CN102249289A - Method for preparing spiauterite ZnS fine nanorod with solvothermal method - Google Patents
Method for preparing spiauterite ZnS fine nanorod with solvothermal method Download PDFInfo
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- CN102249289A CN102249289A CN2011101399937A CN201110139993A CN102249289A CN 102249289 A CN102249289 A CN 102249289A CN 2011101399937 A CN2011101399937 A CN 2011101399937A CN 201110139993 A CN201110139993 A CN 201110139993A CN 102249289 A CN102249289 A CN 102249289A
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- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000002073 nanorod Substances 0.000 title abstract 4
- 238000004729 solvothermal method Methods 0.000 title abstract 3
- 229910052984 zinc sulfide Inorganic materials 0.000 claims abstract description 76
- 239000002904 solvent Substances 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract 2
- KGWDUNBJIMUFAP-KVVVOXFISA-N Ethanolamine Oleate Chemical compound NCCO.CCCCCCCC\C=C/CCCCCCCC(O)=O KGWDUNBJIMUFAP-KVVVOXFISA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 206010013786 Dry skin Diseases 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 11
- 230000001186 cumulative effect Effects 0.000 claims description 11
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 230000003252 repetitive effect Effects 0.000 claims description 11
- 238000005201 scrubbing Methods 0.000 claims description 11
- 239000011701 zinc Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000005864 Sulphur Substances 0.000 claims description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- PODWXQQNRWNDGD-UHFFFAOYSA-L sodium thiosulfate pentahydrate Chemical group O.O.O.O.O.[Na+].[Na+].[O-]S([S-])(=O)=O PODWXQQNRWNDGD-UHFFFAOYSA-L 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims 1
- -1 polytetrafluoroethylene Polymers 0.000 abstract description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 abstract 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 2
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000003760 magnetic stirring Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 36
- 239000002086 nanomaterial Substances 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 2
- 241000237502 Ostreidae Species 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 2
- 239000002127 nanobelt Substances 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 235000020636 oyster Nutrition 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 208000027697 autoimmune lymphoproliferative syndrome due to CTLA4 haploinsuffiency Diseases 0.000 description 1
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- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
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- 230000007704 transition Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种溶剂热制备纤锌矿ZnS细纳米棒的方法，是通过以下工艺过程实现的：将分析纯的S源放入聚四氟乙烯内衬，加入乙醇胺溶剂使溶液体积占聚四氟乙烯内衬总体积的80％。磁搅拌数分钟，再加入分析纯的Zn源，磁搅拌均匀后密封反应釜，置于180℃烘箱中反应24小时，反应完成后清洗得到产物。本发明成功地用简单溶剂热方法，在乙醇胺体系中一步合成具有纤锌矿结构的ZnS细纳米棒。本发明的特点是：方法简单，容易操作；重复性好，产物的结构和形貌可控性好；成本低，利于纤锌矿ZnS细纳米棒的商业化。The invention discloses a method for preparing wurtzite ZnS fine nanorods by solvothermal method, which is realized through the following process: put the analytically pure S source into the polytetrafluoroethylene lining, add ethanolamine solvent to make the solution volume account for polytetrafluoroethylene 80% of the total volume of the tetrafluoroethylene lining. Stir magnetically for several minutes, then add an analytically pure Zn source, seal the reaction vessel after magnetic stirring evenly, place it in an oven at 180°C for 24 hours, and wash to obtain the product after the reaction is completed. The invention successfully uses a simple solvothermal method to synthesize ZnS fine nanorods with a wurtzite structure in one step in an ethanolamine system. The invention is characterized in that the method is simple and easy to operate; the repeatability is good, the structure and shape of the product are well controllable; the cost is low, and it is beneficial to the commercialization of wurtzite ZnS fine nanorods.
Description
Technical field
The invention belongs to the preparation field of nano material, be specifically related to utilize the solvent thermal technology to prepare the method for the thin nanometer rod of wurtzite ZnS.
Background technology
ZnS is as a kind of important wide bandgap semiconductor materials, have excellent light, electricity, chemical property, in photoluminescence, solar cell, infrared window, UV, visible light photodiode and laser apparatus, cathode-ray fluorescent material and flat-panel monitor phosphor material, important application is arranged.ZnS has two kinds of things of zink sulphide and wurtzite mutually, and the former is the ambient-temp-stable phase, and the latter is the metastable phase of high-temperature stable, and the transition temperature from the zink sulphide to the wurtzite is at 1020 ℃.In general, the spectral response curve of wurtzite ZnS is better than zink sulphide.Wurtzite ZnS can be synthetic by the High Temperature Gas phase method, and most of low temperature liquid phase method synthetic are that zink sulphide ZnS is nanocrystalline.Because preparation technology is simple, product is high-purity, ultra-fine, particle diameter is even, is subjected to the investigator and more and more pays close attention to based on liquid phase synthetic chemical process.
It is synthetic that some investigators have reported that wurtzite ZnS nanostructure can be passed through the auxiliary solvent thermal process of quadrol (en), because the en molecule can form lamellar compound ZnSen with Zn and S easily
0.5, and then the thing of having modulated product is mutually and pattern.But need that in most cases organic-inorganic composite body is carried out post annealed and solvent heat treatment and remove the en group to form wurtzite ZnS.Li Yadong research group is by 350-800 ℃ of following vacuum heat treatment ZnSen
0.5Precursor has synthesized wurtzite-type ZnS nanometer thrombocyte, consults the 869th page of Inorg.Chem. the 41st volume; Human dithiocarbonic anhydride later stage solvent heat treatment such as Zhou ZnSen
0.5Precursor has synthesized wurtzite-type ZnS nanometer sheet, consults the 1761st page of Cryst.Growth Des. the 5th volume.
Recently, one dimension ZnS nanostructure (as nanotube, nano wire, nanometer rod and nano belt) is because its unique optics, electrochemistry, and mechanics and thermal property get more and more people's extensive concerning.Adopt the ZnS one dimension Nano structure of easy low temperature liquid phase compounding wurtzite structure to be still full of challenges.Chai etc. use hydrazine hydrate to prepare wurtzite ZnS nano wire bundle as solvent, consult the 12658th page of J.Phys.Chem.C the 111st volume; Yet the solvent thermal reaction that with the hydrazine hydrate is solvent is very violent, the danger coefficient height; Be not suitable for scale operation.Owing to use mixing solutions can form the pattern novel nano materials, adopt binary or polynary mixed solution system to prepare the extensive interest that the ZnS nano material causes people.Research groups such as Chen etc. and Li use en and H
2The O mixed solvent has prepared wurtzite ZnS nanometer rod, consults the 255602nd page of Inorg.Chem. the 42nd the 3100th page of volume and Nanotechnology the 18th volume; Wang etc. have reported use en and ethylene glycol (EG) mixed solvent compounding wurtzite ZnS nanometer rod, and point out solvent volume than and the concentration in sulphur source for the product thing mutually and the control of pattern play an important role, consult Journal of nanoscience and nanotechnology the 10th and roll up the 3131st page.
Thanomin (EA) can be as the structure directing agent of solvent in the solvent thermal reaction and structure amine metallic sulfide 1-dimention nano crystalline substance as the monodentate amine with sequestering action.Compare en, EA is easier to be broken away from from product, does not need to carry out post-processed.Xiong and its co-worker have reported and have adopted zinc acetate and L-halfcystine to prepare wurtzite ZnS hierarchical organization as precursor in the binary solvent of water and EA, it is worthy of note that when they make solvent with straight alcohol amine what obtain is the nano belt reticulated structure; Only at 200 and 240 ℃, V
Water: V
EAJust can obtain nanometer rod at=3: 2 o'clock, and consult the 2728th page of Adv.Funct.Mater. the 17th volume.In addition, mixed solvent is than single solvent system complexity, and the ratio of each solvent is very big to the thing phase and the pattern influence of final product, operates very inconvenient.The controlledly synthesis of semiconductor nano material is very important to scientific research and technology application, and the present invention is the thin nanometer rod of control compounding wurtzite ZnS in pure EA system.
Summary of the invention
The present invention successfully uses the simple solvent by the use of thermal means first, under the condition of gentleness, is the thin nanometer rod of ZnS of solvent one-step synthesis wurtzite structure with the thanomin.
The present invention realizes by following technological process:
Polytetrafluoroethyllining lining is put in the analytically pure S of 2mmol source, added the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure Zn of 1mmol source again, continues magnetic and is stirred to even back sealed reactor, places 180 ℃ of baking ovens reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain product.
The thin nanometer rod of the ZnS that the present invention prepares is wurtzite ZnS, and its XRD composes as Fig. 1, shown in Figure 4, the pattern under its transmission electron microscope such as Fig. 2, Fig. 5, shown in Figure 6, and high-resolution-ration transmission electric-lens figure is as shown in Figure 3.The present invention is solvent with the thanomin, use different Zn sources and S source all to obtain the thin nanometer rod of wurtzite ZnS, and pattern is even, good crystallinity.Simultaneously, the inventive method is simple, is easy to promote, and is suitable for large-scale industrial production.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of embodiment 1 product.
Fig. 2 is transmission electron microscope (TEM) picture of embodiment 1 product.
Fig. 3 is high resolution transmission electron microscopy (HRTEM) picture of embodiment 1 product.
Fig. 4 is the XRD figure sheet of embodiment 2 products.
Fig. 5 is the TEM picture of embodiment 2 products.
Fig. 6 is the TEM picture of embodiment 3 products.
Embodiment
Embodiment 1
With the analytically pure Sulfothiorine (Na of 2mmol
2S
2O
35H
2O) put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure zinc oxide of 1mmol (ZnO) again, continues magnetic and is stirred to even back sealed reactor, places 180 ℃ of baking ovens reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain the oyster white product.As shown in Figure 1, XRD result shows that product is the ZnS of wurtzite structure, as Fig. 1; TEM result shows that product is made up of the nanometer rod of diameter between 5-7nm, as Fig. 2.
Embodiment 2
With the analytically pure Na of 2mmol
2S
2O
35H
2O puts into polytetrafluoroethyllining lining, adds the thanomin solvent and makes liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure zinc acetate of 1mmol (Zn (CH again
3COO)
22H
2O), continue magnetic and be stirred to even back sealed reactor, place 180 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain the oyster white product.XRD result shows that product is the ZnS of wurtzite structure, as Fig. 4; TEM result shows that product is made up of a large amount of nanometer rod, as shown in Figure 5.
Embodiment 3
With the analytically pure Na of 2mmol
2S
2O
35H
2O puts into polytetrafluoroethyllining lining, adds the thanomin solvent and makes liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure zinc chloride (ZnCl of 1mmol again
2), continue magnetic and be stirred to even back sealed reactor, place 180 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain product.TEM result shows that product is made up of a large amount of nanometer rod, as Fig. 6.
Embodiment 4
With analytically pure the thiocarbamide ((NH of 2mmol
2)
2CS) put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure zinc oxide of 1mmol (ZnO) again, continues magnetic and is stirred to even back sealed reactor, places 180 ℃ of baking ovens reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain product.Analyze and show that product is the ZnS nanometer rod of wurtzite structure.
Embodiment 5
With the analytically pure (NH of 2mmol
2)
2CS puts into polytetrafluoroethyllining lining, adds the thanomin solvent and makes liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure Zn (CH of 2mmol again
3COO)
22H
2O continues magnetic and is stirred to even back sealed reactor, places 180 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain product.Analysis is shown as the ZnS nanometer rod of wurtzite structure.
Embodiment 6
With the analytically pure (NH of 2mmol
2)
2CS puts into polytetrafluoroethyllining lining, adds the thanomin solvent and makes liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure ZnCl of 1mmol again
2, continue magnetic and be stirred to even back sealed reactor, place 180 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain product.Analysis is shown as the ZnS nanometer rod of wurtzite structure.
Embodiment 7
The analytically pure sulphur powder of 1mmol (S) is put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure ZnO of 1mmol again, continues magnetic and is stirred to even back sealed reactor, places 180 ℃ of baking ovens reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain product.Analysis is shown as the ZnS nanometer rod of wurtzite structure.
Embodiment 8
The analytically pure S powder of 1mmol is put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure Zn (CH of 2mmol again
3COO)
22H
2O continues magnetic and is stirred to even back sealed reactor, places 180 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain product.Analysis is shown as the ZnS nanometer rod of wurtzite structure.
Embodiment 9
The analytically pure S powder of 1mmol is put into polytetrafluoroethyllining lining, add the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume.Magnetic stirred for several minute adds the analytically pure ZnCl of 2mmol again
2, continue magnetic and be stirred to even back sealed reactor, place 180 ℃ of baking oven reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain product.Analysis is shown as the ZnS nanometer rod of wurtzite structure.
Claims (6)
1. a solvent thermal prepares the method for the thin nanometer rod of wurtzite ZnS, it is characterized in that realizing: polytetrafluoroethyllining lining is put in the analytically pure S of 2mmol source, added the thanomin solvent and make liquor capacity account for 80% of polytetrafluoroethyllining lining cumulative volume by following technological process.Magnetic stirred for several minute adds the analytically pure Zn of 1mmol source again, continues magnetic and is stirred to even back sealed reactor, places 180 ℃ of baking ovens reactions 24 hours.Naturally cool to room temperature, collect cooled product, with deionized water and dehydrated alcohol repetitive scrubbing, 60 ℃ of dryings of vacuum obtain the thin nanometer rod of wurtzite ZnS.
2. a kind of solvent thermal as claimed in claim 1 prepares the method for the thin nanometer rod of wurtzite ZnS, it is characterized in that, described solvent is a thanomin.
3. a kind of solvent thermal as claimed in claim 1 prepares the method for the thin nanometer rod of wurtzite ZnS, it is characterized in that described S source is Sulfothiorine (Na
2S
2O
35H
2O), thiocarbamide ((NH
2)
2CS) and sulphur powder (S).
4. a kind of solvent thermal as claimed in claim 1 prepares the method for the thin nanometer rod of wurtzite ZnS, it is characterized in that, described Zn source is zinc oxide (ZnO), zinc acetate (Zn (CH
3COO)
22H
2O) and zinc chloride (ZnCl
2).
5. a kind of solvent thermal as claimed in claim 1 prepares the method for the thin nanometer rod of wurtzite ZnS, it is characterized in that, described S source and Zn source mol ratio are 1: 2, change ratio that can be suitable.
6. a kind of solvent thermal as claimed in claim 1 prepares the method for the thin nanometer rod of wurtzite ZnS, it is characterized in that, described reaction vessel is the tetrafluoroethylene hydrothermal reaction kettle, can expand in the closed container of other high temperature high voltage resistants.
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| CN103613117A (en) * | 2013-12-02 | 2014-03-05 | 镇江市高等专科学校 | Method for regulating and controlling zinc sulfide nanoparticle morphology by regulating proportion of mixed solvent |
| CN103613117B (en) * | 2013-12-02 | 2016-01-06 | 镇江市高等专科学校 | A kind of method adjusting the ratio regulation and control zinc sulfide nano pattern of mixed solvent |
| CN103771494A (en) * | 2014-01-26 | 2014-05-07 | 王新娟 | Liquid-phase preparation method for manganese-doped zinc sulfide microspheres |
| CN103991850A (en) * | 2014-05-14 | 2014-08-20 | 新疆大学 | Preparation method of S-doped ZnTe |
| CN103991850B (en) * | 2014-05-14 | 2016-10-26 | 新疆大学 | A kind of preparation method of the ZnTe of the S that adulterates |
| CN106517308A (en) * | 2015-09-15 | 2017-03-22 | 宿迁学院 | Preparation method of ZnS hollow microspheres |
| CN105776319A (en) * | 2016-02-03 | 2016-07-20 | 中国科学院新疆理化技术研究所 | Preparation method of zinc sulfide granules of hierarchical structure for rapidly detecting explosive atmosphere |
| CN106430288A (en) * | 2016-11-30 | 2017-02-22 | 江苏大学 | A kind of preparation method of g-C3N4/ZnS nanocomposite material |
| CN107456980A (en) * | 2017-07-07 | 2017-12-12 | 国家纳米科学中心 | A kind of ZnS/ZnO core shell structures and its preparation method and application |
| CN110203962A (en) * | 2019-04-24 | 2019-09-06 | 金华莱顿新能源科技有限公司 | A kind of ZnSP nano-bar material and preparation method thereof for supercapacitor |
| CN110203962B (en) * | 2019-04-24 | 2021-08-03 | 金华莱顿新能源科技有限公司 | ZnSP nanorod material for super capacitor and preparation method thereof |
| CN114835155A (en) * | 2022-04-22 | 2022-08-02 | 哈尔滨理工大学 | Preparation method of ZnS nano material |
| CN114835155B (en) * | 2022-04-22 | 2022-12-09 | 哈尔滨理工大学 | Preparation method of ZnS nano material |
| CN117756097A (en) * | 2023-11-30 | 2024-03-26 | 厦门大学 | Nitrogen-sulfur double-doped and zinc-loaded ultrathin carbon-wall carbon sphere and preparation method and application thereof |
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