CN101559933A - Solvent-thermal method for preparing spring-shaped superstructural Sn(HPO4)2.H2O nanodisk - Google Patents
Solvent-thermal method for preparing spring-shaped superstructural Sn(HPO4)2.H2O nanodisk Download PDFInfo
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- CN101559933A CN101559933A CNA2009100620107A CN200910062010A CN101559933A CN 101559933 A CN101559933 A CN 101559933A CN A2009100620107 A CNA2009100620107 A CN A2009100620107A CN 200910062010 A CN200910062010 A CN 200910062010A CN 101559933 A CN101559933 A CN 101559933A
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Abstract
The invention provides a solvent-thermal method for preparing a spring-shaped superstructural Sn(HPO4)2.H2O nanodisk, which belongs to the category of nanometer material preparation by a wet chemical method. The method is characterized in that the method comprises the following steps of: adopting stannic salt as a raw material, and dissolving the stannic salt into anhydrous ethanol to obtain a tin salt solution; then dripping 85 weight percent strong phosphoric acid into the solution; and obtaining a spring-shaped superstructural Sn(HPO4).2H2O nanodisk powder material through the solvent-thermal treatment at a temperature of between 140 and 200 DEG C, the centrifugal washing and the drying. The method has the advantages that the method has mild preparation conditions, can obtain the spring-shaped superstructural Sn(HPO4)2.H2O nanodisk without high-temperature roasting, can control the size of the material by changing the preparation conditions, has simple equipment and process, and is easy to realize mass industrialized production.
Description
Technical field
The present invention is a kind of preparation spring-like superstructure Sn (HPO
4)
2H
2The method of O nanometer plate belongs to wet chemical method and prepares the nano material category.Utilize present method not need high-temperature roasting can obtain the material of wanting.
Background technology
Lithium-ion secondary cell is to use and the best a kind of power supply of DEVELOPMENT PROSPECT, and negative material is one of key factor of its overall performance of restriction.The negative material that commercial lithium ion battery adopted nearly all is carbon/graphite material the earliest, but because carbon/graphite material when discharging and recharging for the first time, can form passive film at carbon surface, cause capacitance loss; And the current potential of the electropotential of carbon and lithium is very approaching, and when over-charging of battery, metallic lithium may be separated out in carbon electrodes, form dendrite and cause safety problem, and capacity is lower.Thereby need research and development novel high-energy lithium ion battery negative material.The electrode materials that nano material is applied to lithium ion battery has become when previous important research project.The lithium ion cell nano material is compared with the non-nano material, has following advantage: (1) can participate in the micron order size material the reaction that can not carry out; (2) specific surface area is big, helps to reduce the polarization phenomena in the electrode electro Chemical process and increases contact area between electrode and the electrolytic solution, so more help lithium ion in charge and discharge process embedding and deviate from; (3) granularity is little, and lithium ion insert depth therein is shallow, the evolving path is short, help lithium ion therein take off embedding fast; (4) discharge lithium better and embed and take off stress in the embedding process, improve cycle life.
Have not yet to see (HPO about preparation spring-like superstructure Sn
4)
2H
2The patent report of O nanometer plate negative material.
The present invention utilizes the direct preparation of one step of low-temperature solvent thermal response to have spring-like superstructure Sn (HPO
4)
2H
2O nanometer plate negative material, technology is simple and easy to control, and cost is low, is convenient to further extension and produces.
Summary of the invention
The object of the present invention is to provide a kind of employing low temperature to synthesize spring-like superstructure Sn (HPO
4)
2H
2O nanometer plate preparation methods, its material can be used as the negative electrode material of lithium ion battery.
Spring-like superstructure Sn (HPO of the present invention
4)
2H
2The preparation method of O nanometer plate is a solvent-thermal method, may further comprise the steps: step 1, employing tetravalence pink salt are starting material, it are dissolved in obtain tin-salt solution in the dehydrated alcohol, and the concentration of tin-salt solution is 0.2～2mol/L;
Step 2, in the solution that step 1 obtains, drip the strong phosphoric acid of 85wt%, the pH value 5 of regulator solution;
Step 3, step 2 gained solution is placed reactor, 80% volume of water heating kettle is filled, under 140～200 ℃, carried out solvent thermal reaction 12～48 hours;
After step 4, step 3 finish, use distilled water and absolute ethanol washing more than 3 times respectively solid product, drying obtains the white powder material then, promptly gets spring-like superstructure Sn (HPO
4)
2H
2O nanometer plate product.
Spring-like superstructure Sn (HPO provided by the invention
4)
2H
2O nanometer plate preparation method's outstanding advantage is:
1, preparation condition gentleness does not need high-temperature roasting can obtain spring-like superstructure Sn (HPO4)
2H
2The O nanometer plate.
2, preparation equipment and technology are simple, and is with short production cycle, and processing parameter is controlled easily, is easy to industry and promotes.
3, spring-like superstructure Sn (HPO
4)
2H
2The O nanometer plate has higher initial discharge capacity as the negative electrode material of lithium ion battery, is particularly suited for being applied in the negative electrode material aspect.
Description of drawings
Fig. 1 is the spring-like superstructure Sn (HPO of solvent thermal reaction preparation
4)
2H
2The XRD figure of O nanometer plate.
Fig. 2 is the spring-like superstructure Sn (HPO of solvent thermal reaction preparation
4)
2H
2The SEM figure of O nanometer plate.
Fig. 3 is spring-like superstructure Sn (HPO
4)
2H
2The O nanometer plate is as the charge-discharge performance curve of lithium ion battery negative electrode materials.
The gained sample is tested through XRD, and the peak value of the characteristic peak in the diffracting spectrum (seeing Fig. 1) and standard diffracting spectrum (JCPDS, Card No.31-1397) coincide, and illustrates that product is pure Sn (HPO4)
2·H
2The O phase. The gained sample is aobvious through scanning electron Micro mirror (JSM-5600) is observed (seeing Fig. 2), finds that product is made up of spring-like superstructure nanometer plate. The spring-like superstructure Length be 0.5～5.0 μ m. Each spring-like superstructure is that the nanometer plate of 400～800nm forms by diameter. The institute Get sample through charge-discharge performance test (seeing Fig. 3), initial discharge capacity can reach 373.7mAh/g, and this nanometer material is described Material has preferably application prospect as lithium ion battery negative material.
Embodiment
Embodiment 1
Step 1, take by weighing tin chloride, it is dissolved in the dehydrated alcohol, the concentration that is made into 160 milliliters of tin ions is 0.2mol/L solution;
The pH value of the strong phosphoric acid regulator solution of step 2, dropping 85wt% is 5;
Step 3, step 2 gained solution is placed 200 milliliters of reactors, under 180 ℃, carried out solvent thermal reaction 24 hours;
After step 4, step 3 finish, solid product is used distilled water and dehydrated alcohol centrifuge washing respectively 3 times;
Step 5, the product that step 4 is obtained be positioned in the thermostatic drying chamber 60 ℃ dry 12 hours down, obtain spring-like superstructure Sn (HPO
4)
2H
2The O nanometer plate.
Embodiment 2
Step 1, take by weighing tin chloride, it is dissolved in the dehydrated alcohol, the concentration that is made into 160 milliliters of tin ions is 1mol/L solution;
The pH value of the strong phosphoric acid regulator solution of step 2, dropping 85wt% is 5;
Step 3, step 2 gained solution is placed 200 milliliters of reactors, under 180 ℃, carried out solvent thermal reaction 24 hours;
After step 4, step 3 finish, solid product is used distilled water and dehydrated alcohol centrifuge washing respectively 4 times;
Step 5, the product that step 4 is obtained be positioned in the thermostatic drying chamber 60 ℃ dry 12 hours down, obtain spring-like superstructure Sn (HPO
4)
2H
2The O nanometer plate.
Embodiment 3
Step 1, take by weighing tin chloride, it is dissolved in the dehydrated alcohol, the concentration that is made into tin ion in 160 ml solns is 0.2mol/L;
The pH value of the strong phosphoric acid regulator solution of step 2, dropping 85wt% is 5;
Step 3, step 2 gained solution is placed 200 milliliters of reactors, under 180 ℃, carried out solvent thermal reaction 48 hours;
After step 4, step 3 finish, solid product is used distilled water and dehydrated alcohol centrifuge washing respectively 3 times;
Step 5, the product that step 4 is obtained be positioned in the thermostatic drying chamber 60 ℃ dry 12 hours down, obtain spring-like superstructure Sn (HPO
4)
2H
2The O nanometer plate.
Embodiment 4
Step 1, take by weighing tin chloride, it is dissolved in the dehydrated alcohol, the concentration that is made into 160 milliliters of tin ions is 0.2mol/L solution;
The pH value of the strong phosphoric acid regulator solution of step 2, dropping 85wt% is 5;
Step 3, step 2 gained solution is placed 200 milliliters of reactors, under 200 ℃, carried out solvent thermal reaction 24 hours;
After step 4, step 3 finish, solid product is used distilled water and dehydrated alcohol centrifuge washing respectively 3 times;
Step 5, the product that step 4 is obtained be positioned in the thermostatic drying chamber 60 ℃ dry 12 hours down, obtain spring-like superstructure Sn (HPO
4)
2H
2The O nanometer plate.
Embodiment 5
Step 1, take by weighing tin chloride, it is dissolved in the dehydrated alcohol, the concentration that is made into 160 milliliters of tin ions is 1mol/L solution;
The pH value of the strong phosphoric acid regulator solution of step 2, dropping 85wt% is 5;
Step 3, step 2 gained solution is placed 200 milliliters of reactors, 80% volume of water heating kettle is filled, under 180 ℃, carried out solvent thermal reaction 48 hours;
After step 4, step 3 finish, solid product is used distilled water and dehydrated alcohol centrifuge washing respectively 3 times;
Step 5, the product that step 4 is obtained be positioned in the thermostatic drying chamber 60 ℃ dry 12 hours down, obtain spring-like superstructure Sn (HPO
4)
2H
2The O nanometer plate.
Embodiment 6
Step 1, take by weighing tin chloride, it is dissolved in the dehydrated alcohol, the concentration that is made into 160 milliliters of tin ions is 1.4mol/L solution;
The pH value of the strong phosphoric acid regulator solution of step 2, dropping 85wt% is 5;
Step 3, step 2 gained solution is placed 200 milliliters of reactors, under 140 ℃, carried out solvent thermal reaction 36 hours;
After step 4, step 3 finish, solid product is used distilled water and dehydrated alcohol centrifuge washing respectively 3 times;
Step 5, the product that step 4 is obtained be positioned in the thermostatic drying chamber 60 ℃ dry 12 hours down, obtain spring-like superstructure Sn (HPO
4)
2H
2The O nanometer plate.
Embodiment 7
Step 1, take by weighing nitric acid tin, it is dissolved in the dehydrated alcohol, the concentration that is made into 160 milliliters of tin ions is 0.2mol/L solution;
The pH value of the strong phosphoric acid regulator solution of step 2, dropping 85wt% is 5;
Step 3, step 2 gained solution is placed 200 milliliters of reactors, under 180 ℃, carried out solvent thermal reaction 24 hours;
After step 4, step 3 finish, solid product is used distilled water and dehydrated alcohol centrifuge washing respectively 3 times;
Step 5, the product that step 4 is obtained be positioned in the thermostatic drying chamber 60 ℃ dry 12 hours down, obtain spring-like superstructure Sn (HPO
4)
2H
2The O nanometer plate.
Embodiment 8
Step 1, take by weighing nitric acid tin, it is dissolved in the dehydrated alcohol, the concentration that is made into 160 milliliters of tin ions is 2mol/L solution;
The pH value of the strong phosphoric acid regulator solution of step 2, dropping 85wt% is 5;
Step 3, step 2 gained solution is placed 200 milliliters of reactors, under 180 ℃, carried out solvent thermal reaction 12 hours;
After step 4, step 3 finish, solid product is used distilled water and dehydrated alcohol centrifuge washing respectively 3 times;
Step 5, the product that step 4 is obtained be positioned in the thermostatic drying chamber 60 ℃ dry 12 hours down, obtain spring-like superstructure Sn (HPO
4)
2H
2The O nanometer plate.
Claims (2)
1, spring-like superstructure Sn (HPO
4)
2H
2The preparation method of O nanometer plate is characterized in that, solvent-thermal method may further comprise the steps:
1) adopting the tetravalence pink salt is starting material, it is dissolved in obtain tin-salt solution in the dehydrated alcohol, and the concentration of tin-salt solution is 0.2～2mol/L;
2) strong phosphoric acid of dropping 85wt% in the solution that step 1) obtains, the pH value of regulator solution is 5;
3) with step 2) gained solution places reactor, and 80% volume of water heating kettle is filled, and carries out solvent thermal reaction 12～48 hours under 140～200 ℃;
4) after step 3) finishes, use distilled water and absolute ethanol washing more than 3 times respectively solid product, drying obtains the white powder material then, promptly gets spring-like superstructure Sn (HPO
4)
2H
2O nanometer plate product.
2, spring-like superstructure Sn (HPO according to claim 1
4)
2H
2The preparation method of O nanometer plate is characterized in that: described tetravalence pink salt is nitric acid tin or tin chloride.
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|---|---|---|---|
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| CNA2009100620107A CN101559933A (en) | 2009-05-08 | 2009-05-08 | Solvent-thermal method for preparing spring-shaped superstructural Sn(HPO4)2.H2O nanodisk |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103178264A (en) * | 2011-12-20 | 2013-06-26 | 比亚迪股份有限公司 | Cathode active material, preparation method thereof, and lithium ion battery |
| CN106328990A (en) * | 2016-11-07 | 2017-01-11 | 上海碳源汇谷新材料科技有限公司 | Lithium ion battery anode material based on redox graphene/layered metal phosphate composite material |
| CN106328989A (en) * | 2016-11-07 | 2017-01-11 | 上海碳源汇谷新材料科技有限公司 | Application of metal phosphate to negative electrode material of lithium-ion battery |
| CN112928276A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | Composite sulfur positive electrode material and preparation method and application thereof |
-
2009
- 2009-05-08 CN CNA2009100620107A patent/CN101559933A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103178264A (en) * | 2011-12-20 | 2013-06-26 | 比亚迪股份有限公司 | Cathode active material, preparation method thereof, and lithium ion battery |
| CN103178264B (en) * | 2011-12-20 | 2015-07-22 | 比亚迪股份有限公司 | Cathode active material, preparation method thereof, and a lithium battery |
| CN106328990A (en) * | 2016-11-07 | 2017-01-11 | 上海碳源汇谷新材料科技有限公司 | Lithium ion battery anode material based on redox graphene/layered metal phosphate composite material |
| CN106328989A (en) * | 2016-11-07 | 2017-01-11 | 上海碳源汇谷新材料科技有限公司 | Application of metal phosphate to negative electrode material of lithium-ion battery |
| CN106328990B (en) * | 2016-11-07 | 2019-02-12 | 上海碳源汇谷新材料科技有限公司 | Based on redox graphene/layered metal phosphates composite material lithium ion battery negative material |
| CN112928276A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | Composite sulfur positive electrode material and preparation method and application thereof |
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Open date: 20091021 |