CN113620259B - Ag (silver) alloy 2 Se nano material and preparation method and application thereof - Google Patents
Ag (silver) alloy 2 Se nano material and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 21
- 229910052709 silver Inorganic materials 0.000 title claims description 8
- 239000004332 silver Substances 0.000 title claims description 6
- 239000000956 alloy Substances 0.000 title claims description 4
- 229910045601 alloy Inorganic materials 0.000 title claims description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 52
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 45
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 34
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
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- 229910021641 deionized water Inorganic materials 0.000 claims description 2
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- 239000011669 selenium Substances 0.000 description 56
- 238000006243 chemical reaction Methods 0.000 description 26
- 238000000034 method Methods 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 10
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 9
- KDSXXMBJKHQCAA-UHFFFAOYSA-N disilver;selenium(2-) Chemical compound [Se-2].[Ag+].[Ag+] KDSXXMBJKHQCAA-UHFFFAOYSA-N 0.000 description 9
- 239000012071 phase Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
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- 101710134784 Agnoprotein Proteins 0.000 description 3
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000002159 nanocrystal Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- CJCPHQCRIACCIF-UHFFFAOYSA-L disodium;dioxido-oxo-selanylidene-$l^{6}-sulfane Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=[Se] CJCPHQCRIACCIF-UHFFFAOYSA-L 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- KRRRBSZQCHDZMP-UHFFFAOYSA-N selanylidenesilver Chemical compound [Ag]=[Se] KRRRBSZQCHDZMP-UHFFFAOYSA-N 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 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 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910052946 acanthite Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229940101006 anhydrous sodium sulfite Drugs 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 238000005285 chemical preparation method Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
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- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
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- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- MABNMNVCOAICNO-UHFFFAOYSA-N selenophene Chemical compound C=1C=C[se]C=1 MABNMNVCOAICNO-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Images
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- 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
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- 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
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- 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
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- Engineering & Computer Science (AREA)
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- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention discloses an Ag 2 Se nanometer material, a preparation method and application thereof, relating to the field of nanometer material preparation. Ag according to the invention 2 The preparation method of the Se nanometer material comprises the following steps: (1) Uniformly mixing solid sodium hydroxide, se powder and silver nitrate according to a certain proportion to obtain a mixture A; (2) Uniformly mixing glycerol and pure water to prepare a solvent B; (3) Adding the mixture A prepared in the step (1) and the solvent B prepared in the step (2) into a reagent bottle, uniformly mixing, and standing for 10-30min to obtain a precipitate C; (4) Washing the precipitate C prepared in the step (3) until the filtrate is neutral, and drying to obtain the Ag 2 Se nanomaterial.
Description
Technical Field
The invention relates to the field of nano material preparation, in particular to Ag 2 Se nanometer material, and its preparation method and application are provided.
Background
Ag 2 Se is a gray black compound with metallic luster, and is one of semiconductor materials with great application value. Ag (silver) 2 Se has two stable phase structures: low Wenxiang and high temp alpha phase>133 ℃ C.). Wherein the low temperature phase is beta-Ag 2 Se is a very potential thermoelectric material with not only very high electrical conductivity and a high Seebeck coefficient but also very low lattice thermal conductivity at room temperature. At present, ag is prepared 2 The method of Se can be mainly divided into a physical method and a chemical method except directly synthesizing simple substance Ag and Se by high-temperature vacuum smelting.
Physical methods such as mechanical ball milling, ohtani et al prepared Ag by mechanical ball milling 2 Se nanocrystals (Mater. Res. Bull.1997, 32 (3), 343-350.). The method has the characteristics of simple operation, low cost, low product purity and uneven particle distribution. The chemical preparation method mainly comprises template method, sonochemistry method, solvothermal method and light synthesisMethods, and the like. The hydrothermal method has the advantages of simple equipment, easily obtained raw materials, high purity of the obtained product, good uniformity, accurate control of chemical composition and the like, and is favored by many researchers. The hydrothermal method is an effective method that fluid such as water or organic solvent is used as a reaction substance in a specially-made closed reactor (autoclave), a high-temperature high-pressure reaction environment is created by heating a reaction system to a critical temperature (or close to the critical temperature), the reaction is promoted to be carried out in a liquid phase or a gas phase, the solvent of the substance which is difficult to dissolve or insoluble is recrystallized, and then the product is obtained through separation and heat treatment. Yang Fengxia et al (modern chemical industry, 2007, 27 (2), 345-346) prepared alpha-phase Ag with different morphologies in a high-pressure reaction kettle by adopting a hydrothermal synthesis mode by taking AgCl and Se powder as precursor reactants and NaOH as mineralizer 2 Se, however, the reaction temperature is different from 160 ℃ to 240 ℃, the reaction time is different from 24 hours to 72 hours, the preparation period is long, and the equipment requirement is high. Cui et al (Journal of Solid State Chemistry,172 (2003), 17-21) studied maintaining a temperature of 190℃in a high pressure reactor and controlling the reaction time from 12h to 72h, and studied AgCO in different ratios 3 Se powder is used as raw material to produce Ag in ethylenediamine, diethylenetriamine, pyridine or aqueous solution 2 Morphology and yield of Se, the shortest reaction time is up to 12h, and the highest yield is 96%. wang et al (Materials Research Bulletin,1999, 34 (6), 877-882)) by reacting with AgNO 3 Se powder and KBH 4 The raw materials react in pyridine solvent for 4 hours to prepare homogeneous spherical Ag with average size of about 25nm at room temperature 2 Se particles, but the reaction time is long and a large amount of pyridine is consumed.
The synthesis method of the silver selenide nanospheres disclosed in the patent document CN101575088A takes silver nitrate, selenophene and aniline as raw materials, and the raw materials are heated for 5 to 24 hours at the temperature of 240 ℃ in a stainless steel reaction kettle with a polytetrafluoroethylene lining; on one hand, raw materials are not easy to obtain, on the other hand, the required reaction temperature is 240 ℃, and the generated silver selenide nano-pellets are seriously aggregated and have high requirements on equipment. The preparation method of silver selenide nanometer material disclosed in CN101555000A sequentially prepares sodium selenosulfate solution, silver ion protein mixed solution and selenium-silver proteinAnd (3) mixing the liquid. When the sodium selenosulfate solution is prepared, solid anhydrous sodium sulfite and selenium powder are dissolved in distilled water and are subjected to reflux treatment for 24 hours, the prepared selenium-silver protein mixed solution is subjected to centrifugal treatment after standing reaction for 12-96 hours at room temperature, and the whole preparation process is long in time consumption and low in efficiency; the method for preparing the monodisperse semiconductor selenide nanoparticle disclosed in the patent document CN1772599A requires the addition of alkali metal hydroxide and fatty acid, and uses hydrazine hydrate as a reducing agent, so that the toxicity is high, and the operation requirement is high. On the other hand, in the process of preparing silver selenide, the silver selenide is heated in a stainless steel pressure-resistant reaction kettle to react for 24 hours at 140 ℃, and the preparation period is long and the requirement on equipment is high. The preparation method of the monodisperse silver, silver sulfide and silver selenide nanocrystals disclosed in the patent document CN101274751A comprises the steps of firstly thermally decomposing silver nitrate at 160-300 ℃, then adding selenium powder for reaction, and preparing the silver selenide nanocrystals by heating and two-step operation, so that the flow path is long. The preparation method of the spherical silver selenide particles disclosed in the patent document CN105036092B is characterized in that selenium powder and silver-ammonia complex are used as raw materials, and the raw materials are heated in an organic solvent at 160-220 ℃ for 4-24 hours, and then are cleaned and dried to prepare the spherical silver selenide particles. Ag prepared by the method 2 Se has good dispersibility and 50-500nm particle size, can be used for industrial production, but also needs to react at a certain temperature, and has long time and high energy consumption, and simultaneously generates Ag 2 Se is easily oxidized.
Preparation of Ag at present 2 The technology of Se micro-nano materials often needs high temperature, high pressure, time consumption, harsh reaction conditions or precursor solution with complex configuration and high toxicity, or equipment is complex, has high cost and is difficult to realize large-scale production, so that Ag is limited to a great extent 2 Preparation and application of Se materials.
Disclosure of Invention
Based on this, the present invention aims to overcome the above-mentioned disadvantages of the prior art to provide an Ag 2 Se nanometer material, and its preparation method and application are provided. Ag prepared by the method 2 The Se powder has high purity, and the method has the advantages of simple and novel process, small equipment quantity, low energy consumption, green and pollution-free properties and environmental friendlinessGood and convenient popularization.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: ag (silver) alloy 2 The preparation method of the Se nanometer material comprises the following steps:
(1) Uniformly mixing solid sodium hydroxide, se powder and silver nitrate according to a certain proportion to obtain a mixture A;
(2) Uniformly mixing glycerol and pure water to prepare a solvent B;
(3) Adding the mixture A prepared in the step (1) and the solvent B prepared in the step (2) into a reagent bottle, uniformly mixing, and standing for 10-30min to obtain a precipitate C;
(4) Washing the precipitate C prepared in the step (3) until the filtrate is neutral, and drying to obtain the Ag 2 Se nanomaterial.
The invention provides a method for producing Se by disproportionation reaction of Se in a mixed solvent at normal temperature 2- Ion, ag + Ions and Se 2- Ion reaction to produce Ag 2 Se. Ag provided by the invention 2 The preparation method of the Se nanometer material has the advantages of simple and novel process, small equipment quantity, low energy consumption, environment friendliness, no pollution and convenient popularization. The invention adopts a chemical method to prepare the low-temperature beta-phase Ag under the condition of no heating and no high temperature and high pressure 2 Se powder. In the step (1) of the invention, agNO is added 3 After the Se powder and the NaOH powder are fully mixed, a large amount of heat is released by adding the solvent in the step (2) to promote the reaction, and if the step (1) is not performed, the three substances are simply added into the solvent, so that obvious heat cannot be generated, and the reaction cannot be promoted.
Preferably, in the step (1), the molar ratio of the solid sodium hydroxide, the Se powder and the silver nitrate is: solid sodium hydroxide: se powder: silver nitrate=2:1, (1.33-1.37); the mesh number of Se powder is less than 80 mesh. The inventor of the application discovers through a large number of experiments that when the mesh number of Se powder is smaller than 80 meshes, se powder, naOH and AgNO 3 The mixing is more uniform and thorough.
The invention provides a chemical equation of a reaction of solid sodium hydroxide, se powder and silver nitrate under a certain condition, wherein the specific chemical equation is expressed as follows:
4AgNO 3 +3Se+6NaOH＝2Ag 2 Se+Na 2 SeO 3 +4NaNO 3 +3H 2 O
preferably, in the step (2), the volume ratio of glycerol to pure water is: glycerol: pure water= (0.2-1): (1-1.2). The pure water plays a role in dissolving the mixed powder A, the mixture starts to release heat gradually in the dissolved pure water, and the glycerol serving as an organic solvent can assist in separating the reacted solvent from the product well, so that the subsequent filtering and drying are facilitated.
Preferably, in the step (3), the mass-to-volume ratio of the mixture a to the solvent B is: mixture a: solvent b= 1:3-6; preferably, in the step (3), the reagent bottle comprises at least one of a volumetric flask, a glass bottle and a plastic bottle. In the actual process, the heat release degree of the raw materials placed in the container volumes with different volumes is different, and the heat dissipation of the container with proper size is not obvious.
Preferably, in the step (4), the detergent used for washing is at least one of deionized water, ethanol and acetone; drying at 50-90deg.C for 0.5-8 hr, and drying to dryness.
In addition, the invention provides the Ag prepared by the preparation method 2 Se nanomaterial.
Further, the invention provides the Ag 2 Application of Se nano material in thermoelectric material field.
Compared with the prior art, the invention has the beneficial effects that: (1) The heat source is provided by utilizing the reaction solution heat and the self-heating of the reaction heat, and the external heating is not needed, so that the energy consumption is avoided. (2) The raw materials are relatively cheap and easy to obtain, toxic reagents are not used, the reaction is carried out in liquid phase convection, and the method has high yield, uniform phase and high purity. (3) The reaction operation is simple, the whole reaction time is 0.5-1h, and the reaction time is greatly shortened. (4) The reaction device is simple, the reaction is rapid, the reaction can be spontaneously carried out in the reagent bottle, and the high-pressure reaction kettle is not required to be closed.
Drawings
FIG. 1 shows the Ag obtained in example 1 2 SEM image of Se nanomaterial;
FIG. 2 shows the Ag obtained in example 1 2 XRD pattern of Se nanomaterial;
FIG. 3 shows Ag obtained in comparative example 1 2 SEM image of Se nanomaterial;
FIG. 4 shows Ag obtained in comparative example 1 2 XRD pattern of Se nanomaterial.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
Example 1
An embodiment of the present invention is an Ag 2 The preparation method of the Se nanometer material comprises the following steps:
(1) Uniformly mixing solid sodium hydroxide, se powder and silver nitrate according to a certain proportion to obtain a mixture A; the molar ratio of the solid sodium hydroxide to the Se powder to the silver nitrate is as follows: solid sodium hydroxide: se powder: silver nitrate = 2:1:1.33;
(2) Uniformly mixing glycerol and pure water to prepare a solvent B; the volume ratio of the glycerol to the pure water is as follows: glycerol: pure water = 0.2:1, a step of;
(3) Adding the mixture A prepared in the step (1) and the solvent B prepared in the step (2) into a reagent bottle, uniformly mixing, and standing for 10min to obtain a precipitate C; wherein the reagent bottle is a glass bottle with the diameter of 25mm and the height of 120mm; the mass volume ratio of the mixture A to the solvent B is as follows: mixture a: solvent b=1: 3, a step of;
(4) Washing the precipitate C prepared in the step (3) until the filtrate is neutral, and drying to obtain the Ag 2 Se nanomaterial.
Example 2
An embodiment of the present invention is an Ag 2 The preparation method of the Se nanometer material comprises the following steps of：
(1) Uniformly mixing solid sodium hydroxide, se powder and silver nitrate according to a certain proportion to obtain a mixture A; the molar ratio of the solid sodium hydroxide to the Se powder to the silver nitrate is as follows: solid sodium hydroxide: se powder: silver nitrate = 2:1:1.35;
(2) Uniformly mixing glycerol and pure water to prepare a solvent B; the volume ratio of the glycerol to the pure water is as follows: glycerol: pure water = 1:1.2;
(3) Adding the mixture A prepared in the step (1) and the solvent B prepared in the step (2) into a reagent bottle, uniformly mixing, and standing for 30min to obtain a precipitate C; wherein the reagent bottle is a glass bottle with the diameter of 25mm and the height of 120mm; the mass volume ratio of the mixture A to the solvent B is as follows: mixture a: solvent b=1: 6, preparing a base material;
(4) Washing the precipitate C prepared in the step (3) until the filtrate is neutral, and drying to obtain the Ag 2 Se nanomaterial.
Meanwhile, comparative examples were set up in the present invention, and specific comparative examples were set up as follows:
comparative example 1
In comparison with example 1 alone, only the order of addition was different, one Ag as described in comparative example 1 2 The preparation method of the Se nanometer material comprises the following steps:
(1) Sequentially adding solid sodium hydroxide, se powder, silver nitrate, glycerol and pure water into a reagent bottle according to a certain proportion, uniformly mixing, and standing for 10min to obtain a precipitate; wherein the reagent bottle is a glass bottle with the diameter of 25mm and the height of 120mm;
(2) Washing the precipitate prepared in the step (1) until the filtrate is neutral, and drying to obtain the Ag 2 Se nanomaterial.
Effect verification
FIG. 1 is Ag obtained in reaction example 1 2 SEM pictures of Se nano materials show that the powder has uniform size and no agglomeration phenomenon. FIG. 2 is Ag obtained in reaction example 1 2 XRD patterns of Se nanomaterials, from which it can be seen that the resultant is single phase Ag 2 Se, the absence of miscellaneous Ag or Se. Ag prepared according to the present invention 1 and example 2 SEM photographs and XRD patterns of Se nanomaterial are similar to those of example 1 of the present invention, and are not described here.
Comparative example 1 was compared with example 1 alone, and only the order of addition was different, FIG. 3 shows Ag prepared in comparative example 1 2 SEM image of Se nanomaterial; FIG. 4 shows Ag obtained in comparative example 1 2 XRD pattern of Se nanomaterial. The comparative example has no obvious heating phenomenon in the actual experimental process. As can be seen from the SEM image of FIG. 3, ag 2 Se particles are seriously agglomerated and have coarse particle sizes. The XRD results of FIG. 4 show that there is a single impurity peak at the 30℃position, and that a single Ag is not synthesized 2 Se powder.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (6)
1. Ag (silver) alloy 2 The preparation method of the Se nanometer material is characterized by comprising the following steps:
(1) Uniformly mixing solid sodium hydroxide, se powder and silver nitrate according to a certain proportion to obtain a mixture A; wherein, the mole ratio of the solid sodium hydroxide, se powder and silver nitrate is as follows: solid sodium hydroxide: se powder: silver nitrate=2:1, (1.33-1.37);
(2) Uniformly mixing glycerol and pure water to prepare a solvent B;
(3) Adding the mixture A prepared in the step (1) and the solvent B prepared in the step (2) into a reagent bottle, uniformly mixing, and standing for 10-30min to obtain a precipitate C;
(4) Washing the precipitate C prepared in the step (3) until the filtrate is neutral, and drying to obtain the Ag 2 Se nanomaterial.
2. As claimed inThe Ag of claim 1 2 The preparation method of the Se nanometer material is characterized in that in the step (1), the mesh number of Se powder is smaller than 80 mesh.
3. Ag according to claim 1 2 The preparation method of the Se nanometer material is characterized in that in the step (2), the volume ratio of glycerol to pure water is as follows: glycerol: pure water= (0.2-1): (1-1.2).
4. Ag according to claim 1 2 The preparation method of the Se nanometer material is characterized in that in the step (3), the mass volume ratio of the mixture A to the solvent B is as follows: mixture a: solvent b=1: 3-6.
5. Ag according to claim 1 2 The preparation method of the Se nanometer material is characterized in that in the step (3), the reagent bottle comprises at least one of a volumetric flask, a glass bottle and a plastic bottle.
6. Ag according to claim 1 2 The preparation method of the Se nanometer material is characterized in that in the step (4), the washing agent used for washing is at least one of deionized water, ethanol and acetone; the drying temperature is 50-90 ℃, and the drying time is 0.5-8h.
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| IL141527A0 (en) * | 2001-02-20 | 2002-03-10 | Chemergy Ltd | Silver manganese salt cathodes for alkaline batteries |
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