CN102897722B - A kind of solvothermal synthesis method of α-In2Se3 nano curd - Google Patents
A kind of solvothermal synthesis method of α-In2Se3 nano curd Download PDFInfo
- Publication number
- CN102897722B CN102897722B CN201210312074.XA CN201210312074A CN102897722B CN 102897722 B CN102897722 B CN 102897722B CN 201210312074 A CN201210312074 A CN 201210312074A CN 102897722 B CN102897722 B CN 102897722B
- Authority
- CN
- China
- Prior art keywords
- nano
- reactor
- curd
- solvothermal synthesis
- oleic acid
- 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.)
- Expired - Fee Related
Links
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000004729 solvothermal method Methods 0.000 title claims abstract 8
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 20
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 17
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 15
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000005642 Oleic acid Substances 0.000 claims abstract description 15
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims abstract description 15
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 239000011669 selenium Substances 0.000 claims abstract description 11
- 229960005070 ascorbic acid Drugs 0.000 claims abstract 5
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract 5
- 239000011668 ascorbic acid Substances 0.000 claims abstract 5
- 239000003638 chemical reducing agent Substances 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims abstract 2
- 239000002135 nanosheet Substances 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 11
- 239000002086 nanomaterial Substances 0.000 abstract description 8
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 238000005119 centrifugation Methods 0.000 abstract description 3
- 238000004458 analytical method Methods 0.000 abstract description 2
- AKUCEXGLFUSJCD-UHFFFAOYSA-N indium(3+);selenium(2-) Chemical compound [Se-2].[Se-2].[Se-2].[In+3].[In+3] AKUCEXGLFUSJCD-UHFFFAOYSA-N 0.000 description 27
- 239000000463 material Substances 0.000 description 9
- 238000007789 sealing Methods 0.000 description 7
- 238000001291 vacuum drying Methods 0.000 description 7
- 239000012071 phase Substances 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005755 formation reaction Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003346 selenoethers Chemical class 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 241000272525 Anas platyrhynchos Species 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- GGYFMLJDMAMTAB-UHFFFAOYSA-N selanylidenelead Chemical compound [Pb]=[Se] GGYFMLJDMAMTAB-UHFFFAOYSA-N 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Landscapes
- Physical Or Chemical Processes And Apparatus (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
本发明属于环境友好型纳米材料技术领域，涉及纳米材料的制备方法，尤其是涉及一种α-In2Se3纳米花球溶剂热合成方法。本发明提供了一种α-In2Se3纳米花球溶剂热合成方法，是以油酸为溶剂，抗坏血酸为还原剂，将硝酸铟、硒粉在反应釜中进行溶剂热合成反应，然后用无水乙醇洗涤，并离心分离干燥后制得。从生长机理上推断，该方法能适用于其他硒金属化合物纳米材料的制备。本发明的制备方法简单、成本低廉、可控性强、产物结晶性好、绿色环保；从对其低倍扫描电镜图（SEM）、高倍扫描电镜图（SEM）以及透射电镜图（TEM）的分析，制得的α-In2Se3纳米花球直径在1~2微米，是由厚度为13~15纳米的纳米片所组成的。
The invention belongs to the technical field of environment-friendly nano materials, and relates to a preparation method of nano materials, in particular to a solvothermal synthesis method of α-In 2 Se 3 nano curds. The invention provides a method for solvothermal synthesis of α-In 2 Se 3 nano curds, using oleic acid as a solvent and ascorbic acid as a reducing agent, carrying out solvothermal synthesis of indium nitrate and selenium powder in a reactor, and then using Washed with absolute ethanol, and obtained after centrifugation and drying. Inferred from the growth mechanism, this method can be applied to the preparation of other selenium metal compound nanomaterials. The preparation method of the present invention is simple, low in cost, strong in controllability, good in product crystallinity, and environmentally friendly; from its low-power scanning electron microscope (SEM), high-power scanning electron microscope (SEM) and transmission electron microscope (TEM) According to the analysis, the diameter of the prepared α-In 2 Se 3 nano curd is 1-2 microns, and it is composed of nano-sheets with a thickness of 13-15 nanometers.
Description
Technical field
The invention belongs to environmentally friendly technical field of nano material, relate to the preparation method of nano material, especially relate to a kind of α-In
2se
3nanometer bouquet solvent process for thermosynthesizing.
Background technology
Selenide metal semiconductor nano material is due to its unique physicals and chemical property, can be widely used in energy, medicine, the important field of sensor simultaneously and caused more and more people's attention.In numerous selenide, indium selenide is as important III-VI main group compound, the laminate structure being formed by Se-In-In-Se key, strong covalent linkage and faint Van der Waals force make the performances such as its anisotropy, electricity, optics and magnetics, catalysis and air-sensitive with height between layers, thereby make indium selenide on the devices such as phase converter, polarized radiation, photovoltaic solar cells, lithium cell, fluorescent apparatus, dielectric medium, field-effect transistor, have application widely.Meanwhile, indium selenide can also be prepared three different urmaterie as CuInSe as structural unit
2, AgInSe
2with quaternary substance C u (In, Ga) Se
2, be widely used on photoelectric material device and these materials are also good photoelectric materials.In addition, indium selenide is the photoelectric material that a kind of direct band gap is 1.7eV, due to photoelectronic anisotropy, within the scope of visible light wave, has very high uptake factor, can effectively convert solar energy into electrical energy, and be a kind of photovoltaic energy material of excellence., compare with the photoelectric material that cadmium selenide is good with lead selenide etc., indium selenide also has hypotoxicity and environment friendly in low band-gap nano material meanwhile.
Although the research for indium selenide never rested, synthesize indium selenide not a duck soup single, pure phase.In building-up process, the difficulty that indium selenide runs into mainly comes from the limitation of indium selenide phasor.Indium selenide has InSe, In
2se
3, In
4se
3and In
6se
7four kinds of complicated array configurations, these several different moietys are often present in indium selenide within a certain scope simultaneously.Only In in addition
2se
3this composition form, it becomes phase system just complicated especially, for example, In
2se
3there is α, beta, gamma, five kinds of crystal formations of δ and κ, and between crystal formation and crystal formation, be easy to mutually change, so will expect the In of single composition and single crystal form
2se
3, especially difficulty seems.
So far, relevant synthetic In
2se
3method report out successively, but most synthetic method is confined to traditional methods such as gas-phase synthesizing method, organic chemistry steam decomposition method and electrochemical deposition method.And the instrument of the high-end precision of above-mentioned synthetic method needs, temperature of reaction is at 400 ~ 1000 ℃, and energy consumption is large, and can produce poisonous gas, and human body and environment are caused to certain harm, and the sample that these methods obtain also has the feature such as heterogeneity and low yield.Therefore find simple, cheap, green, a controlled method, synthetic InSe nanometer structure is necessary and challenging.
Hydrothermal method has the advantages such as the product purity that equipment is simple, raw material easily obtains, obtain is high, good uniformity, chemical constitution precise control and is subject to many researchers' favor.Hydrothermal method is in special closed reactor (autoclave), take the fluid such as water or organic solvent as reactive material, by reaction system being heated to critical temperature (or approaching critical temperature), create a high-temperature high-voltage reaction environment, impel reaction to carry out in liquid phase or gas phase, make originally indissoluble or insoluble material solvent recrystallization, then through separating and thermal treatment obtains a kind of effective ways of product.Hydrothermal method has the following advantages: (1) is warm (generally between 120 ~ 220 ℃) liquid phase control in adopting, and energy consumption is relatively low, and suitability is wide, both can be used for the nanoparticle preparation that size is less, also can obtain larger-size monocrystalline; (2) raw material is relatively inexpensive is easy to get, and reaction is carried out in the quick convection current of liquid phase, productive rate is high, thing mutually evenly, high, the well-crystallized of purity, and shape size is controlled; (3), in water-heat process, can, by regulating temperature of reaction, pressure, time, pH value, precursor and tensio-active agent etc., reach the object of effective control reaction and growth characteristics; (4) reaction is carried out in the container of sealing, is applicable to the building-up reactions in poisonous system, can reduce environmental pollution.
But rarely have report but utilize hydrothermal method to prepare indium selenide, only have 2011, the people such as poplar have gone out γ-In with ethanol as solvent Hydrothermal Synthesis at 220 ℃
2se
3microballoon, the diameter of this ball is at 2-4 micron.Because the size of material has a great impact for character, so synthetic undersized indium selenide is necessary.In addition, up to now, also not for the controlled α-In of pattern
2se
3the report that solvent thermal is synthetic.Therefore, solvent-applied process for thermosynthesizing, synthetic single component, the controlled α-In of pattern
2se
3imperative.
Summary of the invention
For the defect existing in prior art and deficiency, the invention provides a kind of α-In
2se
3the solvent process for thermosynthesizing of nanometer bouquet, is take oleic acid as solvent, and xitix is reductive agent, by indium nitrate, selenium powder solvent thermal building-up reactions in reactor, then uses absolute ethanol washing, and centrifugation makes after dry.Infer from growth mechanism, the method can be applicable to the preparation of other selenium metallic compound nano materials.
A kind of α-In
2se
3nanometer bouquet solvent process for thermosynthesizing, described solvent thermal building-up reactions comprises the steps:
Steps A, take a certain amount of indium nitrate, selenium powder, xitix and mix in reactor, wherein, the mol ratio of described indium nitrate, selenium powder, xitix is 3:1:1 ~ 2;
Step B, add oleic acid stir 30min, the volume of wherein said oleic acid accounts for 60% ~ 80% of reactor;
Step C, reactor is reacted to 12h ~ 24h at 190 ℃ ~ 220 ℃, be then cooled to room temperature.
In a preferred embodiment of the present invention, the mol ratio of described indium nitrate, selenium powder, xitix is 3:1:1;
The volume of described oleic acid accounts for 80% of reactor;
Described reactor reacts 24h at 200 ℃.
Obtained product is used to absolute ethanol washing at ambient temperature, and centrifugation gets its lower sediment, after vacuum-drying, obtain the powder of black.
α-the In being prepared from according to above-mentioned solvent process for thermosynthesizing
2se
3nanometer bouquet, from the analysis to its low power scanning electron microscope (SEM) photograph (SEM), high power scanning electron microscope (SEM) photograph (SEM) and transmission electron microscope picture (TEM), described α-In
2se
3nano flower spherical diameter is at 1 ~ 2 micron, and the nanometer sheet that is 13 ~ 15nm by thickness forms.
beneficial effect
Preparation method of the present invention is simple, with low cost, controllability is strong, product good crystallinity, environmental protection.
Accompanying drawing explanation
The X-ray diffraction analysis figure (XRD) of flower ball-shaped indium selenide prepared by Fig. 1;
The low power scanning electron microscope (SEM) photograph (SEM) of flower ball-shaped indium selenide prepared by Fig. 2;
The high power scanning electron microscope (SEM) photograph (SEM) of flower ball-shaped indium selenide prepared by Fig. 3;
Flower ball-shaped indium selenide transmission electron microscope picture (TEM) prepared by Fig. 4.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
Embodiment 1:
A kind of synthetic α-In
2se
3the solvent-thermal method of nanometer bouquet, concrete steps are as follows:
(1) take respectively 0.2292g indium nitrate with electronic balance, 0.0158g selenium powder, 0.0352g xitix, 30ml oleic acid is in 50ml reactor, and magneton stirs 30 minutes;
(2) reactor sealing is put into 200 ℃ of baking oven constant temperature 24 hours, then naturally cool to room temperature, use absolute ethanol washing 8 times, the dry black flower ball-shaped indium selenide that obtains in 60 ℃ of vacuum drying ovens.
Fig. 1 is the XRD figure of the flower ball-shaped indium selenide of preparation, as can be seen from the figure the peak type of the material that obtains and the card 34-1313 of JCPDS (JCPDS) match, and in this peak, there is no the peak of other impurity, illustrate that obtain is the α-In of pure phase
2se
3.
Fig. 2 is the low power SEM figure of the flower ball-shaped indium selenide of preparation, and as can be seen from the figure, bouquet dispersiveness is relatively good, and surface ratio is more coarse, and diameter is greatly about 1-2 micron.
Fig. 3 is the high power SEM figure of the flower ball-shaped indium selenide of preparation, and as can be seen from the figure, bouquet is made up of for the nanometer sheet of 15 nanometers left and right thickness.
Fig. 4 is the flower ball-shaped indium selenide TEM figure of preparation, understands furtherly what bouquet was made up of sheet.
Embodiment 2:
A kind of synthetic α-In
2se
3the solvent-thermal method of nanometer bouquet, concrete steps are as follows:
(1) take respectively 0.2292g indium nitrate with electronic balance, 0.0158g selenium powder, 0.0704g xitix, 30ml oleic acid is in 50ml reactor, and magneton stirs 30 minutes;
(2) reactor sealing is put into 200 ℃ of baking oven constant temperature 24 hours, then naturally cool to room temperature, use absolute ethanol washing 8 times, the dry black flower ball-shaped indium selenide that obtains in 60 ℃ of vacuum drying ovens.
Embodiment 3:
A kind of synthetic α-In
2se
3the solvent-thermal method of nanometer bouquet, concrete steps are as follows:
(1) take respectively 0.2292g indium nitrate with electronic balance, 0.0158g selenium powder, 0.0352g xitix, 40ml oleic acid is in 50ml reactor, and magneton stirs 30 minutes;
(2) reactor sealing is put into 200 ℃ of baking oven constant temperature 24 hours, then naturally cool to room temperature, use absolute ethanol washing 8 times, the dry black flower ball-shaped indium selenide that obtains in 60 ℃ of vacuum drying ovens.
Embodiment 4:
A kind of synthetic α-In
2se
3the solvent-thermal method of nanometer bouquet, concrete steps are as follows:
(1) take respectively 0.2292g indium nitrate with electronic balance, 0.0158g selenium powder, 0.0352g xitix, 40ml oleic acid is in 50ml reactor, and magneton stirs 30 minutes;
(2) reactor sealing is put into 190 ℃ of baking oven constant temperature 24 hours, then naturally cool to room temperature, use absolute ethanol washing 8 times, the dry black flower ball-shaped indium selenide that obtains in 60 ℃ of vacuum drying ovens.
Embodiment 5:
A kind of synthetic α-In
2se
3the solvent-thermal method of nanometer bouquet, concrete steps are as follows:
(1) take respectively 0.2292g indium nitrate with electronic balance, 0.0158g selenium powder, 0.0352g xitix, 40ml oleic acid is in 50ml reactor, and magneton stirs 30 minutes;
(2) reactor sealing is put into 220 ℃ of baking oven constant temperature 24 hours, then naturally cool to room temperature, use absolute ethanol washing 8 times, the dry black flower ball-shaped indium selenide that obtains in 60 ℃ of vacuum drying ovens.
Embodiment 6:
A kind of synthetic α-In
2se
3the solvent-thermal method of nanometer bouquet, concrete steps are as follows:
(1) take respectively 0.2292g indium nitrate with electronic balance, 0.0158g selenium powder, 0.0352g xitix, 40ml oleic acid is in 50ml reactor, and magneton stirs 30 minutes;
(2) reactor sealing is put into 200 ℃ of baking oven constant temperature 12 hours, then naturally cool to room temperature, use absolute ethanol washing 8 times, the dry black flower ball-shaped indium selenide that obtains in 60 ℃ of vacuum drying ovens.
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210312074.XA CN102897722B (en) | 2012-08-29 | 2012-08-29 | A kind of solvothermal synthesis method of α-In2Se3 nano curd |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210312074.XA CN102897722B (en) | 2012-08-29 | 2012-08-29 | A kind of solvothermal synthesis method of α-In2Se3 nano curd |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102897722A CN102897722A (en) | 2013-01-30 |
| CN102897722B true CN102897722B (en) | 2014-05-28 |
Family
ID=47570260
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210312074.XA Expired - Fee Related CN102897722B (en) | 2012-08-29 | 2012-08-29 | A kind of solvothermal synthesis method of α-In2Se3 nano curd |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102897722B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103273079B (en) * | 2013-05-10 | 2015-07-22 | 安徽医科大学 | Gold nanoflower preparing method and application of gold nanoflowers |
| CN105776154A (en) * | 2016-05-10 | 2016-07-20 | 电子科技大学 | Preparation method of tungsten diselenide nanosheet |
| CN111960390A (en) * | 2020-08-06 | 2020-11-20 | 西安近代化学研究所 | Preparation method of monodisperse gamma-indium selenide nano particles |
| CN111841583B (en) * | 2020-08-12 | 2023-04-18 | 西安近代化学研究所 | Preparation method of indium selenide/titanium dioxide nanosheet composite material |
| CN114988371B (en) * | 2022-06-10 | 2023-06-13 | 南昌航空大学 | A size-controllable solvothermally synthesized indium zinc selenide nanosheet and its preparation method and application |
-
2012
- 2012-08-29 CN CN201210312074.XA patent/CN102897722B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN102897722A (en) | 2013-01-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102583517B (en) | Preparation method of strontium titanate nanometer piece | |
| CN105669045B (en) | A kind of Cu2ZnSnS4The preparation method and applications of/graphene composite semiconductor films | |
| CN102897722B (en) | A kind of solvothermal synthesis method of α-In2Se3 nano curd | |
| CN103213956B (en) | A kind of preparation method of CuInSe2 and CuIn1-xGaxSe2 nanoparticles with chalcopyrite structure | |
| CN103058265B (en) | Preparation method of mesoporous nano flaky zinc oxide powder with high specific surface area | |
| CN113087016A (en) | Preparation method of rod-shaped bismuth sulfide/reduced graphene oxide composite material | |
| CN103819099A (en) | Method for preparing graphene structure-like copper-indium-sulfur nanosheet array membrane | |
| CN102557116B (en) | A kind of method for preparing hollow solar energy absorbing material CuInS2 | |
| CN103872186A (en) | FeS2 thin film and its preparation method | |
| CN104291278B (en) | A kind of method of hydrazine hydrate auxiliary polyhydric alcohol based sols synthesis β phase indium selenide flaky nanocrystalline | |
| KR20090110090A (en) | Method for producing indium selenide nano compound using ultrasonic wave and compound semiconductor solar cell comprising same | |
| CN108117052B (en) | Two-dimensional mesoporous (GaN)1-x(ZnO)x solid solution nanomaterial and preparation method thereof | |
| CN102249199A (en) | Microwave-assisted solvothermal synthesis method of I-III-VI semiconductor material nano-powder | |
| CN102786038B (en) | Hydro-thermal synthesis method of cubic phase InSe nano sheet | |
| CN102815676B (en) | Polyhydric alcohol solution chemical synthesis method for preparing non-stoichiometric Cu-In-Se series compound nano-crystalline | |
| CN102899713B (en) | Hydrothermal synthesis of dumbbell-like Sb2Te3-Te heterostructures | |
| CN102509648A (en) | Preparation method for Ga-doped ZnO nanometer material | |
| CN102923763A (en) | Method for synthesizing copper indium diselenide nanosheet through ion exchange method | |
| CN106881118B (en) | A kind of method of ion-exchange synthesis heterojunction photocatalyst | |
| CN104085915A (en) | Preparation method for hexagonal CdS nanosheet with high-energy crystal face (001) exposed | |
| CN101327915A (en) | Preparation of Sb2Te3 thermoelectric compound | |
| CN105692680B (en) | A kind of nano composite material of hierarchy zinc oxide@graphenes and preparation method thereof | |
| CN110272065B (en) | Method for preparing graphene-coated zinc oxide nanocomposite material by using blue algae | |
| CN108408788B (en) | Preparation method of octahedral poly-crystal with directionally attached and grown pyrite nanosheets | |
| CN101734712A (en) | Method for preparing high-quality copper indium sulfide by employing single-source molecular precursor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140528 Termination date: 20160829 |