CN102583574A - Cathode material, alpha-Fe2O3, of high-capacity lithium ion battery and preparation method for material - Google Patents
Cathode material, alpha-Fe2O3, of high-capacity lithium ion battery and preparation method for material Download PDFInfo
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- CN102583574A CN102583574A CN2012100612475A CN201210061247A CN102583574A CN 102583574 A CN102583574 A CN 102583574A CN 2012100612475 A CN2012100612475 A CN 2012100612475A CN 201210061247 A CN201210061247 A CN 201210061247A CN 102583574 A CN102583574 A CN 102583574A
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Abstract
The invention relates to a cathode material, alpha-Fe2O3, of a high-capacity lithium ion battery and a preparation method for the cathode material. According to the preparation method, soluble trivalent molysite and an alkali metal hydroxide easy to dissolve are adopted as raw materials, and the hematite alpha-Fe2O3 is prepared by a hydrothermal method. The preparation method comprises the following specific steps that: 1) aqueous solution of the trivalent molysite with molarity being 0.5mol/L-2mol/L and aqueous solution of the alkali metal hydroxide easy to dissolve with molarity being 2mol/L-6mol/L are prepared; 2) the aqueous solution of the trivalent molysite and the aqueous solution of the alkali metal hydroxide obtained in the step 1) are mixed to generate suspension, the suspension is stirred for certain time, and then ammonia water drops into the suspension, so that the pH value of the suspension is adjusted to be 9-13; and 3) the suspension obtained in the step 2) is poured into a hydrothermal reaction kettle which can be airtight, the hydrothermal reaction kettle is put into an oven to be heated at a temperature of 160 DEG C-200 DEG C and then is subjected to thermal insulation for 3 hours to 20 hours, and after the reaction is finished, a product is subjected to solid-liquid separation, washing and drying so as to obtain the alpha-Fe2O3. When serving as the cathode material of the lithium ion battery, the alpha-Fe2O3 prepared by the method has higher specific capacity and better cycling stability. According to the method, the operation is simple, the cost is low, additives are not required, and the product quality is stable.
Description
Technical field
The invention belongs to electrochemical field at this, be specifically related to a kind of high capacity type lithium ion battery negative material α-Fe
2O
3And preparation method thereof.
Background technology
Lithium ion battery becomes present good comprehensive properties battery system because of it has excellent characteristic; Along with its Application Areas from civilian information industry (high-performance portable electronicss such as mobile telephone, notebook computer) to the further expanding of energy traffic (electromobile etc.), the capacity and the fast charging and discharging ability of lithium ion battery are all had higher requirement.Negative material is one of key factor of decision lithium ion battery over-all properties.At present, the commercialization lithium ion battery negative material still the graphite-like negative pole be main, but it exists specific storage low, multiplying power discharging property is poor, is easy to generate the problems such as deposition of metallic lithium in the charge and discharge process, thereby can cause certain potential safety hazard.Therefore, try to explore the specific storage height, the capacity attenuation rate is little, the rate charge-discharge performance is good and safe new type lithium ion battery negative material system has become the focus of research in the world.The research at present heavy body negative pole of heat mainly comprises alloy type negative pole and oxide-based negative pole
[1-6]But because of alloy type such as silicon-based anode material volume change high about 400% in the removal lithium embedded process; Cycle performance is very poor, influenced its practical application, and transition metal oxide is because of having very high theoretical specific capacity; The smaller volume rate of expansion is more promising one type of negative material relatively.
Wherein, α
-Fe
2O
3Because of specific storage is high, cost is low, and good stability is free from environmental pollution and receive people's great attention [7-19].Consult pertinent literature and find that hydrothermal method synthesizing submicron lithium ion battery is used negative material α
-Fe
2O
3Become one of main stream approach, hydrothermal method technology makes active material particle contact reacts in liquid phase, and crystallization nucleation is also grown up, and can obtain the α that particle diameter is little, be evenly distributed and do not reunite
-Fe
2O
3, the α of this method preparation
-Fe
2O
3Pattern is abundanter, can regulate and control, and chemical property is good.But most articles of report all control the granule-morphology and the size distribution of product through adding tensio-active agent, also do not find about Hydrothermal Preparation lithium ion battery negative material α at present
-Fe
2O
3Patent, so the present invention has prepared submicron order and finely disseminated globular under the situation of not adding any tensio-active agent
-Fe
2O
3, and with it as lithium ion battery negative material, find that it shows very high electrochemical specific capacity, have as the potentiality of large vol energy storage with lithium ion battery negative material.
Reference
[1] Poizot?P,?Laruelle?S,?Grugeon?S,?Dupont?L,?Tarascon?JM.?Nature?2000;407:496-9.
[2] Wang?L,?Xu?HW,?Chen?PC,?Zhang?DW,?Ding?CX,?Chen?CH.?J?Power?Sources?2009;193:846-50.
[3] Rahman?MM,?Wang?JZ,?Deng?XL,?Li?Y,?Liu?HK.?Electrochim?Acta?2009;55:504-10.
[4]?Xiang?JY,?Tua?JP,?Yuan?YF,?Wang?XL,?Huang?XH,?Zeng?ZY.?Electrochim?Acta?2009;54:1160-5.
[5]?Ji?LW,?Zhang?XW.?Electrochem?Commun?2009;11:795-8.
[6]?Huang?XH,?Tu?JP,?Xia?XH,?Wang?XL,?Xiang?JY,?Zhang?L,?et?al.?J?Power?Sources?2009;188:588-91.
[7]?Morimoto?H,?Tobishima?S,?Iizuka?Y.?J?Power?Sources?2005;146:315-8.
[8]?Yu?WJ,?Hou?PX,?Zhang?LL,?Li?F,?Liu?C,?Cheng?HM.?Chem?Commun?2010;46:8576-8.
[9]?Wang?PC,?Ding?HP,?Bark?T,?Chen?CH.?Electrochim?Acta?2007;52:6650-5.
[10]?NuLi?Y,?Zhang?P,?Guo?ZP,?Munroe?P,?Liu?HK.?Electrochim?Acta?2008;53:4213-8.
[11]?Zhang?P,?Guo?ZP,?Liu?HK.?Electrochim?Acta?2010;55:8521-6.
[12]?Nagao?M,?Otani?M,?Tomita?H,?Kanzaki?S,?Yamada?A,?Kanno?R.?J?Power?Sources?2011;196:4741-6.
[13]?Hu?XL,?Yu?JC,?Gong?JM,?Li?Q,?Li?GS.?Adv?Mater?2007;19:2324-9.
[14]?Zheng?YH,?Cheng?Y,?Wang?YS,?Bao?F,?Zhou?LH,?Wei?XF,?et?al.?J?Phy?Chem?B?2006;110:3093-7.
[15]?Zhu?WC,?Cui?XL,?Wang?L,?Liu?T,?Zhang?Q.?Mater?Lett?2011;65:1003-6.
[16]?Wu?ZC,?Yu?K,?Zhang?SD,?Xie?Y.?J?Phy?Chem?C?2008;112:11307—13.
[17]?Zhu?LP,?Liao?GH,?Bing?NC,?Zhao?X,?Gu?YY.?Mater?Lett?2011;65:1287-90.
[18]?Liu?H,?Wexler?D,?Wang?GX.?J?Alloy?Compd?2009;487:L24-7.
[19]?Tong?GX,?Guan?JG,?Wu?WH,?Li?LC,?Guan?Y,?Hua?Q.?Sci?China?Technol?Sc?2010;53:1897-903。
Summary of the invention
The purpose of this invention is to provide the simple and hydrothermal method that need not any surfactant additive of a kind of technology and prepare high capacity type lithium ion battery negative material α-Fe
2O
3Sub-micron ball.
Preparation α provided by the invention
-Fe
2O
3Method comprise the steps:
1) adopting deionized water is solvent, and disposing volumetric molar concentration respectively is the trivalent iron salt aqueous solution of 0.5-2 mol/L and the processable alkali metal hydroxide aqueous solution that volumetric molar concentration is 2-6 mol/L;
2) step 1) gained alkali metal hydroxide aqueous solution is poured in the trivalent iron salt aqueous solution reacted, the suspension-s of formation stirs certain hour and also regulates pH value to 9 ~ 13;
3) with step 2) the gained mixing solutions pours in the sealable reactor drum, places baking oven to be heated to 160-220 ℃ and be incubated 3-20 hour, and reaction is carried out solid-liquid separation after finishing, is washed, is drying to obtain said α
-Fe
2O
3
In the step 1) of aforesaid method, at least a in the muriate of the nitrate salt of said solubility trivalent iron salt chosen from Fe, the vitriol of iron, iron and the acetate of iron; The volumetric molar concentration of the said solubility trivalent iron salt aqueous solution is 0.5-2 mol/L; Said easy capacitive alkali metal hydroxide is selected from least a in Lithium Hydroxide MonoHydrate, sodium hydroxide, Pottasium Hydroxide and the hydrated barta; The volumetric molar concentration of said easy capacitive alkali metal hydroxide aqueous solution is 2-6 mol/L.
Said step 2) in, the ratio of the amount of substance of said solubility trivalent iron salt and easy capacitive alkali metal hydroxide is 1
:3; In the said adjusting pH value step, regulator is ammoniacal liquor or potassium hydroxide aqueous solution, and the mass percentage concentration of said ammoniacal liquor or potassium hydroxide aqueous solution is 25-28%.
In the said step 3), hydrothermal temperature is 160-220 ℃, and the hydro-thermal reaction time is 3-20 hour; Drying temperature is 80-120 ℃, and be 8-12 hour time of drying.
The α for preparing according to the method described above
-Fe
2O
3Negative active core-shell material mainly as lithium ion battery.
Compare with other existing methods, the present invention has following characteristics:
1) concentration of employed solubility trivalent iron salt concentration and processable alkali hydroxide soln is all adjustable in the inventive method, moreover this method do not add any tensio-active agent, reduces cost and free from environmental pollution.
2) lithium ion battery negative material α provided by the invention
-Fe
2O
3Hydrothermal preparing process be to separate out Fe (OH) through trivalent iron salt and alkaline reaction
3Deposition, it decomposes and accomplishes under hydrothermal condition then, has that energy consumption is low, productive rate is high, the easy to operate controlled and advantage being convenient to accomplish scale production.
3) the starting material wide material sources that the present invention adopted, with low cost, hydrothermal temperature is lower, and the time is shorter.
4) the lithium ion battery negative material α of the present invention's preparation
-Fe
2O
3Complete in crystal formation, particle size is little, and grain morphology rule and being evenly distributed shows higher electrochemical specific capacity and good cyclical stability, still has 1167 mAh/g after the 0.15C rate charge-discharge circulation 30 times under the room temperature.
5) the prepared lithium ion battery negative material α of the inventive method
-Fe
2O
3Can be used as lithium ion battery negative material.
Description of drawings
Fig. 1 is embodiment 1 gained α
-Fe
2O
3X ray diffracting spectrum.
Fig. 2 is embodiment 1 gained α
-Fe
2O
3Sem (SEM) photo.
Fig. 3 is embodiment 1 gained α
-Fe
2O
3Charge-discharge performance curve during as lithium ion battery negative material under the 0.15C multiplying power.
Fig. 4 is embodiment 1 gained α
-Fe
2O
3Charge-discharge performance during as lithium ion battery negative material under the different electric flow density.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is done further elaboration.
Embodiment 1
Take by weighing the analytically pure Fe (NO of 20.2g
3)
39H
2O is dissolved in and processes 50ml in the deionized water, the Fe (NO of 1 mol/L
3)
3The aqueous solution is measured the KOH aqueous solution 30ml of 5 mol/L that prepare in advance again, is poured into Fe (NO
3)
3Reaction precipitation obtains suspension-s in the aqueous solution; And with 25% ammonia soln adjusting pH value to 10; Vigorous stirring changes this mixing solutions over to 100ml Teflon hydrothermal reaction kettle after half a hour; Reaction kettle is put into baking oven, keep 180 ℃ of reaction 5h, be cooled in the air that the room temperature after-filtration separates, cleans, 80 ℃ of oven dry 12h can obtain α provided by the invention
-Fe
2O
3
Embodiment 2
Take by weighing the analytically pure Fe (NO of 20.2g
3)
39H
2O is dissolved in and processes 50ml in the deionized water, the Fe (NO of 1 mol/L
3)
3The aqueous solution is measured the KOH aqueous solution 30ml of 5 mol/L that prepare in advance again, is poured into Fe (NO
3)
3Reaction precipitation obtains suspension-s in the aqueous solution; And with 25% ammonia soln adjusting pH value to 10; Vigorous stirring changes this mixing solutions over to 100ml Teflon hydrothermal reaction kettle after half a hour; Reaction kettle is put into baking oven, keep 190 ℃ of reaction 5h, be cooled in the air that the room temperature after-filtration separates, cleans, 120 ℃ of oven dry 8h can obtain α provided by the invention
-Fe
2O
3
Embodiment 3
Take by weighing the analytically pure Fe (NO of 20.2g
3)
39H
2O is dissolved in and processes 50ml in the deionized water, the Fe (NO of 1 mol/L
3)
3The aqueous solution is measured the KOH aqueous solution 30ml of 5 mol/L that prepare in advance again, is poured into Fe (NO
3)
3Reaction precipitation obtains suspension-s in the aqueous solution; And with 25% ammonia soln adjusting pH value to 10; Vigorous stirring changes this mixing solutions over to 100ml Teflon hydrothermal reaction kettle after half a hour; Reaction kettle is put into baking oven, keep 200 ℃ of reaction 5h, be cooled in the air that the room temperature after-filtration separates, cleans, 100 ℃ of oven dry 12h can obtain α provided by the invention
-Fe
2O
3
Embodiment 4
Take by weighing the analytically pure Fe (NO of 20.2g
3)
39H
2O is dissolved in and processes 50ml in the deionized water, the Fe (NO of 1 mol/L
3)
3The aqueous solution is measured the KOH aqueous solution 30ml of 4 mol/L that prepare in advance again, is poured into Fe (NO
3)
3Reaction precipitation obtains suspension-s in the aqueous solution; And with 25% ammonia soln adjusting pH value to 10; Vigorous stirring changes this mixing solutions over to 100ml Teflon hydrothermal reaction kettle after half a hour; Reaction kettle is put into baking oven, keep 180 ℃ of reaction 6h, be cooled in the air that the room temperature after-filtration separates, cleans, 80 ℃ of oven dry 12h can obtain α provided by the invention
-Fe
2O
3
The result of Fig. 1-4 for embodiment 1 products therefrom is characterized and tests.The rhombohedral iron ore α that has the rhombohedral system structure among Fig. 1 in the XRD figure spectral line of product and the JCPDS DB
-Fe
2O
3Spectral line No.33-0664 very identical, show that this invents prepared product is monophasic α
-Fe
2O
3Fig. 2 shows prepared α
-Fe
2O
3Be finely dispersed spheroidal particle, about 200 nm of particle diameter; Can find out that from the Electrochemical results of Fig. 3 and Fig. 4 when under the 0.15C multiplying power, discharging and recharging, this bill of material reveals very high reversible specific capacity, specific storage remains 1167mAh/g behind the cycle charge discharge 30 times; Under the 1.5C multiplying power, test, its specific storage is about 380 mAh/g, still a little more than the theoretical specific capacity (372 mAh/g) of graphite cathode.
Embodiment 2-4 products therefrom is carried out thing characterize mutually, all can obtain monophasic α
-Fe
2O
3, and during as lithium ion battery negative material, all can reach the result close with embodiment, 0.15C rate charge-discharge round-robin specific storage reaches more than the 1100mAh/g under the room temperature.
Claims (7)
1. α-Fe who can be used for lithium ion battery negative material
2O
3And preparation method thereof, this α-Fe
2O
3Electrode materials mainly comprises and is prepared as follows step:
1) adopting deionized water is solvent, and disposing volumetric molar concentration respectively is the trivalent iron salt aqueous solution of 0.5-2 mol/L and the processable alkali metal hydroxide aqueous solution that volumetric molar concentration is 2-6 mol/L;
2) step 1) gained alkali metal hydroxide aqueous solution and trivalent iron salt aqueous solution are reacted, the suspension-s of formation stirs certain hour and regulates pH value to 9 ~ 13;
3) with step 2) the gained mixing solutions pours in the sealable reactor drum, places baking oven to be heated to 160-220 ℃ and be incubated 3-20 hour, and reaction is carried out solid-liquid separation after finishing, is washed, is drying to obtain said α-Fe
2O
3
2. method according to claim 1 is characterized in that: in the said step 1), and at least a in the muriate of the nitrate salt of said solubility trivalent iron salt chosen from Fe, the vitriol of iron, iron and the acetate of iron; Said easy capacitive alkali metal hydroxide is selected from least a in Lithium Hydroxide MonoHydrate, sodium hydroxide, Pottasium Hydroxide and the hydrated barta.
3. according to claims 1 described method, it is characterized in that: in the said step 1), the volumetric molar concentration of the said solubility trivalent iron salt aqueous solution is 0.5-2 mol/L; The volumetric molar concentration of said easy capacitive alkali metal hydroxide aqueous solution is 2-6 mol/L.
4. said step 2), the ratio of the amount of substance of said solubility trivalent iron salt and easy capacitive alkali metal hydroxide is 1:3; In the said adjusting pH value step, regulator is alkali aqueous solutions such as ammoniacal liquor or Pottasium Hydroxide, and the mass percentage concentration of said ammoniacal liquor is 25-28%, and the volumetric molar concentration of alkali aqueous solutions such as Pottasium Hydroxide is 2-6 mol/L.
5. method according to claim 1, gas is characterised in that: in the said step 3), hydrothermal temperature is 160-220 ℃, and the hydro-thermal reaction time is 3-20 hour; Drying temperature is 80-120 ℃, and be 8-12 hour time of drying.
6. α-Fe of preparing of the arbitrary said method of claim 1-4
2O
3Ion cathode material lithium.
7. the described α-Fe of claim 5
2O
3Use mainly as the lithium ion battery negative active material.
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Cited By (4)
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| CN104450790A (en) * | 2014-12-22 | 2015-03-25 | 中国科学院新疆理化技术研究所 | Biological method of preparing p-ferrite-modified n-hematite heterostructure |
| CN107706413A (en) * | 2017-11-08 | 2018-02-16 | 苏州宇量电池有限公司 | A kind of leaf Cyclic dart type iron oxide cathode material of nanometer three and preparation method thereof |
| CN114394626A (en) * | 2022-01-20 | 2022-04-26 | 西南石油大学 | Preparation method of rod-like ferric oxide negative electrode material of lithium ion battery |
| CN113000008B (en) * | 2021-03-08 | 2023-04-25 | 苏州工业园区蒙纳士科学技术研究院 | Iron-containing nano adsorbent and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104450790A (en) * | 2014-12-22 | 2015-03-25 | 中国科学院新疆理化技术研究所 | Biological method of preparing p-ferrite-modified n-hematite heterostructure |
| CN104450790B (en) * | 2014-12-22 | 2017-07-04 | 中国科学院新疆理化技术研究所 | It is a kind of to prepare the biological method that p ferrites modify n bloodstone heterojunction structures |
| CN107706413A (en) * | 2017-11-08 | 2018-02-16 | 苏州宇量电池有限公司 | A kind of leaf Cyclic dart type iron oxide cathode material of nanometer three and preparation method thereof |
| CN107706413B (en) * | 2017-11-08 | 2020-08-04 | 苏州宇量电池有限公司 | Nano three-leaf boomerang type iron oxide negative electrode material and preparation method thereof |
| CN113000008B (en) * | 2021-03-08 | 2023-04-25 | 苏州工业园区蒙纳士科学技术研究院 | Iron-containing nano adsorbent and preparation method and application thereof |
| CN114394626A (en) * | 2022-01-20 | 2022-04-26 | 西南石油大学 | Preparation method of rod-like ferric oxide negative electrode material of lithium ion battery |
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Application publication date: 20120718 |