CN109437297B - Preparation method of sodium thioantimonate micro-nano multilevel structure material - Google Patents
Preparation method of sodium thioantimonate micro-nano multilevel structure material Download PDFInfo
- Publication number
- CN109437297B CN109437297B CN201910012825.8A CN201910012825A CN109437297B CN 109437297 B CN109437297 B CN 109437297B CN 201910012825 A CN201910012825 A CN 201910012825A CN 109437297 B CN109437297 B CN 109437297B
- Authority
- CN
- China
- Prior art keywords
- micro
- structure material
- nano
- multilevel structure
- sodium
- 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.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
- C01G30/002—Compounds containing, besides antimony, 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
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- 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
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of a sodium thioantimonate micro-nano multilevel structure material, belonging to the field of preparation of nanomaterials. The method has the advantages that water is used as a solvent, so that the safety hazard caused by thermal evaporation of an organic solvent and the influence on the purity of a sample are avoided, the safety is high, reaction raw materials are easy to obtain, the feasibility is high, the process equipment is simple, the reaction is more fully and uniformly performed by stirring, the method is a process condition which is mild in condition, environment-friendly, simple and low in price, the prepared sodium thioantimonate nano-particles and nano-rod composite multi-level structure material is good in crystallinity, high in purity, strong in crystallinity, uniform in appearance, economical, environment-friendly, high in practicability and good in industrialization prospect.
Description
Technical Field
The invention belongs to the field of nano material preparation, relates to a preparation method of a sodium thioantimonate micro-nano multilevel structure material, and particularly relates to a preparation method of a solid electrolyte precursor of a sodium ion battery.
Background
The ideal solid electrolyte has to have high ionic conductivity, excellent chemical and electrochemical stability and lower synthesis cost, and the S-based solid electrolyte is more popular than the NASICON solid electrolyte due to the higher ionic conductivity.
Na3SbS4NaS in the structure6Distorted tetrahedral structure and NaS6The dodecahedron structures are arranged in a staggered mode and connected in a coplanar mode; na (Na)3SbS4Na element in the structure forms Na of-Na (1) -Na (2) -Na (1) -Na (2) -in a planar channel network structure+A transmission channel in which Na (2) has a preferential vibration direction compared with that of adjacent four Na (1), Sb is less likely to occur, Na (1) is more likely to connect Na (2) sites with Na (1) in the Z-axis direction in the XY plane, and Na (2) has 5% of vacancies in the above transmission channel, which are favorable for Na + transition; in the Z-axis directionTo NaS6Are connected to each other at common edges, therefore Na+Transmission by hopping, Na3SbS4Form Na in+So that the ionic conductivity thereof can reach 10-3S cm-1。
Sodium thioantimonate (Na)3SbS4·9H2O), also known as Schlippe's, is a commercially available precursor salt. Na (Na)3SbS4·9H2The O is mainly used for preparing antimony pentasulfide and cleaning a solvent to separate out metal zinc in the zinc electrolysis process. Due to Sb5+(Soft acid) with Soft base S2-Form strong body between them, so Na3SbS4·9H2In O (Sbs)4)3-The ions are stable in the environment, and the crystal water can be removed at the low-temperature heat treatment temperature to obtain Na3SbS4Sodium ion solid electrolyte.
The nano-structure material (1-100 nm) has a quantum size effect, so that the semiconductor light absorber with the nano-structure forms an adjustable energy band structure due to the quantum size effect, has a large optical absorption coefficient, and can generate a plurality of excitons by one photon; in addition, the special effect of large surfaces of one-dimensional nanomaterials such as nanomaterials, nanotubes, nanoribbons, etc. makes them often exhibit properties different from those exhibited by the material in its bulk state in terms of melting point, magnetic, optical, thermal, electrical conductivity, etc. Thus, multi-level nanostructured Na was prepared3SbS4·9H2O has great application value.
The methods for preparing the nano-materials reported at present mainly comprise a uniform precipitation method [1], a sol-gel method [2] and a solid phase method [3], wherein the product obtained by the uniform precipitation method has relatively weak crystallinity and the size distribution of the product is not uniform; the sol-gel method has long reaction period, and the post-treatment of the obtained product is complicated; the powder particles prepared by the solid phase method have no agglomeration, good filling property, low cost, large yield and simple preparation process, but the powder has large energy consumption, low efficiency and insufficiently fine powder and is easy to mix with impurities.
Disclosure of Invention
In order to overcome the defects of the prior art,the invention aims to provide Na with high purity, strong crystallinity and uniform appearance3SbS4·9H2A preparation method of O micro-nano multilevel structure material.
The present invention provides such Na3SbS4·9H2The preparation method of the O micro-nano multilevel structure material comprises the following steps:
(1) dissolving sodium sulfide in proper amount of solvent to obtain CNa0.6-1.0 mol/L sodium sulfide solution;
(2) adding sublimed sulfur into the sodium sulfide solution obtained in the step (1) according to a preset proportion, and stirring at the temperature of 70-90 ℃ until the sulfur is completely dissolved to obtain a mixed solution;
(3) adding an antimony source into the mixed solution obtained in the step (2) according to a set proportion, and uniformly mixing to obtain a suspension;
(4) transferring the suspension obtained in the step (3) into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 3-15 h at 140-200 ℃, cooling to room temperature, washing and drying the product in sequence to obtain Na3SbS4·9H2O micro-nano multilevel structure material.
Preferably, in the step (1), the solvent is one of deionized water, distilled water or ultrapure water.
Preferably, the molar ratio n isNa：nS1: (1.2-1.8) adding sublimed sulfur into the sodium sulfide solution obtained in the step (1);
the antimony source is Sb2S3Controlling the molar ratio nNa：nSb＝(2.90～3.15)：1。
Preferably, the molar ratio n isNa：nS1: (1.1-1.5) adding sublimed sulfur into the sodium sulfide solution obtained in the step (1);
the antimony source is Sb powder, and the molar ratio n is controlledNa：nSb＝(2.9～3.3)：1。
Preferably, in step (4), the product is washed with absolute ethanol by centrifugation for several times until the centrifugate is clear and clear.
Preferably, in the step (4), the centrifugal product is dried in a vacuum drying oven at the temperature of 60-100 ℃ for 8-12 hours.
Compared with the prior art, the invention has the beneficial technical effects that:
the method adopts a homogeneous hydrothermal method, takes water as a solvent, avoids safety hazard and influence on sample purity caused by thermal evaporation of an organic solvent, has high safety, easily obtained reaction raw materials, strong feasibility and simple process equipment, ensures that the reaction is more sufficient and uniform by stirring, is a process condition with mild condition, environmental protection, simplicity and low cost, and prepares the Na3SbS4·9H2The O nanoparticle and nanorod composite multi-level structure material has the advantages of good crystallinity, high purity, strong crystallinity, uniform appearance, economy, environmental friendliness, strong practicability and good industrialization prospect.
Drawings
FIG. 1 shows Na prepared in example 1 of the present invention3SbS4·9H2XRD pattern of O material.
FIG. 2 shows Na prepared in example 1 of the present invention3SbS4·9H2SEM image of O material.
FIG. 3 is Na prepared in example 2 of the present invention3SbS4·9H2XRD pattern of O material.
FIG. 4 is Na prepared in example 2 of the present invention3SbS4·9H2SEM image of O material.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by those skilled in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
In this example, unless otherwise specified, the chemical reagents used were analytical reagents, all of which were common commercial products or prepared by conventional means, and the equipment used was conventional in the art, and the following are some examples of the inventors in the experiment:
example 1
The invention provides Na3SbS4·9H2The preparation method of the O micro-nano multilevel structure material comprises the following steps:
(1) dissolving sodium sulfide in proper amount of deionized water to obtain CNa0.6mol/L sodium sulfide solution;
(2) in molar ratio of nNa：nS1: 1.3 adding sublimed sulfur into a sodium sulfide solution, and stirring at the temperature of 70 ℃ until the sulfur is completely dissolved to prepare a mixed solution;
(3) in molar ratio of nNa：nSb3.0: 1 general formula Sb2S3Adding the mixture into the mixed solution obtained in the step (2), and uniformly mixing to obtain a suspension;
(4) transferring the suspension into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 3h at 140 ℃, cooling to room temperature, carrying out centrifugal washing on the product for several times by using absolute ethyl alcohol until the centrifugal liquid is transparent and clear, and drying the centrifugal product in a vacuum drying oven at 60 ℃ for 8h to obtain Na3SbS4·9H2O micro-nano multilevel structure material.
FIG. 1 is a diagram showing preparation of Na in example 13SbS4·9H2XRD pattern of O product, from which it can be seen that the product is phase-pure Na3SbS4·9H2O, the crystallinity is better; FIG. 2 is a diagram showing preparation of Na in example 13SbS4·9H2And the SEM atlas of the O product shows that the obtained product is a coexisting structure of nano particles and nano short rods, the particle size of the nano particles is about 50-70 nm, the nano rods grow up by crystallization of the nano particles, the length of the rods is about 3-4 mu m, the diameter of the nano rods is about 70-150 nm, and the surfaces of the nano rods are smooth.
Example 2
The invention provides Na3SbS4·9H2The preparation method of the O micro-nano multilevel structure material comprises the following steps:
(1) dissolving sodium sulfide in proper amount of deionized water to obtain CNa0.6mol/L sodium sulfide solution;
(2) in molar ratio of nNa：nS＝1: 1.4 adding sublimed sulfur into a sodium sulfide solution, and stirring at the temperature of 70 ℃ until the sulfur is completely dissolved to prepare a mixed solution;
(3) in molar ratio of nNa：nSb2.9: 1, adding Sb powder into the mixed solution obtained in the step (2), and uniformly mixing to obtain a suspension;
(4) transferring the suspension into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 3h at 140 ℃, cooling to room temperature, carrying out centrifugal washing on the product for several times by using absolute ethyl alcohol until the centrifugal liquid is transparent and clear, and drying the centrifugal product in a vacuum drying oven at 60 ℃ for 8h to obtain Na3SbS4·9H2O micro-nano multilevel structure material.
FIG. 3 is preparation of Na in example 23SbS4·9H2XRD pattern of O product, from which it can be seen that the product is phase-pure Na3SbS4·9H2O, better crystallinity and more obvious crystal orientation, which shows that Na3SbS4·9H2And the O preferentially grows along a certain crystal plane. FIG. 4 is preparation of Na in example 23SbS4·9H2And (3) an SEM image of the O product, wherein the obtained product is a coexisting structure of nano particles and nano short rods, the particle size of the nano particles is about 40-80 nm, the nano particles are agglomerated, the nano rods grow in a staggered mode, the length of each nano rod is about 500-5 mu m, the diameter of each nano rod is about 70-150 nm, the nano rods are uniform in size and smooth in surface, and the result is consistent with the result of an XRD test.
Example 3
The invention provides Na3SbS4·9H2The preparation method of the O micro-nano multilevel structure material comprises the following steps:
(1) dissolving sodium sulfide in proper amount of deionized water to obtain CNa0.8mol/L sodium sulfide solution;
(2) in molar ratio of nNa：nS1: 1.5 adding sublimed sulfur into a sodium sulfide solution, and stirring at the temperature of 80 ℃ until the sulfur is completely dissolved to prepare a mixed solution;
(3) in molar ratio of nNa：nSb3.0: 1, adding Sb powder into the mixed solution obtained in the step (2), and uniformly mixing to obtain the Sb-containing mixed solutionA suspension;
(4) transferring the suspension into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 10h at 180 ℃, cooling to room temperature, carrying out centrifugal washing on the product for several times by using absolute ethyl alcohol until the centrifugal liquid is transparent and clear, and drying the centrifugal product in a vacuum drying oven at 80 ℃ for 10h to obtain Na3SbS4·9H2O micro-nano multilevel structure material.
Example 4
The invention provides Na3SbS4·9H2The preparation method of the O micro-nano multilevel structure material comprises the following steps:
(1) dissolving sodium sulfide in proper amount of deionized water to obtain CNa1.0mol/L sodium sulfide solution;
(2) in molar ratio of nNa：nS1: 1.1 adding sublimed sulfur into a sodium sulfide solution, and stirring at the temperature of 90 ℃ until the sulfur is completely dissolved to prepare a mixed solution;
(3) in molar ratio of nNa：nSb3.3: 1, adding Sb powder into the mixed solution obtained in the step (2), and uniformly mixing to obtain a suspension;
(4) transferring the suspension into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 15h at 200 ℃, cooling to room temperature, carrying out centrifugal washing on the product for several times by using absolute ethyl alcohol until the centrifugal liquid is transparent and clear, and drying the centrifugal product in a vacuum drying oven at 100 ℃ for 12h to obtain Na3SbS4·9H2O micro-nano multilevel structure material.
Example 5
The invention provides Na3SbS4·9H2The preparation method of the O micro-nano multilevel structure material comprises the following steps:
(1) dissolving sodium sulfide in proper amount of deionized water to obtain CNa0.9mol/L sodium sulfide solution;
(2) in molar ratio of nNa：nS1: 1.2 adding sublimed sulfur into a sodium sulfide solution, and stirring at the temperature of 80 ℃ until the sulfur is completely dissolved to prepare a mixed solution;
(3) in molar ratio of nNa：nSb2.9: 1 general formula Sb2S3Adding the mixture into the mixed solution obtained in the step (2), and uniformly mixing to obtain a suspension;
(4) transferring the suspension into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 9h at 180 ℃, cooling to room temperature, carrying out centrifugal washing on the product for several times by using absolute ethyl alcohol until the centrifugal liquid is transparent and clear, and drying the centrifugal product in a vacuum drying oven at 80 ℃ for 10h to obtain Na3SbS4·9H2O micro-nano multilevel structure material.
Example 6
The invention provides Na3SbS4·9H2The preparation method of the O micro-nano multilevel structure material comprises the following steps:
(1) dissolving sodium sulfide in proper amount of deionized water to obtain CNa1.0mol/L sodium sulfide solution;
(2) in molar ratio of nNa：nS1: 1.8 adding sublimed sulfur into a sodium sulfide solution, and stirring at the temperature of 90 ℃ until the sulfur is completely dissolved to prepare a mixed solution;
(3) in molar ratio of nNa：nSb3.15: 1 general formula Sb2S3Adding the mixture into the mixed solution obtained in the step (2), and uniformly mixing to obtain a suspension;
(4) transferring the suspension into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 15h in a vacuum drying oven at 200 ℃, cooling to room temperature, carrying out centrifugal washing on the product for several times by using absolute ethyl alcohol until the centrifugal liquid is transparent and clear, and drying the centrifugal product in the vacuum drying oven at 100 ℃ for 12h to obtain Na3SbS4·9H2O micro-nano multilevel structure material.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. Modifications and variations that may occur to those skilled in the art without departing from the spirit and scope of the invention are to be considered as within the scope of the invention.
Reference to the literature
[1]Wei Zhang,Shaoyi Jia,Studies of the magnetic field intensity on the synthesis of chitosan-coated magnetite nanocomposites by co-precipitation method[J],Materials Science and Engineering:C,2012,32(2):381-384.
[2]Mohammad Hossein Habibi,Bahareh Karimi,Preparation of nanostructure CuO/ZnO mixed oxide by sol–gel thermal decomposition of a CuCO3and ZnCO3:TG,DTG,XRD,FESEM and DRS investigations[J],Journal of Industrial and Engineering Chemistry:2014,20(3):925-929.
[3]Hu S,Yue W,Qiang W,et al.Synthesis of highly conductive thin-walled Al-doped ZnO single-crystal microtubes by a solid state method[J].Journal of Crystal Growth.491,(2018),97-102.
Claims (6)
1. A preparation method of a sodium thioantimonate micro-nano multilevel structure material is characterized by comprising the following steps:
(1) dissolving sodium sulfide in proper amount of solvent to obtain CNaSodium sulfide solution of = 0.6-1.0 mol/L;
(2) adding sublimed sulfur into the sodium sulfide solution obtained in the step (1) according to a preset proportion, and stirring at the temperature of 70-90 ℃ until the sulfur is completely dissolved to obtain a mixed solution;
(3) adding an antimony source into the mixed solution obtained in the step (2) according to a set proportion, and uniformly mixing to obtain a suspension;
(4) transferring the suspension obtained in the step (3) into a hydrothermal reaction kettle, carrying out hydrothermal reaction for 3-15 h at 140-200 ℃, cooling to room temperature, washing and drying the product in sequence to obtain Na3SbS4·9H2O micro-nano multilevel structure material.
2. The method for preparing the sodium thioantimonate micro-nano multilevel structure material according to claim 1, wherein in the step (1), the solvent is one of deionized water, distilled water or ultrapure water.
3. The method for preparing the sodium thioantimonate micro-nano multilevel structure material according to claim 1, wherein the method is characterized in thatIn terms of molar ration Na：n S= 1: (1.2-1.8) adding sublimed sulfur into the sodium sulfide solution obtained in the step (1);
the antimony source is Sb2S3Controlling the molar ration Na ：n Sb =（2.90～3.15）：1。
4. The method for preparing the sodium thioantimonate micro-nano multilevel structure material according to claim 1, wherein the micro-nano multilevel structure material is prepared according to a molar ration Na：n S= 1: (1.1-1.5) adding sublimed sulfur into the sodium sulfide solution obtained in the step (1);
the antimony source is Sb powder, and the molar ratio is controlledn Na ：n Sb =（2.9～3.3）：1。
5. The method for preparing the sodium thioantimonate micro-nano multilevel structure material according to claim 1, wherein in the step (4), the product is centrifugally washed with absolute ethyl alcohol for several times until a centrifugate is transparent and clear.
6. The preparation method of the sodium thioantimonate micro-nano multilevel structure material according to claim 5, wherein in the step (4), the centrifugal product is dried in a vacuum drying oven at 60-100 ℃ for 8-12 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910012825.8A CN109437297B (en) | 2019-01-07 | 2019-01-07 | Preparation method of sodium thioantimonate micro-nano multilevel structure material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910012825.8A CN109437297B (en) | 2019-01-07 | 2019-01-07 | Preparation method of sodium thioantimonate micro-nano multilevel structure material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109437297A CN109437297A (en) | 2019-03-08 |
| CN109437297B true CN109437297B (en) | 2020-12-04 |
Family
ID=65542433
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910012825.8A Active CN109437297B (en) | 2019-01-07 | 2019-01-07 | Preparation method of sodium thioantimonate micro-nano multilevel structure material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109437297B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105845976A (en) * | 2016-04-12 | 2016-08-10 | 燕山大学 | Tetragonal phase Na3SbS4 sodium fast ion conductor and preparation method thereof |
| CN108163890A (en) * | 2017-12-29 | 2018-06-15 | 广西生富锑业科技股份有限公司 | A kind of preparation method of nanometer sulfo antimony acid antimony |
| CN108455669A (en) * | 2018-04-23 | 2018-08-28 | 长沙烨星锑业有限公司 | A kind of preparation method of schlippe's salt |
-
2019
- 2019-01-07 CN CN201910012825.8A patent/CN109437297B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105845976A (en) * | 2016-04-12 | 2016-08-10 | 燕山大学 | Tetragonal phase Na3SbS4 sodium fast ion conductor and preparation method thereof |
| CN108163890A (en) * | 2017-12-29 | 2018-06-15 | 广西生富锑业科技股份有限公司 | A kind of preparation method of nanometer sulfo antimony acid antimony |
| CN108455669A (en) * | 2018-04-23 | 2018-08-28 | 长沙烨星锑业有限公司 | A kind of preparation method of schlippe's salt |
Non-Patent Citations (1)
| Title |
|---|
| Aqueous-solution synthesis of Na3SbS4 solid electrolytes for all-solid-state Na-ion batteries;Tae Won Kim等;《J. Mater. Chem. A,》;20171218;840–844 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109437297A (en) | 2019-03-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Yang et al. | Growth of CdS nanorods in nonionic amphiphilic triblock copolymer systems | |
| Ma et al. | Hierarchical, star-shaped PbS crystals formed by a simple solution route | |
| Qin et al. | Mechanism for hydrothermal synthesis of LiFePO4 platelets as cathode material for lithium-ion batteries | |
| Ibarguen et al. | Synthesis of SnO2 nanoparticles through the controlled precipitation route | |
| Liu et al. | Mesocrystals of rutile TiO2: Mesoscale transformation, crystallization, and growth by a biologic molecules-assisted hydrothermal process | |
| CN102259190A (en) | Method for quickly preparing nano silver wires with high length-diameter ratio in large batch | |
| CN102728852B (en) | Preparation method of oxide or meta-coated nickel ultrafine powder | |
| CN103193273A (en) | Preparation method of extra-long manganese dioxide nanowires | |
| CN102910615A (en) | Preparation method of graphene oxide/iron disulfide composite nano particles | |
| CN104418382B (en) | A kind of hydrothermal method prepares the method for zinc metastannate | |
| An et al. | Facile template-free synthesis and characterization of elliptic α-Fe2O3 superstructures | |
| CN109243710B (en) | Ca2+Preparation method of needle-shaped titanium dioxide/graphene nano composite conductive material doped with nano array | |
| CN106811832A (en) | A kind of pearl-decorated curtain shape BiFeO3The preparation method and products obtained therefrom of micro nanometer fiber | |
| Kawano et al. | A simple preparation technique for shape-controlled zinc oxide nanoparticles: Formation of narrow size-distributed nanorods using seeds in aqueous solutions | |
| Liu | Hydrothermal synthesis and characterization of nickel and cobalt sulfides nanocrystallines | |
| Shi et al. | Shape evolution, photoluminescence and degradation properties of novel Cu 2 O micro/nanostructures | |
| CN102976344A (en) | Preparation method of zinc silicate nanometer material | |
| CN106277040B (en) | Controllable stannic oxide microballoon of a kind of crystallite dimension and preparation method and application | |
| Li et al. | Crystal-facet-controllable synthesis of Cu 2 O microcrystals, shape evolution and their comparative photocatalytic activity | |
| Ye et al. | Microemulsion-assisted hydrothermal preparation and infrared radiation property of TiO2 nanomaterials with tunable morphologies and crystal form | |
| CN103787405A (en) | Preparation method of rutile-phase tin dioxide sol | |
| CN109437297B (en) | Preparation method of sodium thioantimonate micro-nano multilevel structure material | |
| Shanmugam et al. | Synthesis and characterization of surfactant assisted Mn2+ doped ZnO nanocrystals | |
| CN109437298B (en) | Preparation method of sodium thioantimonate nano material | |
| Dhaouadi et al. | Structural and electrical properties of nanostructured cerium phosphate |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |