CN109896542B - Magnesium-zinc stannate nano composite material and preparation method thereof - Google Patents
Magnesium-zinc stannate nano composite material and preparation method thereof Download PDFInfo
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 21
- PGTXKIZLOWULDJ-UHFFFAOYSA-N [Mg].[Zn] Chemical compound [Mg].[Zn] PGTXKIZLOWULDJ-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229940071182 stannate Drugs 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims abstract description 12
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011592 zinc chloride Substances 0.000 claims abstract description 11
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 10
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 9
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 9
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229940069446 magnesium acetate Drugs 0.000 claims abstract description 7
- 235000011285 magnesium acetate Nutrition 0.000 claims abstract description 7
- 239000011654 magnesium acetate Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000011777 magnesium Substances 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000007773 negative electrode material Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 4
- 239000010406 cathode material Substances 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract description 2
- 229910003107 Zn2SnO4 Inorganic materials 0.000 description 12
- BHSXLOMVDSFFHO-UHFFFAOYSA-N (3-ethylsulfanylphenyl)methanamine Chemical compound CCSC1=CC=CC(CN)=C1 BHSXLOMVDSFFHO-UHFFFAOYSA-N 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011366 tin-based material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- RRXGIIMOBNNXDK-UHFFFAOYSA-N [Mg].[Sn] Chemical compound [Mg].[Sn] RRXGIIMOBNNXDK-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229940097364 magnesium acetate tetrahydrate Drugs 0.000 description 1
- XKPKPGCRSHFTKM-UHFFFAOYSA-L magnesium;diacetate;tetrahydrate Chemical compound O.O.O.O.[Mg+2].CC([O-])=O.CC([O-])=O XKPKPGCRSHFTKM-UHFFFAOYSA-L 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a magnesium zinc stannate nano composite material and a preparation method thereof, wherein a certain amount of stannic chloride, zinc chloride, magnesium acetate and Cetyl Trimethyl Ammonium Bromide (CTAB) are dissolved in distilled water with a certain volume, then the distilled water is transferred to a magnetic stirrer to be stirred to obtain a mixture solution, then a proper amount of sodium hydroxide is added to adjust the pH value, the mixture solution is transferred to a high-pressure reaction kettle to carry out high-temperature high-pressure reaction, and a product after the reaction is washed, dried and then sintered in a muffle furnace to obtain the magnesium zinc stannate nano composite material. Electrochemical experiments prove that the composite material prepared by the method has wide application prospect as a lithium ion battery cathode material. The whole preparation process is simple to operate, low in raw material cost, low in equipment investment and suitable for batch production.
Description
Technical Field
The invention belongs to the field of material chemistry, and particularly relates to a magnesium-zinc stannate nano composite material and a preparation method thereof.
Background
Lithium ion batteries have become important power sources of mobile energy storage devices, and the capacity of graphite used as a negative electrode material of the lithium ion batteries is only 372mAhg at present-1The low energy density still cannot meet the mobile power requirement of social development. The pollution caused by greenhouse gases emitted by the combustion of various fossil fuels is more and more serious, and a series of problems of global warming, reduction of variety of species and the like are caused. With the rapid growth of population and the rapid development of economy in the world, the traditional non-renewable energy sources no longer meet the requirements of people, and therefore, the development of novel green renewable energy sources to replace the traditional energy sources is urgently needed. And the development and utilization of green energy sources such as wind energy, tidal energy, solar energy and the like are in urgent need of novel high-capacity energy storage materials. Secondary batteries that can be charged and discharged many times have become an important energy storage device indispensable in human society at present. Lithium ion batteries have gained wide attention because of their advantages of stable cycle, high energy density, wide working temperature range, long service life, etc. However, with the rapid development of scientific technology, it is more and more difficult for traditional lithium ion batteries to meet the actual needs, which requires researchers to continuously develop new lithium ion batteries with better performance. The tin-based material has the characteristics of high theoretical capacity, high conductivity, simple preparation, environmental friendliness, low cost and the like, and has attracted great interest of researchers, so that the tin-based material is considered to be one of the lithium battery negative electrode materials with the most application prospect.
Recently, as a composite oxide of zinc and tin, Zn2SnO4Attracts more attention of researchers due to the inverse spinel structure. Zn2SnO4Are very important materials in advanced manufacturing, such as gas sensors, photoelectrochemical cells and synergistic flame retardants (Xianjun Zhu et al, j. power Sources,2009,189, 828-. But Zn2SnO4The material expands due to volume and poor conductivity in the circulation processThe problems of poor cycle stability and poor rate performance are still not well solved. Magnesium tin composite oxide Mg2SnO4Is considered to be a substitute negative electrode material for lithium ion batteries, and has wide application and development prospects because of the characteristics of large lithium ion capacity and no pollution under low potential (Ting Xiao et al, electrochemistry. In order to better reduce the volume expansion of tin-based compounds and increase the rate capability and the cycle performance of the tin-based compounds, the invention successfully prepares the magnesium stannate zinc nano composite material through hydrothermal reaction, and the chemical formula of the nano composite material is Mg2SnO4·Zn2SnO4。
Disclosure of Invention
The invention aims to solve the technical problem of providing magnesium zinc stannate Mg in the prior art2SnO4·Zn2SnO4A nanocomposite and a method of making the same.
The technical scheme adopted by the invention for solving the technical problems is as follows: magnesium zinc stannate Mg2SnO4·Zn2SnO4The preparation method of the nano composite material is characterized in that tin tetrachloride, zinc chloride, magnesium acetate and hexadecyl trimethyl ammonium bromide are used as main raw materials, a proper amount of sodium hydroxide is added to adjust the pH value of a solution to 9-10 to obtain a precipitate mixture, then the mixture is transferred into a high-pressure reaction kettle to react for 24 hours at the temperature of 200 ℃, the precipitate product obtained by the reaction is washed and then sintered at high temperature in a muffle furnace to obtain the magnesium stannate zinc Mg2SnO4·Zn2SnO4The nano composite material specifically comprises the following steps:
1) weighing a certain amount of stannic chloride (SnCl)4·5H2O), zinc chloride (ZnCl)2) Magnesium acetate (C)4H6O4Mg·4H2O) and Cetyl Trimethyl Ammonium Bromide (CTAB) are dissolved in a certain volume of distilled water to form a mixture, and then the mixture is transferred to a magnetic stirrer to be stirred for 4 to 6 hours to obtain a mixture solution;
2) under the condition of stirring, dropwise adding 1.0mol/L NaOH solution into the mixture solution to adjust the pH value of the mixture solution to 9-10, and continuously stirring for 0.5h to obtain white turbid solution;
3) and transferring the turbid solution into a high-pressure reaction kettle, reacting at 180-200 ℃ for 24 hours, naturally cooling to room temperature, filtering precipitates after reaction, and washing with distilled water and absolute ethyl alcohol for 3 times respectively.
4) Drying the washed precipitate product at 120 ℃ for 2h, calcining at 500-600 ℃ for 8h, and naturally cooling to room temperature to obtain the magnesium-zinc stannate nanocomposite material with the chemical formula of Mg2SnO4·Zn2SnO4Or abbreviated as Mg2SnO4/Zn2SnO4。
The magnesium zinc stannate nano composite material prepared by the invention has good electrochemical performance, and the first discharge specific capacity of the nano wire as a lithium ion battery cathode material is 671.9mAh g-1After 380 times of charge-discharge circulation, the coulomb efficiency is kept above 98%.
Compared with the prior art, the invention has the following characteristics:
the composite material prepared by the method has good electrochemical performance and has wide application prospect as a lithium ion battery cathode material. The whole preparation process is simple to operate, low in raw material cost, low in equipment investment and suitable for batch production.
Drawings
FIG. 1 is an XRD pattern of a magnesium zinc stannate nanocomposite prepared according to the present invention;
FIG. 2 is an SEM image of a magnesium zinc stannate nanocomposite prepared according to the present invention;
FIG. 3 is a charge-discharge cycle chart of the magnesium zinc stannate nanocomposite prepared by the invention as a battery material.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
1) Weighing 10.0mmol (3.5060g) of stannic chloride pentahydrate, 10.0mmol of zinc chloride, 10.0mmol of magnesium acetate tetrahydrate and 0.60g of cetyltrimethylammonium bromide (CTAB) and dissolving in 30mL of distilled water to form a mixture, and then transferring to a magnetic stirrer to stir for 4 hours to obtain a mixture solution;
2) under the condition of stirring, dropwise adding 1.0mol/L NaOH solution into the mixture solution to adjust the pH of the mixture solution to 9, and continuously stirring for 0.5h to obtain white turbid solution;
3) transferring the turbid solution to a high-pressure reaction kettle, reacting at 180 ℃ for 24 hours, naturally cooling to room temperature, filtering precipitates after reaction, and washing with distilled water and absolute ethyl alcohol for 3 times respectively.
4) Drying the washed precipitate product at 120 ℃ for 2h, calcining at 500 ℃ for 8h, and naturally cooling to room temperature to obtain the magnesium zinc stannate Mg2SnO4·Zn2SnO4A nanocomposite material. Subjecting the obtained nanocomposite to powder X-ray diffraction XRD test (FIG. 1), wherein FIG. 1 shows that the X-ray diffraction peaks of the prepared material correspond to those of magnesium stannate and zinc stannate, and scanning electron microscope SEM shows that the prepared material is composed of large particles composed of fine nanoparticles (FIG. 2); the electrochemical performance of the nano-wire is tested by an electrochemical tester (figure 3), and as can be seen from figure 3, the first discharge specific capacity of the nano-wire as the negative electrode material of the lithium ion battery is 671.9mAh g-1After 380 times of charge-discharge circulation, the coulomb efficiency is kept above 98%.
Example 2
1) 5.0mmol of stannic chloride pentahydrate, 5.0mmol of zinc chloride and 5.0mmol of magnesium acetate (C) were weighed4H6O4Mg·4H2O) and 0.30g of cetyltrimethylammonium bromide (CTAB) are dissolved in 30mL of distilled water to form a mixture, and then the mixture is transferred to a magnetic stirrer to be stirred for 6 hours to obtain a mixture solution;
2) under the condition of stirring, dropwise adding 1.0mol/L NaOH solution into the mixture solution to adjust the pH value of the mixture solution to 10, and continuously stirring for 0.5h to obtain white turbid solution;
3) transferring the turbid solution into a high-pressure reaction kettle, reacting at 200 ℃ for 24 hours, naturally cooling to room temperature, filtering precipitates after reaction, and washing with distilled water and absolute ethyl alcohol for 3 times respectively;
4) drying the washed precipitate product at 120 ℃ for 2h, then calcining at 600 ℃ for 8h, and naturally cooling to room temperature to obtain the magnesium zinc stannate Mg2SnO4·Zn2SnO4A nanocomposite material.
Example 3
1) 5.0mmol of stannic chloride pentahydrate and 5.0mmol of zinc chloride (ZnCl) were weighed2) 5.0mmol of magnesium acetate (C)4H6O4Mg·4H2O) and 0.30g of cetyltrimethylammonium bromide (CTAB) are dissolved in 25mL of distilled water to form a mixture, and then the mixture is transferred to a magnetic stirrer to be stirred for 5 hours to obtain a mixture solution;
2) under the condition of stirring, dropwise adding 1.0mol/L NaOH solution into the mixture solution to adjust the pH of the mixture solution to 9.5, and continuously stirring for 0.5h to obtain white turbid solution;
3) transferring the turbid solution into a high-pressure reaction kettle, reacting at 190 ℃ for 24 hours, naturally cooling to room temperature, filtering precipitates after reaction, and washing with distilled water and absolute ethyl alcohol for 3 times respectively;
4) drying the washed precipitate product at 120 ℃ for 2h, calcining at 550 ℃ for 8h, and naturally cooling to room temperature to obtain the magnesium zinc stannate Mg2SnO4·Zn2SnO4A nanocomposite material.
Claims (2)
1. The preparation method of the magnesium-zinc stannate nano composite material is characterized by comprising the following steps:
1) weighing a certain amount of stannic chloride, zinc chloride, magnesium acetate and hexadecyl trimethyl ammonium bromide, dissolving in a certain volume of distilled water to form a mixture, and then transferring to a magnetic stirrer to stir for 4-6h to obtain a mixture solution;
2) under the condition of stirring, dropwise adding 1.0mol/L NaOH solution into the mixture solution to adjust the pH value of the mixture solution to 9-10, and continuously stirring for 0.5h to obtain white turbid solution;
3) transferring the turbid solution into a high-pressure reaction kettle, reacting at 180-200 ℃ for 24 hours, naturally cooling to room temperature, filtering precipitates after reaction, and washing with distilled water and absolute ethyl alcohol for 3 times respectively;
4) drying the washed precipitate product at 120 ℃ for 2h, calcining at 500-600 ℃ for 8h, and naturally cooling to room temperature to obtain a magnesium zinc stannate nanocomposite;
the chemical formula of the stannic chloride is SnCl4·5H2O, the chemical formula of the zinc chloride is ZnCl2The chemical formula of the magnesium acetate is C4H6O4Mg·4H2O；
The solvents, reagents or raw materials for the reaction are all chemically pure.
2. A magnesium zinc stannate nanocomposite obtained by the preparation method as recited in claim 1, wherein the nanocomposite is used as a negative electrode material of a lithium ion battery.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106512978A (en) * | 2016-11-29 | 2017-03-22 | 洛阳理工学院 | Method for preparing visible-light response photocatalyst by utilizing nano Zn2SnO4 |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106512978A (en) * | 2016-11-29 | 2017-03-22 | 洛阳理工学院 | Method for preparing visible-light response photocatalyst by utilizing nano Zn2SnO4 |
Non-Patent Citations (7)
| Title |
|---|
| Characterization of zinc magnesium stannate phosphor fine particles synthesized by electromagnetic wave heating;Mamoru Kitaura等;《Journal of Vacuum Science & Technology B》;20100330;C2C20-C2C25 * |
| Elucidating the microwave dielectric properties of (Mg(1−x)Znx)2SnO4 ceramics;Yih-Chien Chen;《Journal of Alloys and Compounds》;20120309;84-89 * |
| Hydrothermal synthesis, phase structure, optical and photocatalytic properties of Zn2SnO4 nanoparticles;Monaam Ben Ali等;《Journal of Colloid and Interface Science》;20150709;360-369 * |
| Phase structure and the dielectric properties of the (Zn,Mg)2(Ti,Sn)O4 ceramics;Xiangchun Liu等;《Journal of Alloys and Compounds》;20140522;544-548 * |
| SnO2与锡酸盐化合物纳米颗粒的合成及其电化学性能研究;余改革;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20140515;B015-72 * |
| Structural and humidity sensing characteristics of Zn2−xMgxSnO4 spinels;D. KOVACHEVA等;《JOURNAL OF MATERIALS SCIENCE LETTERS》;20011231;1597-1599 * |
| Synthesis of monodisperse single crystal Zn2SnO4 cubes with high lithium storage capacity;Na Feng等;《Materials Letters》;20120223;66-68 * |
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