674 A CN 201210118674A CN 103373741 A CN103373741 A CN 103373741A
- Authority
- CN
- China
- Prior art keywords
- powder
- zinc
- tin
- copper
- sulphur powder
- 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
Abstract
The invention relates to a method for preparing copper, zinc, tin and sulphur powder, and belongs to the technical field of photovoltaic materials. The method is characterized by comprising the following steps of: uniformly mixing cuprous sulfide, zinc sulfide, tin powder and sulphur powder; hermetically heating the powder under inert protective atmosphere; and after cooling the sample obtained, taking out and grinding the sample to obtain the copper, zinc, tin and sulphur powder. The method for preparing copper, zinc, tin and sulphur powder provided by the invention further has the characteristics of low demand on equipment, simple technical flow, cheap raw materials, low heat treatment temperature, adaptability to large scale industrialized production and the like. The copper, zinc, tin and sulphur powder prepared can be pressed to blocks or target materials in various specifications and has a huge application prospect in the field of scientific research and production of solar batteries.
Description
Technical field
The invention belongs to the photovoltaic material technical field, relate to a kind of preparation method of copper-zinc-tin-sulfur powder body material.
Background technology
Copper-zinc-tin-sulfur is the quaternary compound that is made of the higher element of abundance in the earth's crust, to have replaced the phosphide element that abundance is lower in the copper-indium-galliun-selenium and gallium element with zinc element and tin element, its energy gap is about 1.5eV, very approaching with the best energy gap of semiconductor solar cell absorption layer, uptake factor can reach 10
4Cm
-1, do not contain poisonous composition, so be the optimal candidate material of instead of copper indium gallium Se solar cell absorption layer.It is environmentally friendly and cheap, has broad application prospects.
At present, the main method of preparation copper-zinc-tin-sulfur quaternary compound has magnetron sputtering method, pulsed laser deposition, metal refining presoma again through sulfuration and solvent-thermal method.Magnetron sputtering method, pulsed laser deposition, metal refining presoma are again through sulfuration, and these method complex process, the stoichiometric ratio of product are difficult to control, but also need to use the hydrogen sulfide of severe toxicity.Solvent-thermal method is expensive, and organic solvent is difficult to remove, and has hindered the raising of thin-film solar cells cost performance.Therefore, propose new can be mass-produced, with low cost, environmental friendliness and nontoxic copper-zinc-tin-sulfur material preparation method are highly significant.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of copper-zinc-tin-sulfur powder body material, be characterized in that device requirement is low, technical process is simple, starting material are cheap, thermal treatment temp is low, be fit to large-scale commercial production etc., and finished product is powder, can be pressed into easily bulk or the target of all size.
A kind of method for preparing the copper-zinc-tin-sulfur powder provided by the present invention may further comprise the steps:
1. cuprous sulfide powder, zinc sulphide powder, glass putty and sulphur powder are mixed;
2. the powder that mixes is heated at the inert protective atmosphere lower seal;
3. after waiting the cooling of gained sample, take out grinding and obtain the copper-zinc-tin-sulfur powder.
The purity of described cuprous sulfide powder, zinc sulphide powder, glass putty and sulphur powder is 3N～6N.
The mol ratio of described cuprous sulfide powder, zinc sulphide powder, glass putty and sulphur powder is: (1～1.1): (1～1.1): (1～1.1): (2.0～2.6).
Described mixing step is that craft or mechanical stirring are 10～120 minutes under air atmosphere or under the inert gas atmosphere.
Described heated sealed is, is incubated 1～12 hour after being heated to 450 ℃～1200 ℃ with the temperature rise rate of 1～8 ℃ of per minute.
Compared with prior art; the present invention's employing solid state reaction under protection of inert gas prepares the copper-zinc-tin-sulfur powder; avoided prior art equipment or raw material costliness, complex process, be not easy to scale operation, needed to use the shortcomings such as poisonous hydrogen sulfide, device requirement is low, technical process is simple, starting material are cheap, thermal treatment temp is low, be fit to the advantage such as large-scale commercial production.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the copper-zinc-tin-sulfur powder of embodiment 1 preparation;
Fig. 2 is the X ray diffracting spectrum of the copper-zinc-tin-sulfur powder of embodiment 2 preparations;
Fig. 3 is the X ray diffracting spectrum of the copper-zinc-tin-sulfur powder of embodiment 3 preparations;
Embodiment
Embodiment 1
With cuprous sulfide powder (4N), zinc sulphide powder (4N), glass putty (4N) and sulphur powder (5N) 1: 1: 1 in molar ratio: 2.2 mixed (hand lapping is 30 minutes in mortar, makes it to mix).Put into silica tube, pass into nitrogen, be heated to 450 ℃ with the temperature rise rate of 2 ℃ of per minutes after insulation 3 hours, wait the cooling of gained sample after, take out to grind and obtain the copper-zinc-tin-sulfur powder.The X-ray diffractogram of material such as Fig. 1.
Embodiment 2
With cuprous sulfide powder (4N), zinc sulphide powder (4N), glass putty (4N) and sulphur powder (5N) 1: 1: 1 in molar ratio: 2 mixed (hand lapping is 10 minutes in mortar, makes it to mix).Put into silica tube, pass into high-purity argon gas, be heated to 550 ℃ with the temperature rise rate of 4 ℃ of per minutes after insulation 6 hours, wait the cooling of gained sample after, take out to grind and obtain the copper-zinc-tin-sulfur powder.The X-ray diffractogram of material such as Fig. 2.
Embodiment 3
With cuprous sulfide powder (4N), zinc sulphide powder (4N), glass putty (4N) and sulphur powder (5N) 1: 1: 1 in molar ratio: 2.4 mixed (hand lapping is 10 minutes in mortar, makes it to mix).Put into silica tube, pass into nitrogen, be heated to 500 ℃ with the temperature rise rate of 3 ℃ of per minutes after insulation 12 hours, wait the cooling of gained sample after, take out to grind and obtain the copper-zinc-tin-sulfur powder.The X-ray diffractogram of material such as Fig. 3.
Claims (5)
1. a method for preparing the copper-zinc-tin-sulfur powder is characterized in that, may further comprise the steps:
1. cuprous sulfide powder, zinc sulphide powder, glass putty and sulphur powder are mixed;
2. the powder that mixes is heated at the inert protective atmosphere lower seal;
3. after waiting the cooling of gained sample, take out grinding and obtain the copper-zinc-tin-sulfur powder.
2. the preparation method of the copper-zinc-tin-sulfur powder described in according to claim 1 is characterized in that the purity of described cuprous sulfide powder, zinc sulphide powder, glass putty and sulphur powder is 3N～6N.
According to claim 1 with the preparation method of the copper-zinc-tin-sulfur powder described in 2, it is characterized in that the mol ratio of described cuprous sulfide powder, zinc sulphide powder, glass putty and sulphur powder is: (1～1.1): (1～1.1): (1～1.1): (2.2～2.6).
4. the preparation method of the copper-zinc-tin-sulfur powder described in according to claim 1 is characterized in that, describedly is mixed under air atmosphere or craft or mechanical stirring 10～120 minutes under the inert gas atmosphere.
5. the preparation method of the copper-zinc-tin-sulfur powder described in according to claim 1 is characterized in that, described heated sealed is incubated 1～12 hour for the temperature rise rate with 1～8 ℃ of per minute after being heated to 450 ℃～1200 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210118674 CN103373741A (en) | 2012-04-13 | 2012-04-13 | Method for preparing copper, zinc, tin and sulphur powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210118674 CN103373741A (en) | 2012-04-13 | 2012-04-13 | Method for preparing copper, zinc, tin and sulphur powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103373741A true CN103373741A (en) | 2013-10-30 |
Family
ID=49459639
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210118674 Pending CN103373741A (en) | 2012-04-13 | 2012-04-13 | Method for preparing copper, zinc, tin and sulphur powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103373741A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104538499A (en) * | 2014-12-30 | 2015-04-22 | 湖南省华京粉体材料有限公司 | Method for preparing solar film material copper zinc tin sulfide powder |
| CN105016376A (en) * | 2014-04-21 | 2015-11-04 | 渤海大学 | Preparation method of zinc sulfide twin nanobelt |
| CN111924874A (en) * | 2020-08-17 | 2020-11-13 | 华北理工大学 | Preparation method of copper-zinc-tin-based powder |
-
2012
- 2012-04-13 CN CN 201210118674 patent/CN103373741A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105016376A (en) * | 2014-04-21 | 2015-11-04 | 渤海大学 | Preparation method of zinc sulfide twin nanobelt |
| CN105016376B (en) * | 2014-04-21 | 2016-08-24 | 渤海大学 | The preparation method of zinc sulphide twin nanobelt |
| CN104538499A (en) * | 2014-12-30 | 2015-04-22 | 湖南省华京粉体材料有限公司 | Method for preparing solar film material copper zinc tin sulfide powder |
| CN104538499B (en) * | 2014-12-30 | 2016-09-14 | 湖南省华京粉体材料有限公司 | Solar energy film material copper-zinc-tin-sulfur raw powder's production technology |
| CN111924874A (en) * | 2020-08-17 | 2020-11-13 | 华北理工大学 | Preparation method of copper-zinc-tin-based powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102194989B (en) | Method for preparing thermoelectric material of ternary diamond structure | |
| CN100511729C (en) | Process for preparing Cu*ZnSnS* semiconductor thin film solar cell | |
| Zhou et al. | Preparation and characterization of Cu2ZnSnS4 microparticles via a facile solution route | |
| CN102372302A (en) | Copper-zinc-tin-sulfur or copper-zinc-tin-selenium target for absorbed layer of thin-film solar battery, preparation method for target and application of target | |
| CN103572089B (en) | A kind of preparation method of Cu-Im-Ga-Se quaternary semiconductor alloy | |
| CN101723336A (en) | Preparation method of Cu2ZnSnSxSe4-x nanocrystal | |
| CN101101939A (en) | A technology for making absorption layer of Cu2ZnSnS4 film solar battery | |
| CN102306685B (en) | Low-cost preparation method of CZTS (Cu2ZnSnS4) thin film solar battery absorption layer | |
| CN103373741A (en) | Method for preparing copper, zinc, tin and sulphur powder | |
| CN104445379B (en) | The solid sintering technology of gradient temperature prepares cesium triiodide tin | |
| CN102390856B (en) | Method for preparing high-stability gamma-phase nanometer lanthanum sulfide powder in low temperature | |
| CN109802011B (en) | Method for preparing copper-zinc-tin-sulfur film through sulfurization annealing in air | |
| CN103633165B (en) | Yellow copper structure Intermediate Gray solar battery obsorbing layer material and preparation method thereof | |
| CN103950909A (en) | Preparation method of zinc phosphide | |
| CN102610670A (en) | Near-infrared transparent conducting film and method for producing same | |
| CN104404456A (en) | Preparation method of CZTS (copper-zinc-tin-sulfur) quaternary target | |
| CN103681934B (en) | Preparation method for copper-zinc-stannum-sulfur powder, or copper-zinc-stannum-selenium powder or copper-zinc-stannum-sulfur-selenium powder | |
| CN105821376A (en) | Preparation method for copper-zinc-tin sulfide target | |
| CN104726825A (en) | Preparation method of P-type transparent and conductive cobalt oxide metal nano-composite film | |
| CN102344166B (en) | Preparation method for Cu2ZnSnS4 solar energy absorption layer material | |
| CN103290249A (en) | Method and apparatus for producing thermoelectric conversion material, and sputtering target production method | |
| CN103449436A (en) | Method for preparing negative-expansion manganese-carbon compound (Mn3SnC) with perovskite-like structure | |
| CN103626495B (en) | Preparation method for CIGS target material through pressureless sintering | |
| CN103949634B (en) | A kind of preparation method of rare-earth sulfide | |
| CN104538499B (en) | Solar energy film material copper-zinc-tin-sulfur raw powder's production technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131030 |