CN103708539B - A kind of preparation method of rock salt type LiTiO2 nanoparticle - Google Patents
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 title claims description 15
- 235000002639 sodium chloride Nutrition 0.000 title claims description 14
- 239000011780 sodium chloride Substances 0.000 title claims description 14
- 229910012675 LiTiO2 Inorganic materials 0.000 title abstract description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 57
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910012672 LiTiO Inorganic materials 0.000 claims abstract description 22
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 239000002121 nanofiber Substances 0.000 claims abstract description 9
- 239000011435 rock Substances 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000010335 hydrothermal treatment Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 229910052744 lithium Inorganic materials 0.000 abstract description 2
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- 229910001416 lithium ion Inorganic materials 0.000 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910018068 Li 2 O Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明涉及一种岩盐型LiTiO2纳米颗粒的制备方法，采用水热法，以K2Ti6O13纳米纤维为钛源前躯体，硝酸锂为锂源，氢氧化钾为矿化剂，利用简单的一步水热反应制得形貌较规则，尺寸较小，物相较纯的岩盐型LiTiO2纳米颗粒。本发明制备工艺简单，易于控制，无污染，成本低，适于规模化生产。The invention relates to a method for preparing rock salt-type LiTiO2 nanoparticles. A hydrothermal method is adopted, and K2Ti6O13 nanofibers are used as a titanium source precursor, lithium nitrate is used as a lithium source, and potassium hydroxide is used as a mineralizer . A simple one-step hydrothermal reaction produces rock-salt-type LiTiO 2 nanoparticles with regular morphology, small size and relatively pure phase. The preparation process of the invention is simple, easy to control, pollution-free, low in cost and suitable for large-scale production.
Description
技术领域 technical field
本发明涉及一种岩盐型LiTiO2纳米颗粒的制备方法，属于无机非金属材料技术领域。 The invention relates to a method for preparing rock salt-type LiTiO2 nanoparticles, which belongs to the technical field of inorganic non-metallic materials.
背景技术 Background technique
LiTiO2可以作为第二代锂离子电池的阴极材料，为NaCl结构，氧原子为面心立方堆积，并且阳离子位于八面体的空隙里并且形成超结构。这种超结构可以提供可供Li离子出入的隧道，在锂离子电池材料的应用方面有较好的应用前景。目前，岩盐型LiTiO2通常采取高温烧结和高温电化学合成方法制备，如Lecerf在1000℃，以Ti2O3与Li2O为原料制得纯度不高，颗粒尺寸较大的LiTiO2，Jiang等在700℃熔融的LiCl中对锐钛矿TiO2进行电解，电压介于3.2~2V时，产物为尺寸在4μm左右大颗粒的岩盐型LiTiO2。 LiTiO 2 can be used as the cathode material of the second-generation lithium-ion battery. It has a NaCl structure, and the oxygen atoms are face-centered cubic stacked, and the cations are located in the octahedral gaps and form a superstructure. This superstructure can provide a tunnel for Li ions to enter and exit, and has a good application prospect in the application of lithium ion battery materials. At present, rock-salt LiTiO 2 is usually prepared by high-temperature sintering and high-temperature electrochemical synthesis. For example, Lecerf used Ti 2 O 3 and Li 2 O as raw materials to prepare LiTiO 2 with low purity and large particle size at 1000 ° C. Jiang et al. Electrolyzed anatase TiO 2 in molten LiCl at 700°C, and when the voltage was between 3.2 and 2V, the product was rock-salt LiTiO 2 with a size of about 4 μm.
相对于高温烧结及高温电化学合成方法而言，水热法可在相对较低温度实现岩盐型LiTiO2的合成，如裴先茹等人以LiOH和锐钛矿TiO2为反应物料利用水热法成功合成出岩盐型LiTiO2，且水热法可以通过调节溶剂、矿化剂、温度、时间等很简洁方便的来控制合成晶体的维度和其几何形状。 Compared with high-temperature sintering and high-temperature electrochemical synthesis methods, the hydrothermal method can realize the synthesis of rock-salt LiTiO2 at a relatively low temperature . The rock-salt type LiTiO 2 is synthesized, and the hydrothermal method can control the dimension and geometry of the synthesized crystal simply and conveniently by adjusting the solvent, mineralizer, temperature, time, etc.
在锂离子电池的应用方面，一方面尺寸较小的岩盐型LiTiO2纳米颗粒由于其比表面积的增大能一定程度上提升其在锂离子电池阴极材料上的应用性能，另一方面其可通过煅烧-高温热处理合成其他的钛酸锂氧化物，如目前研究比较热的锂离子负极材料-Li4Ti5O12，一种结构稳定的“零应变”嵌入式材料，具有优异的循环性能，李伟，肖方明等人对LiTiO2在空气中600~900℃灼烧1~3h可得Li4Ti5O12，但截止目前为止，对于岩盐型LiTiO2纳米材料的研究并不多，而对于在相对较低温度下利用水热法制得纯度相对较高，颗粒尺寸较小的岩盐型LiTiO2纳米颗粒几乎没有。 In the application of lithium-ion batteries, on the one hand, the smaller rock-salt-type LiTiO 2 nanoparticles can improve their application performance in lithium-ion battery cathode materials to a certain extent due to the increase in their specific surface area; Calcination-high-temperature heat treatment to synthesize other lithium titanate oxides, such as Li 4 Ti 5 O 12 , a lithium-ion negative electrode material that is currently being studied, is a structurally stable "zero-strain" embedded material with excellent cycle performance. Li Wei, Xiao Fangming and others obtained Li 4 Ti 5 O 12 by burning LiTiO 2 in the air at 600-900°C for 1-3 hours, but so far, there are not many studies on rock-salt LiTiO 2 nanomaterials, and for There are almost no rock-salt-type LiTiO2 nanoparticles with relatively high purity and small particle size produced by hydrothermal method at relatively low temperature.
发明内容 Contents of the invention
本发明的目的在于提供一种工艺简单，过程易于控制的岩盐型LiTiO2纳米颗粒的制备方法。 The object of the present invention is to provide a method for preparing rock salt type LiTiO2 nanoparticles with simple process and easy process control.
本发明的岩盐型LiTiO2纳米颗粒的制备方法，包括以下步骤： Rock salt type LiTiO of the present invention The preparation method of nanoparticle may further comprise the steps:
1）将K2Ti6O13纳米纤维溶解于去离子水中，调节Ti4+的浓度为0.13~0.2mol/L； 1) Dissolve K 2 Ti 6 O 13 nanofibers in deionized water, and adjust the concentration of Ti 4+ to 0.13~0.2mol/L;
2）在搅拌状态下，向步骤1）制得的溶液中加入KOH，使得KOH浓度为8mol/L，得悬浊液； 2) Under stirring, add KOH to the solution prepared in step 1) so that the KOH concentration is 8mol/L to obtain a suspension;
3）搅拌状态下，向步骤2）所制备的悬浊液中加入硝酸锂，使得Li+的浓度为1.33~5.34mol/L,继续搅拌至少6h，得到用于水热反应的悬浊液； 3) Under stirring, add lithium nitrate to the suspension prepared in step 2), so that the concentration of Li + is 1.33~5.34mol/L, and continue stirring for at least 6 hours to obtain a suspension for hydrothermal reaction;
4）将步骤3）所得到的悬浊液转移到水热反应釜内胆中，用去离子水调节物料体积为反应釜容积的2/3~4/5，搅拌至少2h，其中Ti4+的摩尔浓度为0.1~0.15mol/L，Li+的摩尔浓度为1~4mol/L，KOH摩尔浓度为6mol/L，摩尔浓度的体积基数为前躯体浆料的总体积； 4) Transfer the suspension obtained in step 3) to the inner tank of the hydrothermal reactor, adjust the volume of the material to 2/3~4/5 of the volume of the reactor with deionized water, and stir for at least 2 hours, in which Ti 4+ The molar concentration of Li+ is 0.1~0.15mol/L, the molar concentration of Li + is 1~4mol/L, the molar concentration of KOH is 6mol/L, and the volume base of the molar concentration is the total volume of the precursor slurry;
5）将装有前驱体浆料的反应釜内胆置于反应釜中，密封，置于200℃~240℃保温16~64小时水热处理，然后，在空气中冷却，降至室温，取出反应产物，过滤，依次用去离子水、无水乙醇清洗，60~100℃烘干，得到岩盐型LiTiO2的纳米颗粒。 5) Put the liner of the reactor containing the precursor slurry in the reactor, seal it, and heat it at 200°C~240°C for 16~64 hours for hydrothermal treatment, then cool it in the air, drop it to room temperature, and take out the reaction The product is filtered, washed with deionized water and absolute ethanol in turn, and dried at 60-100°C to obtain rock salt-type LiTiO 2 nanoparticles.
上述的K2Ti6O13纳米纤维、硝酸锂、氢氧化钾、无水乙醇和去离子水的纯度均不低于化学纯。 The purity of the aforementioned K 2 Ti 6 O 13 nanofibers, lithium nitrate, potassium hydroxide, absolute ethanol and deionized water is not less than chemically pure.
本发明采用水热反应，以K2Ti6O13纳米纤维，硝酸锂为反应物料前躯体，利用矿化剂KOH促进晶化，在未引入表面修饰剂的情况下，制得形貌较规则，尺寸较小，物相较纯的岩盐型LiTiO2纳米颗粒。本发明制备过程中，对水热合成产物的清洗是为了去除硝酸根等水溶性离子。 The invention adopts hydrothermal reaction, uses K 2 Ti 6 O 13 nanofibers and lithium nitrate as the precursor of the reaction material, and utilizes the mineralizer KOH to promote the crystallization, and without the introduction of the surface modifier, the obtained morphology is more regular , smaller size, relatively pure rock-salt LiTiO 2 nanoparticles. In the preparation process of the present invention, the cleaning of the hydrothermal synthesis product is to remove water-soluble ions such as nitrate.
本发明制备工艺简单，易于控制，无污染，成本低，适于规模化生产。 The preparation process of the invention is simple, easy to control, pollution-free, low in cost and suitable for large-scale production.
附图说明 Description of drawings
图1是本发明制备的岩盐型LiTiO2纳米颗粒的XRD图谱； Fig. 1 is the rock-salt type LiTiO prepared by the present invention The XRD spectrum of nanoparticles;
图2是本发明制备的岩盐型LiTiO2纳米颗粒的扫描电镜照片。 Fig. 2 is the scanning electron micrograph of the rock-salt type LiTiO 2 nanoparticles prepared by the present invention.
具体实施方式 Detailed ways
以下结合实施例对本发明方法做进一步详细说明 Below in conjunction with embodiment the method of the present invention is described in further detail
实施例1： Example 1:
1）将1mmol K2Ti6O13纳米纤维溶解于去离子水中，调节Ti4+的浓度为0.2mol/L； 1) Dissolve 1mmol K 2 Ti 6 O 13 nanofibers in deionized water, and adjust the concentration of Ti 4+ to 0.2mol/L;
2）在搅拌状态下，向步骤1）制得的溶液中加入KOH，使得KOH浓度为8mol/L，得到悬浊液； 2) In the stirring state, add KOH to the solution prepared in step 1) so that the KOH concentration is 8mol/L to obtain a suspension;
3）在搅拌状态下，向步骤2）所制备的悬浊液中加入硝酸锂，使得Li+的浓度为1.33mol/L, 继续搅拌6h，得到用于水热反应的悬浊液； 3) Under stirring, add lithium nitrate to the suspension prepared in step 2), so that the concentration of Li + is 1.33mol/L, and continue stirring for 6 hours to obtain a suspension for hydrothermal reaction;
4）将步骤3）所得到的悬浊液转移到水热反应釜内胆中，用去离子水调节使其体积占反应釜容积的2/3，搅拌2h，其中Ti4+的摩尔浓度为0.15mol/L，Li+的摩尔浓度为1mol/L，KOH摩尔浓度为6mol/L，摩尔浓度的体积基数为前躯体浆料的总体积； 4) Transfer the suspension obtained in step 3) to the inner tank of the hydrothermal reaction kettle, adjust it with deionized water to make the volume account for 2/3 of the reaction kettle volume, stir for 2 hours, and the molar concentration of Ti 4+ is 0.15mol/L, the molar concentration of Li + is 1mol/L, the molar concentration of KOH is 6mol/L, and the volume base of the molar concentration is the total volume of the precursor slurry;
5）将装有前驱体浆料的反应釜内胆置于反应釜中，密封，置于200℃保温32小时水热处理，然后，在空气中冷却，降至室温，取出反应产物，过滤，依次用去离子水、无水乙醇清洗，在70℃烘干，得到岩盐型LiTiO2纳米颗粒。其XRD图如图1所示，由图可见，所制备的LiTiO2纳米颗粒为纯度较高的岩盐型物相，无其他杂相的存在。 5) Put the liner of the reaction kettle containing the precursor slurry in the reaction kettle, seal it, and heat it at 200°C for 32 hours for hydrothermal treatment, then cool it in the air, lower it to room temperature, take out the reaction product, filter, and then Wash with deionized water and absolute ethanol, and dry at 70°C to obtain rock salt-type LiTiO 2 nanoparticles. Its XRD pattern is shown in Figure 1. It can be seen from the figure that the prepared LiTiO 2 nanoparticles are rock-salt phases with high purity and no other impurity phases exist.
实施例2： Example 2:
1）将1mmol K2Ti6O13纳米纤维溶解于去离子水中，调节Ti4+的浓度为0.2mol/L； 1) Dissolve 1mmol K 2 Ti 6 O 13 nanofibers in deionized water, and adjust the concentration of Ti 4+ to 0.2mol/L;
2）在搅拌状态下，向步骤1）制得的悬浊液中加入KOH，使得KOH浓度为8mol/L，得到悬浊液； 2) Under stirring, add KOH to the suspension prepared in step 1) so that the KOH concentration is 8mol/L to obtain a suspension;
3）在搅拌状态下，向步骤2）所制备的悬浊液中加入硝酸锂，使得Li+的浓度为2.67mol/L, 继续搅拌12h，得到用于水热反应的悬浊液； 3) Under stirring, add lithium nitrate to the suspension prepared in step 2), so that the concentration of Li + is 2.67mol/L, and continue stirring for 12 hours to obtain a suspension for hydrothermal reaction;
4）将步骤3）所得到的悬浊液转移到水热反应釜内胆中，用去离子水调节使其体积占反应釜容积的4/5，搅拌2h，其中Ti4+的摩尔浓度为0.15mol/L, Li+的摩尔浓度为2mol/L，KOH摩尔浓度为6mol/L，摩尔浓度的体积基数为前躯体浆料的总体积； 4) Transfer the suspension obtained in step 3) to the liner of the hydrothermal reactor, adjust it with deionized water so that its volume accounts for 4/5 of the reactor volume, stir for 2 hours, and the molar concentration of Ti 4+ is 0.15mol/L, the molar concentration of Li + is 2mol/L, the molar concentration of KOH is 6mol/L, and the volume base of the molar concentration is the total volume of the precursor slurry;
5）将装有前驱体浆料的反应釜内胆置于反应釜中，密封，置于220℃保温16小时水热处理，然后，在空气中冷却，降至室温，取出反应产物，过滤，依次用去离子水、无水乙醇清洗，在80℃烘干，得到岩盐型LiTiO2纳米颗粒。其SEM图如图2所示，由图可见，所制备的LiTiO2纳米颗粒的形貌较规则。 5) Put the liner of the reaction kettle containing the precursor slurry in the reaction kettle, seal it, and heat it at 220°C for 16 hours for hydrothermal treatment, then cool it in the air, drop it to room temperature, take out the reaction product, filter, and then Wash with deionized water and absolute ethanol, and dry at 80°C to obtain rock salt-type LiTiO 2 nanoparticles. Its SEM image is shown in Figure 2. It can be seen from the figure that the morphology of the prepared LiTiO 2 nanoparticles is relatively regular.
实施例3： Example 3:
1）将0.67mmol K2Ti6O13纳米纤维溶解于去离子水中，调节Ti4+的浓度为0.13mol/L； 1) Dissolve 0.67mmol K 2 Ti 6 O 13 nanofibers in deionized water, and adjust the concentration of Ti 4+ to 0.13mol/L;
2）在搅拌状态下，向步骤1）制得的悬浊液中加入KOH，使得KOH浓度为8mol/L，得到悬浊液； 2) Under stirring, add KOH to the suspension prepared in step 1) so that the KOH concentration is 8mol/L to obtain a suspension;
3）在搅拌状态下，向步骤2）所制备的悬浊液中加入硝酸锂，使得Li+的浓度为4mol/L, 继续搅拌12h，得到用于水热反应的悬浊液； 3) Under stirring, add lithium nitrate to the suspension prepared in step 2), so that the concentration of Li + is 4mol/L, and continue stirring for 12 hours to obtain a suspension for hydrothermal reaction;
4）将步骤3）所得到的悬浊液转移到水热反应釜内胆中，用去离子水调节使其体积占反应釜容积的4/5，搅拌2h，其中Ti4+的摩尔浓度为0.1mol/L, Li+的摩尔浓度为3mol/L，KOH摩尔浓度为6mol/L，摩尔浓度的体积基数为前躯体浆料的总体积； 4) Transfer the suspension obtained in step 3) to the liner of the hydrothermal reactor, adjust it with deionized water so that its volume accounts for 4/5 of the reactor volume, stir for 2 hours, and the molar concentration of Ti 4+ is 0.1mol/L, the molar concentration of Li + is 3mol/L, the molar concentration of KOH is 6mol/L, and the volume base of the molar concentration is the total volume of the precursor slurry;
5）将装有前驱体浆料的反应釜内胆置于反应釜中，密封，置于240℃保温24小时水热处理，然后，在空气中冷却，降至室温，取出反应产物，过滤，依次用去离子水、无水乙醇清洗，在100℃烘干，得到岩盐型LiTiO2纳米颗粒。 5) Put the liner of the reaction kettle with the precursor slurry in the reaction kettle, seal it, and heat it at 240°C for 24 hours for hydrothermal treatment, then cool it in the air, drop it to room temperature, take out the reaction product, filter, and then Wash with deionized water and absolute ethanol, and dry at 100°C to obtain rock salt-type LiTiO 2 nanoparticles.
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| CN1416190A (en) * | 2002-11-05 | 2003-05-07 | 南开大学 | Chemical compound batteries with embedded lithium ferrate-lithium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1416190A (en) * | 2002-11-05 | 2003-05-07 | 南开大学 | Chemical compound batteries with embedded lithium ferrate-lithium |
| CN103290426A (en) * | 2013-07-12 | 2013-09-11 | 广州有色金属研究院 | Preparation method of lithium titanate |
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| Title |
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| 唐定国等.直接水热法合成钛酸锂.《中南民族大学学报(自然科学版)》.2009,第28卷(第4期),第9-13页. * |
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