CN109950525B - Hair belly-shaped Nb2O5Preparation method of lithium ion battery electrode material - Google Patents
Hair belly-shaped Nb2O5Preparation method of lithium ion battery electrode material Download PDFInfo
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 30
- 239000007772 electrode material Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000012153 distilled water Substances 0.000 claims abstract description 24
- 239000002244 precipitate Substances 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 10
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000005642 Oleic acid Substances 0.000 claims abstract description 10
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 8
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 8
- 239000008103 glucose Substances 0.000 claims abstract description 8
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 8
- XNHGKSMNCCTMFO-UHFFFAOYSA-D niobium(5+);oxalate Chemical compound [Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XNHGKSMNCCTMFO-UHFFFAOYSA-D 0.000 claims abstract description 8
- 238000001556 precipitation Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 11
- 238000004108 freeze drying Methods 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 7
- 210000001015 abdomen Anatomy 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 238000009827 uniform distribution Methods 0.000 abstract description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 239000007773 negative electrode material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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Abstract
一种毛肚状的Nb2O5锂离子电池电极材料的制备方法，首先将分析纯的水合草酸铌加入蒸馏水中得到A；然后将葡萄糖加入蒸馏水中得B；将A和B混合得混合液C；将混合液C在均相反应仪中水热反应后冷却至室温得沉淀；将所得的沉淀物在真空干燥箱中干燥得到前驱物D；取前驱物D加入蒸馏水中得溶液E；再取三聚氰胺加入到油酸中得到溶液F；将溶液E和溶液F混合进行二次水热反应自然冷却至室温后沉淀；将所得的沉淀物冷冻干燥得毛肚状的Nb2O5锂离子电池电极材料。本发明采用二次水热的方法，制备出结晶性较好，分布均匀的毛肚状Nb2O5纳米材料，采用不同的油酸添加量，将其作为碳源和表面活性剂，可以利于调控所制备材料的结构及形貌，工艺简单，成本低廉。A method for preparing a hairy belly-shaped Nb 2 O 5 lithium ion battery electrode material, firstly adding analytically pure hydrated niobium oxalate into distilled water to obtain A; then adding glucose into distilled water to obtain B; mixing A and B to obtain a mixed solution C; the mixed solution C is hydrothermally reacted in a homogeneous reactor and then cooled to room temperature to obtain a precipitate; the obtained precipitate is dried in a vacuum drying oven to obtain a precursor D; the precursor D is added to distilled water to obtain a solution E; Take melamine and add it to oleic acid to obtain solution F; mix solution E and solution F for secondary hydrothermal reaction and naturally cool down to room temperature for precipitation; freeze-dry the resulting precipitate to obtain a hairy Nb 2 O 5 lithium ion battery electrode material. The invention adopts the secondary hydrothermal method to prepare the hairy belly-like Nb 2 O 5 nanomaterials with good crystallinity and uniform distribution, and uses different oleic acid addition amounts as carbon sources and surfactants, which can be beneficial to the The structure and morphology of the prepared material are regulated, the process is simple, and the cost is low.
Description
技术领域technical field
本发明属于电池材料技术领域，涉及一种制备锂离子电池负极材料的制备方法，具体涉及一种毛肚状的Nb2O5锂离子电池电极材料的制备方法。The invention belongs to the technical field of battery materials, relates to a preparation method for preparing a negative electrode material for a lithium ion battery, and in particular relates to a preparation method for a hairy belly - shaped Nb2O5 lithium ion battery electrode material.
背景技术Background technique
由于科技的发展和进步，煤、石油和天然气等一次能源出现危机，开发新能源广受关注。锂离子电池作为实现电能和化学能互相转化的装置，随着民用电子产品数量和质量的提高，其作为一种清洁能源，已被大规模应用于现代生活中。Due to the development and progress of science and technology, primary energy sources such as coal, oil and natural gas are in crisis, and the development of new energy sources has attracted wide attention. As a device for realizing the mutual conversion of electrical energy and chemical energy, lithium-ion batteries have been widely used in modern life as a clean energy with the improvement of the quantity and quality of civilian electronic products.
目前，市场上开发了很多过渡金属氧化物用作锂离子电池电极材料，它们大部分发生合金化反应和转化反应，伴随着很大的体积膨胀，而Nb2O5作为过渡金属氧化物之一，它发生插层反应[Augustyn V,Come J,Lowe M,et al.High-rate electrochemical energystorage through Li+intercalation pseudocapacitance.Nature Materials,2013,12(6): 518-522]，体积膨胀较小。Kent J.Griffith等[Griffith K,Forse A,Griffin J,etal.High-rate intercalation without nanostructuring in metastable Nb2O5 bronzephases.Journal of the American Chemical Society,2016,138(28):8888-8899]利用煅烧法制备了四种不同晶型的Nb2O5，有TT相，T相，B相和H相。文献记载[Zeng G,Wang H,GuoJ,et al. Fabrication of Nb2O5/C nanocomposites as a high performance anode forlithium ion battery. Chinese Chemical Letters,2017,28(4):755-758]了T相Nb2O5具有赝电容行为，由于其 (001)的晶面间距为
目前已有的办法并没有很大程度提高Nb2O5本身的导电性，从而提高其作为锂离子电池负极材料的放电比容量。并且已有的制备方法过程复杂繁琐，成本高昂，因此，开发一种低成本、反应周期短的制备Nb2O5电极的方法，这具有很大的研究意义。The existing methods have not greatly improved the conductivity of Nb 2 O 5 itself, so as to improve its specific discharge capacity as a negative electrode material for lithium ion batteries. In addition, the existing preparation methods are complicated and expensive, so it is of great research significance to develop a method for preparing Nb 2 O 5 electrodes with low cost and short reaction period.
发明内容SUMMARY OF THE INVENTION
本发明的目的在于提供一种制备成本低廉，样品形貌特殊的毛肚状的Nb2O5锂离子电池电极材料的制备方法，按本发明的制备方法能够制备出分散均匀、结构稳定的毛肚状Nb2O5锂离子电池电极材料，且此电极材料表现出很高的放电比容量。The object of the present invention is to provide a method for preparing a Nb 2 O 5 lithium ion battery electrode material with low preparation cost and special sample morphology, which has the shape of a hairy belly. Belly-shaped Nb 2 O 5 lithium ion battery electrode material, and this electrode material shows a high specific discharge capacity.
为达到上述目的，本发明采用的技术方案是：To achieve the above object, the technical scheme adopted in the present invention is:
1)首先将0.60～1.0g分析纯的水合草酸铌加入30ml蒸馏水中搅拌均匀，得到透明溶液A；1) First, add 0.60-1.0 g of analytically pure hydrated niobium oxalate into 30 ml of distilled water and stir to obtain a transparent solution A;
2)然后将1.2～2.0g的葡萄糖加入30ml蒸馏水中搅拌均匀，得到透明溶液B；2) Then add 1.2-2.0 g of glucose into 30 ml of distilled water and stir to obtain a transparent solution B;
3)将溶液A和溶液B混合，然后超声分散得混合液C；3) Mix solution A and solution B, then ultrasonically disperse to obtain mixed solution C;
4)将混合液C加入到反应釜中，密封好后在均相反应仪中于120～160℃水热反应，反应结束后自然冷却至室温后沉淀；4) The mixed solution C is added to the reactor, and after being sealed, it is hydrothermally reacted in a homogeneous reactor at 120 to 160 ° C, and the reaction is naturally cooled to room temperature and then precipitated;
5)将步骤4)所得的沉淀物分别水洗、醇洗后在真空干燥箱中干燥得到前驱物D；5) the precipitate obtained in step 4) is washed with water and alcohol, respectively, and dried in a vacuum drying oven to obtain precursor D;
6)取1.0～1.8g的前驱物D加入30ml蒸馏水中搅拌均匀，得到悬浮液E；6) Add 1.0-1.8 g of precursor D into 30 ml of distilled water and stir to obtain suspension E;
7)再取0.2～0.6g的三聚氰胺加入到30～60ml油酸中，搅拌均匀，得到溶液F；7) Take 0.2～0.6g of melamine and add it to 30～60ml of oleic acid, stir evenly to obtain solution F;
8)将悬浮液E和溶液F混合，搅拌均匀，加入到反应内釜中，于160～200℃进行二次水热反应，反应结束后自然冷却至室温后沉淀；8) Mix suspension E and solution F, stir evenly, add to the inner reactor, carry out secondary hydrothermal reaction at 160～200 ℃, after the reaction finishes, naturally cool to room temperature for precipitation;
9)将步骤8)所得的沉淀物分别水洗、醇洗后在冷冻干燥箱中干燥得毛肚状的Nb2O5锂离子电池电极材料。9) Wash the precipitate obtained in step 8) with water and alcohol, respectively, and then dry it in a freeze-drying oven to obtain a hairy Nb 2 O 5 lithium ion battery electrode material.
所述步骤3)超声分散时间为20～60min。The step 3) ultrasonic dispersion time is 20～60min.
所述步骤4)混合液C加入到反应釜的填充比为30～60％。Described step 4) the filling ratio that mixed solution C is added to the reaction kettle is 30～60%.
所述步骤4)水热反应时间为12～24h。The step 4) hydrothermal reaction time is 12～24h.
所述步骤5)真空干燥箱的干燥温度为60～80℃。In the step 5), the drying temperature of the vacuum drying oven is 60-80°C.
所述步骤8)水热反应时间为12～24h。The step 8) hydrothermal reaction time is 12～24h.
所述步骤9)冷冻干燥温度为-40～-30℃，干燥时间为8～12h。The step 9) freeze-drying temperature is -40～-30 ℃, and drying time is 8～12h.
本发明采用二次水热的方法，制备出结晶性较好，分布均匀的毛肚状Nb2O5纳米材料，采用不同的油酸添加量，将其作为碳源和表面活性剂，可以利于调控所制备材料的结构及形貌，工艺简单，成本低廉。The invention adopts the secondary hydrothermal method to prepare the hairy belly-like Nb 2 O 5 nanomaterials with good crystallinity and uniform distribution, and uses different oleic acid addition amounts as carbon sources and surfactants, which can be beneficial to the The structure and morphology of the prepared material are regulated, the process is simple, and the cost is low.
附图说明Description of drawings
图1是本发明实施例1制备的毛肚状的Nb2O5锂离子电池电极材料的XRD图谱。FIG. 1 is the XRD pattern of the hairy belly-shaped Nb 2 O 5 lithium ion battery electrode material prepared in Example 1 of the present invention.
图2是本发明实施例1制备的毛肚状的Nb2O5锂离子电池电极材料的SEM照片。2 is a SEM photograph of the hairy belly-shaped Nb 2 O 5 lithium ion battery electrode material prepared in Example 1 of the present invention.
图3是本发明实施例1制备的毛肚状的Nb2O5锂离子电池电极材料的循环性能图片。3 is a picture of cycle performance of the hairy belly-shaped Nb 2 O 5 lithium ion battery electrode material prepared in Example 1 of the present invention.
具体实施方式Detailed ways
下面结合实施例对本发明作进一步详细说明。The present invention will be described in further detail below in conjunction with the examples.
实施例1：Example 1:
1)首先将0.6g分析纯的水合草酸铌加入30ml蒸馏水中搅拌均匀，得到透明溶液A；1) First, add 0.6 g of analytically pure hydrated niobium oxalate into 30 ml of distilled water and stir to obtain a transparent solution A;
2)然后将1.2g的葡萄糖加入30ml蒸馏水中搅拌均匀，得到透明溶液B；2) Then add 1.2g of glucose into 30ml of distilled water and stir to obtain transparent solution B;
3)将溶液A和溶液B混合，然后超声分散20min得混合液C；3) Mix solution A and solution B, then ultrasonically disperse for 20min to obtain mixed solution C;
4)按30％的填充比将混合液C加入到反应釜中，密封好后在均相反应仪中于120℃水热反应24h，反应结束后自然冷却至室温后沉淀；4) The mixed solution C was added to the reaction kettle at a filling ratio of 30%, and after sealing, it was hydrothermally reacted in a homogeneous reactor at 120 ° C for 24 hours, and after the reaction was finished, it was naturally cooled to room temperature and precipitated;
5)将步骤4)所得的沉淀物分别水洗、醇洗后在真空干燥箱中于70℃干燥得到前驱物D；5) The precipitate obtained in step 4) was washed with water and alcohol, respectively, and dried in a vacuum drying oven at 70° C. to obtain precursor D;
6)取1.8g的前驱物D加入30ml蒸馏水中搅拌均匀，得到溶液E；6) get 1.8g of precursor D and add it to 30ml of distilled water and stir to obtain solution E;
7)再取0.6g的三聚氰胺加入到60ml油酸中，搅拌均匀，得到溶液F；7) Take 0.6g of melamine and add it to 60ml of oleic acid, stir evenly to obtain solution F;
8)将溶液E和溶液F混合，搅拌均匀，加入到反应内釜中，于160℃进行二次水热反应24h，反应结束后自然冷却至室温后沉淀；8) Mix solution E and solution F, stir evenly, add to the inner reaction kettle, carry out a secondary hydrothermal reaction at 160 ° C for 24 hours, after the reaction is completed, it is naturally cooled to room temperature and precipitated;
9)将步骤8)所得的沉淀物分别水洗、醇洗后在冷冻干燥箱中于-40℃干燥8h 得毛肚状的Nb2O5锂离子电池电极材料。9) Wash the precipitate obtained in step 8) with water and alcohol respectively, and then dry it in a freeze-drying oven at -40° C. for 8 hours to obtain a hairy Nb 2 O 5 lithium ion battery electrode material.
从图1中可看出采用本发明成功制备出了T-Nb2O5。可以看到其衍射峰对应着(001)、(180)、(181)、(002)、(380)和(202)晶面，说明样品是纯粹的T-Nb2O5。It can be seen from Fig. 1 that T-Nb 2 O 5 is successfully prepared by the present invention. It can be seen that the diffraction peaks correspond to (001), (180), (181), (002), (380) and (202) crystal planes, indicating that the sample is pure T-Nb 2 O 5 .
从图2中可看出，所制备的毛肚状Nb2O5分散均匀，可以清晰看出很多小棒长在片上，像毛肚的形状。It can be seen from Figure 2 that the prepared hairy belly-like Nb 2 O 5 is evenly dispersed, and it can be clearly seen that many small rods grow on the sheet, like the shape of hairy belly.
图3是实施例1制备的毛肚状Nb2O5纳米材料的循环性能图片(电流密度100 mA/g)。在电流密度为100mA/g下，产物的比容量达到为375mAh/g，并且循环40 圈后，Nb2O5电极的比容量还具有上升的趋势。故将Nb2O5作为锂离子电池负极材料时，其表现出很高的放电比容量以及良好的可逆性。3 is a picture of the cycle performance of the hairy belly-like Nb 2 O 5 nanomaterial prepared in Example 1 (
实施例2：Example 2:
1)首先将0.7g分析纯的水合草酸铌加入30ml蒸馏水中搅拌均匀，得到透明溶液A；1) First, add 0.7 g of analytically pure hydrated niobium oxalate to 30 ml of distilled water and stir to obtain a transparent solution A;
2)然后将1.4g的葡萄糖加入30ml蒸馏水中搅拌均匀，得到透明溶液B；2) Then add 1.4g of glucose into 30ml of distilled water and stir to obtain transparent solution B;
3)将溶液A和溶液B混合，然后超声分散30min得混合液C；3) Mix solution A and solution B, then ultrasonically disperse for 30min to obtain mixed solution C;
4)按50％的填充比将混合液C加入到反应釜中，密封好后在均相反应仪中于150℃水热反应15h，反应结束后自然冷却至室温后沉淀；4) The mixed solution C was added to the reaction kettle at a filling ratio of 50%, and after sealing, it was hydrothermally reacted in a homogeneous reactor at 150 ° C for 15 hours, and after the reaction was finished, it was naturally cooled to room temperature and precipitated;
5)将步骤4)所得的沉淀物分别水洗、醇洗后在真空干燥箱中于60℃干燥得到前驱物D；5) the precipitate obtained in step 4) was washed with water and alcohol, respectively, and dried in a vacuum drying oven at 60° C. to obtain precursor D;
6)取1.6g的前驱物D加入30ml蒸馏水中搅拌均匀，得到溶液E；6) get 1.6g of precursor D, add 30ml of distilled water and stir to obtain solution E;
7)再取0.5g的三聚氰胺加入到50ml油酸中，搅拌均匀，得到溶液F；7) Take 0.5g of melamine and add it to 50ml of oleic acid, stir evenly to obtain solution F;
8)将溶液E和溶液F混合，搅拌均匀，加入到反应内釜中，于170℃进行二次水热反应21h，反应结束后自然冷却至室温后沉淀；8) Mix the solution E and the solution F, stir evenly, add it to the inner reaction kettle, carry out a secondary hydrothermal reaction at 170 ° C for 21 h, and then naturally cool to room temperature and precipitate after the reaction;
9)将步骤8)所得的沉淀物分别水洗、醇洗后在冷冻干燥箱中于-30℃干燥12h 得毛肚状的Nb2O5锂离子电池电极材料。9) Wash the precipitate obtained in step 8) with water and alcohol respectively, and then dry it in a freeze-drying oven at -30° C. for 12 hours to obtain a hairy Nb 2 O 5 lithium ion battery electrode material.
实施例3：Example 3:
1)首先将0.8g分析纯的水合草酸铌加入30ml蒸馏水中搅拌均匀，得到透明溶液A；1) First, add 0.8 g of analytically pure hydrated niobium oxalate into 30 ml of distilled water and stir to obtain a transparent solution A;
2)然后将1.6g的葡萄糖加入30ml蒸馏水中搅拌均匀，得到透明溶液B；2) Then add 1.6g of glucose into 30ml of distilled water and stir to obtain transparent solution B;
3)将溶液A和溶液B混合，然后超声分散40min得混合液C；3) Mix solution A and solution B, then ultrasonically disperse for 40min to obtain mixed solution C;
4)按60％的填充比将混合液C加入到反应釜中，密封好后在均相反应仪中于16℃水热反应12h，反应结束后自然冷却至室温后沉淀；4) The mixed solution C was added to the reaction kettle at a filling ratio of 60%, and after being sealed, it was hydrothermally reacted in a homogeneous reactor at 16 °C for 12 hours, and after the reaction was completed, it was naturally cooled to room temperature and precipitated;
5)将步骤4)所得的沉淀物分别水洗、醇洗后在真空干燥箱中于80℃干燥得到前驱物D；5) the precipitate obtained in step 4) was washed with water and alcohol, respectively, and dried in a vacuum drying oven at 80° C. to obtain precursor D;
6)取1.4g的前驱物D加入30ml蒸馏水中搅拌均匀，得到溶液E；6) get 1.4g of precursor D, add 30ml of distilled water and stir to obtain solution E;
7)再取0.4g的三聚氰胺加入到45ml油酸中，搅拌均匀，得到溶液F；7) Take 0.4g of melamine and add it to 45ml of oleic acid, stir evenly to obtain solution F;
8)将溶液E和溶液F混合，搅拌均匀，加入到反应内釜中，于180℃进行二次水热反应18h，反应结束后自然冷却至室温后沉淀；8) Mix solution E and solution F, stir evenly, add to the inner reaction kettle, conduct secondary hydrothermal reaction at 180 ° C for 18 hours, and then naturally cool to room temperature and precipitate after the reaction;
9)将步骤8)所得的沉淀物分别水洗、醇洗后在冷冻干燥箱中于-35℃干燥10h 得毛肚状的Nb2O5锂离子电池电极材料。9) Wash the precipitate obtained in step 8) with water and alcohol, respectively, and then dry it in a freeze-drying oven at -35° C. for 10 hours to obtain a hairy Nb 2 O 5 lithium ion battery electrode material.
实施例4：Example 4:
1)首先将0.9g分析纯的水合草酸铌加入30ml蒸馏水中搅拌均匀，得到透明溶液A；1) First, add 0.9 g of analytically pure hydrated niobium oxalate into 30 ml of distilled water and stir to obtain a transparent solution A;
2)然后将1.8g的葡萄糖加入30ml蒸馏水中搅拌均匀，得到透明溶液B；2) Then add 1.8g of glucose into 30ml of distilled water and stir to obtain transparent solution B;
3)将溶液A和溶液B混合，然后超声分散50min得混合液C；3) Mix solution A and solution B, then ultrasonically disperse for 50min to obtain mixed solution C;
4)按40％的填充比将混合液C加入到反应釜中，密封好后在均相反应仪中于130℃水热反应20h，反应结束后自然冷却至室温后沉淀；4) The mixed solution C was added to the reaction kettle at a filling ratio of 40%, and after sealing, hydrothermally reacted in a homogeneous reactor at 130° C. for 20 hours, and after the reaction was finished, it was naturally cooled to room temperature and precipitated;
5)将步骤4)所得的沉淀物分别水洗、醇洗后在真空干燥箱中于65℃干燥得到前驱物D；5) the precipitate obtained in step 4) was washed with water and alcohol, respectively, and dried in a vacuum drying oven at 65° C. to obtain precursor D;
6)取1.2g的前驱物D加入30ml蒸馏水中搅拌均匀，得到溶液E；6) get 1.2g of precursor D and add it to 30ml of distilled water and stir to obtain solution E;
7)再取0.3g的三聚氰胺加入到40ml油酸中，搅拌均匀，得到溶液F；7) Take 0.3g of melamine and add it to 40ml of oleic acid, stir evenly to obtain solution F;
8)将溶液E和溶液F混合，搅拌均匀，加入到反应内釜中，于190℃进行二次水热反应15h，反应结束后自然冷却至室温后沉淀；8) Mix solution E and solution F, stir evenly, add to the inner reaction kettle, carry out a secondary hydrothermal reaction at 190 ° C for 15 h, after the reaction is completed, it is naturally cooled to room temperature and precipitated;
9)将步骤8)所得的沉淀物分别水洗、醇洗后在冷冻干燥箱中于-40℃干燥11h 得毛肚状的Nb2O5锂离子电池电极材料。9) Wash the precipitate obtained in step 8) with water and alcohol respectively, and then dry it in a freeze-drying oven at -40° C. for 11 hours to obtain a hairy Nb 2 O 5 lithium ion battery electrode material.
实施例5：Example 5:
1)首先将1.0g分析纯的水合草酸铌加入30ml蒸馏水中搅拌均匀，得到透明溶液A；1) First, add 1.0 g of analytically pure hydrated niobium oxalate to 30 ml of distilled water and stir to obtain a transparent solution A;
2)然后将2.0g的葡萄糖加入30ml蒸馏水中搅拌均匀，得到透明溶液B；2) Then add 2.0g of glucose into 30ml of distilled water and stir to obtain transparent solution B;
3)将溶液A和溶液B混合，然后超声分散60min得混合液C；3) Mix solution A and solution B, then ultrasonically disperse for 60min to obtain mixed solution C;
4)按50％的填充比将混合液C加入到反应釜中，密封好后在均相反应仪中于140℃水热反应18h，反应结束后自然冷却至室温后沉淀；4) The mixed solution C was added to the reaction kettle at a filling ratio of 50%, and after sealing, it was hydrothermally reacted in a homogeneous reactor at 140 ° C for 18 hours, and after the reaction was finished, it was naturally cooled to room temperature and precipitated;
5)将步骤4)所得的沉淀物分别水洗、醇洗后在真空干燥箱中于75℃干燥得到前驱物D；5) The precipitate obtained in step 4) was washed with water and alcohol, respectively, and dried in a vacuum drying oven at 75° C. to obtain precursor D;
6)取1.0g的前驱物D加入30ml蒸馏水中搅拌均匀，得到溶液E；6) get 1.0g of precursor D, add 30ml of distilled water and stir to obtain solution E;
7)再取0.2g的三聚氰胺加入到30ml油酸中，搅拌均匀，得到溶液F；7) Take 0.2g of melamine and add it to 30ml of oleic acid, stir evenly to obtain solution F;
8)将溶液E和溶液F混合，搅拌均匀，加入到反应内釜中，于200℃进行二次水热反应12h，反应结束后自然冷却至室温后沉淀；8) Mix solution E and solution F, stir evenly, add it to the inner reaction kettle, carry out a secondary hydrothermal reaction at 200 ° C for 12 hours, and then naturally cool to room temperature and precipitate after the reaction;
9)将步骤8)所得的沉淀物分别水洗、醇洗后在冷冻干燥箱中于-30℃干燥9h 得毛肚状的Nb2O5锂离子电池电极材料。9) Wash the precipitate obtained in step 8) with water and alcohol respectively, and then dry it in a freeze-drying oven at -30° C. for 9 hours to obtain a hairy Nb 2 O 5 lithium ion battery electrode material.
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