CN104724751A - Method for synthesizing tin sulfide nano-wires at low temperature and application - Google Patents
Method for synthesizing tin sulfide nano-wires at low temperature and application Download PDFInfo
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- CN104724751A CN104724751A CN201510078909.3A CN201510078909A CN104724751A CN 104724751 A CN104724751 A CN 104724751A CN 201510078909 A CN201510078909 A CN 201510078909A CN 104724751 A CN104724751 A CN 104724751A
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Abstract
The invention relates to tin sulfide nano-wires serving as a cathode material of a lithium ion battery, belongs to the field of lithium ion battery materials, and particularly relates to a method for synthesizing tin sulfide nano-wires at a low temperature and application. By adopting a one-pot method and low-temperature synthesis, the required equipment is simple, the reaction conditions are mild, and the method is simple, feasible, low in cost and easy to realize industrialized production. The manufactured tin sulfide nano-wires are mainly applied to lithium ion batteries, super capacitors, solar cells and the like, so that the tin sulfide nano-wires have huge market prospect and development potential.
Description
Technical field
The present invention relates to a kind of by tin sulfide nano wire as lithium ion battery negative material, belong to field of lithium ion battery material, particularly relate to method and the application of a kind of low temperature synthesis tin sulfide nano wire.
Background technology
Along with developing rapidly of electronic technology, increasing industrialization product as: TV, computer, mobile phone, new-energy automobile etc. have entered in daily life, improve the living condition of people greatly.But the exhaustion day by day of consequent global environmental pollution and the energy, quality little to volume be light, have extended cycle life, the requirement of battery that specific storage is high is also more and more higher.Compared with other traditional energy-storage batteries, lithium ion battery energy density is high, can reach 150 ~ 200Wh/kg, far above the 60-75Wh/Kg of Ni-MH battery; The open circuit voltage very Gao Keda 3.3 ~ 4.2V of lithium ion battery, far above the 2V of lead-acid cell; In addition lithium ion battery also has the advantages such as output rating is large, charge/discharge rates is fast, operating temperature range is wide.These factors all will be embodied predictive of the following status of lithium dynamical battery.
Tin sulfide has CdI2 type laminate structure, one deck tin atom is mixed between two-layer sulphur atom, metallic tin ion is placed between two-layer sulfonium ion, six sulfonium ions are had to form regular octahedron coordination around each tin ion, namely sulfonium ion takes AB AB hexagonal closs packing, be covalent bonds in layer, there is weak Van der Waals force between layers.There is a lot of lattice vacancy in this laminate structure of SnS2, can be used as the host lattice of " intercalation ".This structural superior snappiness makes it as substrate, by the insertion of conjugated compound, can form the intercalation compound with unique photoelectric property.Lithium ion also can insert wherein, and therefore, tin sulfide is also considered to promising lithium ion battery negative material.
Tradition prepares the complicated process of preparation of tin sulfide nano wire, energy consumption is large, and the requirement for experiment condition of these methods is harsh, and some hydrothermal temperatures are up to 200 DEG C, and it is even longer that the hydro-thermal time also reaches 24h.In conventional hydrothermal method, the reaction vessel used is all teflon-lined autoclave.The condition of these preparation methods is high, and energy consumption is high.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide a kind of low temperature to synthesize method and the application of tin sulfide nano wire.
Technical scheme of the present invention: a kind of method of low temperature synthesis tin sulfide nano wire, is characterized in that, the method for described low temperature synthesis tin sulfide nano wire adopts one pot process, and step is as follows:
1) in reaction vessel, by protein water soln and Sn (NO3) 4 aqueous solution even, the concentration of protein water soln is 50 mg/ml, the concentration of Sn (NO3) 4 aqueous solution is for being 10 mM/ls, the volume ratio of protein water soln and Sn (NO3) 4 aqueous solution is for being 1:1, under magnetic agitation, normal-temperature reaction 5 minutes, obtains colourless transparent liquid;
2) aforesaid liquid pH is regulated to be 10.0 with the NaOH aqueous solution that concentration is 1 mol/L;
3) by above-mentioned 1), 2) the step liquid of preparing one group of volume identical adds in container respectively, in each container, add concentration be respectively the chalcogenide compound aqueous solution of 10-100 mM/l and regulate the mol ratio of Sn element and S element to be 1:2-4, under stirring, 48 DEG C of conditions, reaction 10 hours, can obtain tin sulfide nano wire.
As preferably, described protein is bovine serum albumin.
As preferably, described chalcogenide compound is potassium sulphide, ammonium sulfide, Thioglycolic acid sodium salt or gsh.
The application of tin sulfide nano wire in lithium ion battery negative material of the method synthesis of low temperature synthesis tin sulfide nano wire.
By technique scheme, the advantage that the present invention has and beneficial effect are:
1, the present invention is by tin sulfide nano wire, wherein by tin sulfide material nano, greatly reduce in circulating battery process, the volume effect of electrode materials, and that innovates has obtained the tin sulfide of nano wire, and between nano wire and nano wire, have enough large space, nano wire is in lithium ion insertion and deintercalation process, owing to there being enough large space between the lines, material of main part can not be caused mutually to extrude efflorescence, the lithium storage content of further increase lithium ion battery negative material, makes irreversible capacity reduce.
2, the material obtained by the present invention is mainly used in the aspects such as lithium ion battery, ultracapacitor, solar cell, therefore, and the market outlook that it is beaten before having and development potentiality.And the low temperature synthesis that the present invention is used, required equipment is simple, and reaction conditions is gentle, and simple, cost is low, is easy to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of embodiment 1 according to the tin sulfide nano wire of the method synthesis of low temperature synthesis tin sulfide nano wire provided by the invention, and (b) is the partial enlarged drawing of (a).
Embodiment
Below by way of specific specific examples, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification sheets can understand other advantages of the present invention and effect easily.The present invention can also be implemented by embodiments different in addition, and the every details in this specification sheets also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
Embodiment 1: a kind of method of low temperature synthesis tin sulfide nano wire, it is characterized in that, the synthetic method of described tin sulfide nano wire adopts one pot process, and step is as follows:
1) in round-bottomed flask, be the Bovine Serum Albumin in Aqueous Solution of 50 mg/ml and 5 ml concns by 5 ml concns for for 10 mM/ls of Sn (NO3) 4 aqueous solution even, under magnetic agitation, normal-temperature reaction 5 minutes, obtains colourless transparent liquid;
2) aforesaid liquid pH is regulated to be 10.0 with the ammonia soln that 0.5 ml concn is 1 mol/L;
3) by above-mentioned 1), 2) step prepares the liquid that three parts of volumes are 10.5 milliliters and adds in three containers respectively, in three containers, add 0.5 ml concn is respectively that the potassium sulfide aqueous solution of 16.7 mM/ls, 25 mM/ls and 100 mM/ls is to regulate the mol ratio of Sn element and S element for 1:2,1:3,1:4.Under stirring, 37 DEG C of conditions, reaction 10 hours, can obtain SnS2 nano wire.The SnS2 obtained is nano thread structure, and its diameter is about 10nm, and length is 200-300nm.
Embodiment 2: a kind of method of low-temperature growth tin sulfide nano wire, is characterized in that, the preparation method of described tin sulfide nano wire adopts one pot process, and step is as follows:
1) in round-bottomed flask, be the Bovine Serum Albumin in Aqueous Solution of 50 mg/ml and 5 ml concns by 5 ml concns for for 10 mM/ls of Sn (NO3) 4 aqueous solution even, under magnetic agitation, normal-temperature reaction 5 minutes, obtains colourless transparent liquid;
2) aforesaid liquid pH is regulated to be 10.0 with the ammonia soln that 0.5 ml concn is 1 mol/L;
3) by above-mentioned 1), 2) step prepares the liquid that three parts of volumes are 10.5 milliliters and adds in three containers respectively, in three containers, add 0.5 ml concn is respectively that the ammonium sulfide solution of 16.7 mM/ls, 25 mM/ls and 100 mM/ls is to regulate the mol ratio of Sn element and S element for 1:2,1:3,1:4.Under stirring, 37 DEG C of conditions, reaction 10 hours, can obtain SnS2 nano wire.The SnS2 obtained is nano thread structure, and its diameter is about 10nm, and length is 200-300nm.
Embodiment 3: a kind of method of low temperature synthesis tin sulfide nano wire, it is characterized in that, the synthetic method of described tin sulfide nano wire adopts one pot process, and step is as follows:
1) in round-bottomed flask, be the Bovine Serum Albumin in Aqueous Solution of 50 mg/ml and 5 ml concns by 5 ml concns for for 10 mM/ls of Sn (NO3) 4 aqueous solution even, under magnetic agitation, normal-temperature reaction 5 minutes, obtains colourless transparent liquid;
2) aforesaid liquid pH is regulated to be 10.0 with the ammonia soln that 0.5 ml concn is 1 mol/L;
3) by above-mentioned 1), 2) step prepares the liquid that three parts of volumes are 10.5 milliliters and adds in three containers respectively, in three containers, add 0.5 ml concn is respectively that the Thiovanic acid sodium water solution of 16.7 mM/ls, 25 mM/ls and 100 mM/ls is to regulate the mol ratio of Sn element and S element for 1:2,1:3,1:4.Under stirring, 37 DEG C of conditions, reaction 10 hours, can obtain SnS2 nano wire.The SnS2 obtained is nano thread structure, and its diameter is about 10nm, and length is 200-300nm.
Embodiment 4: a kind of method of low temperature synthesis tin sulfide nano wire, it is characterized in that, the synthetic method of described tin sulfide nano wire adopts one pot process, and step is as follows:
1) in round-bottomed flask, be the Bovine Serum Albumin in Aqueous Solution of 50 mg/ml and 5 ml concns by 5 ml concns for for 10 mM/ls of Sn (NO3) 4 aqueous solution even, under magnetic agitation, normal-temperature reaction 5 minutes, obtains colourless transparent liquid;
2) aforesaid liquid pH is regulated to be 10.0 with the ammonia soln that 0.5 ml concn is 1 mol/L;
3) by above-mentioned 1), 2) step synthesizes the liquid that three parts of volumes are 10.5 milliliters and adds in three containers respectively, in three containers, add 0.5 ml concn is respectively that the gsh aqueous solution of 16.7 mM/ls, 25 mM/ls and 100 mM/ls is to regulate the mol ratio of Sn element and S element for 1:2,1:3,1:4.Under stirring, 37 DEG C of conditions, reaction 10 hours, can obtain SnS2 nano wire.The SnS2 obtained is nano thread structure, and its diameter is about 10nm, and length is 200-300nm.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (4)
1. a method for low temperature synthesis tin sulfide nano wire, is characterized in that, the method for described low temperature synthesis tin sulfide nano wire adopts one pot process, and step is as follows:
1) in reaction vessel, by protein water soln and Sn (NO3) 4 aqueous solution even, the concentration of protein water soln is 50 mg/ml, the concentration of Sn (NO3) 4 aqueous solution is for being 10 mM/ls, the volume ratio of protein water soln and Sn (NO3) 4 aqueous solution is for being 1:1, under magnetic agitation, normal-temperature reaction 5 minutes, obtains colourless transparent liquid;
2) aforesaid liquid pH is regulated to be 10.0 with the NaOH aqueous solution that concentration is 1 mol/L;
3) by above-mentioned 1), 2) the step liquid of preparing one group of volume identical adds in container respectively, in each container, add concentration be respectively the chalcogenide compound aqueous solution of 10-100 mM/l and regulate the mol ratio of Sn element and S element to be 1:2-4, under stirring, 48 DEG C of conditions, reaction 10 hours, can obtain tin sulfide nano wire.
2. the method for low temperature synthesis tin sulfide nano wire according to claim 1, is characterized in that: described protein is bovine serum albumin.
3. low temperature synthesizes the method for tin sulfide nano wire according to claim 1, it is characterized in that: described chalcogenide compound is potassium sulphide, ammonium sulfide, Thioglycolic acid sodium salt or gsh.
4. adopt the application of tin sulfide nano wire in lithium ion battery negative material of the method synthesis of the low temperature synthesis tin sulfide nano wire according to any one of claim 1-3.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107814408A (en) * | 2017-11-15 | 2018-03-20 | 龙岩学院 | A kind of SnS rich in S vacancies position2The preparation method of ultrathin nanometer piece |
| CN114380325A (en) * | 2021-12-11 | 2022-04-22 | 上海工程技术大学 | Ultra-thin SnS2Nanosheet and SnS2Film, preparation and application thereof |
Citations (5)
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| US3642464A (en) * | 1968-12-09 | 1972-02-15 | Univ Minnesota | Tin ore treating process |
| US20090029258A1 (en) * | 2007-07-25 | 2009-01-29 | Samsung Electro-Mechanics Co., Ltd. | Preparing method of tin sulfide nanoparticles and manufacturing method of lithium ion battery using the same |
| CN101844799A (en) * | 2010-06-17 | 2010-09-29 | 安阳师范学院 | Preparation method of hexagon stannic disulphide nano slice |
| CN102897827A (en) * | 2012-10-09 | 2013-01-30 | 东华大学 | Method for phased synthesis of SnS, SnS2 or SnS/SnS2 heterojunction nanocrystalline material by one-step process |
| CN103915625A (en) * | 2014-04-09 | 2014-07-09 | 暨南大学 | Preparation method and application of spherical tin sulfide consisting of nanorods |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3642464A (en) * | 1968-12-09 | 1972-02-15 | Univ Minnesota | Tin ore treating process |
| US20090029258A1 (en) * | 2007-07-25 | 2009-01-29 | Samsung Electro-Mechanics Co., Ltd. | Preparing method of tin sulfide nanoparticles and manufacturing method of lithium ion battery using the same |
| CN101844799A (en) * | 2010-06-17 | 2010-09-29 | 安阳师范学院 | Preparation method of hexagon stannic disulphide nano slice |
| CN102897827A (en) * | 2012-10-09 | 2013-01-30 | 东华大学 | Method for phased synthesis of SnS, SnS2 or SnS/SnS2 heterojunction nanocrystalline material by one-step process |
| CN103915625A (en) * | 2014-04-09 | 2014-07-09 | 暨南大学 | Preparation method and application of spherical tin sulfide consisting of nanorods |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107814408A (en) * | 2017-11-15 | 2018-03-20 | 龙岩学院 | A kind of SnS rich in S vacancies position2The preparation method of ultrathin nanometer piece |
| CN107814408B (en) * | 2017-11-15 | 2020-01-31 | 龙岩学院 | SnS rich in S vacancy2Preparation method of ultrathin nanosheet |
| CN114380325A (en) * | 2021-12-11 | 2022-04-22 | 上海工程技术大学 | Ultra-thin SnS2Nanosheet and SnS2Film, preparation and application thereof |
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