CN102826616B - Ferric fluoride nano material and preparation method thereof - Google Patents
Ferric fluoride nano material and preparation method thereof Download PDFInfo
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- CN102826616B CN102826616B CN201210339101.2A CN201210339101A CN102826616B CN 102826616 B CN102826616 B CN 102826616B CN 201210339101 A CN201210339101 A CN 201210339101A CN 102826616 B CN102826616 B CN 102826616B
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- 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
Abstract
The invention discloses a ferric fluoride nano material and a preparation method thereof. The preparation method comprises the following steps of: dissolving inorganic ferric salt in an alcohol solvent to obtain alcohol solution containing iron; dispersing an inorganic fluorine source into the alcohol solution containing iron and adding the solution into a hydrothermal reaction kettle; carrying out the hydrothermal reaction kettle solution for 1 hour to 7 days at a temperature of 40 to 140 DEG C, naturally cooling, carrying out centrifugal separation, washing by ethanol and carrying out vacuum drying to obtain the ferric fluoride nano material. According to the preparation method of ferric fluoride, a volatile hydrofluoric acid fluorine source does not need to be used as a raw material, low-toxicity fluoride is used as the fluorine source, common ferric salt is used as a ferric source, the FeF3.0.33H2O nano material containing trace moisture is obtained by the simple solvent heat treatment, the preparation process is simple, the yield is high and the obtained material has high crystallinity. The method disclosed by the invention is a novel and practical process route for preparing the ferric fluoride nano material and has high actual application value.
Description
Technical field
The invention belongs to electrode materials field, specifically, the present invention relates to a kind of three and fluoridize ferrum nano material and preparation method thereof.
Background technology
Existing lithium-ion secondary cell also cannot meet the requirement to battery high energy metric density such as electromobile, and the specific storage of electrode materials directly affects the energy density of battery, therefore design and develop and there is the top priority that high reversible capacity electrode materials is development lithium-ion secondary cell.Reversible chemical transformation mechanism positive electrode material---transition metal fluorides, due to higher output voltage and theoretical specific capacity can be provided, obtains researchist's extensive concern.
From last century the seventies, existing a large amount of relevant fluorochemicals are used as the research work of lithium ion secondary battery anode material.The earliest be reported in 1970, synthesized NiF by Seiger etc.
2and realize the limited reversible cycle (H.N.Seiger of material, A.E.Lyall, R.C.Shair, in Proceedings of the 6thInternational Symposium on Power Sources 2:Res:Develop.Non-Mech.Elec.Power Sources, 1970, p.267).Afterwards, Arai etc. has reported TiF
3, VF
3, FeF
3also there is electrochemical activity (H.Arai, S.Okada, Y.Sakurai and J.Yamaki, J.Power Sources, 1997,68,716.) Deng material.These materials reach 80mAh g at the reversible capacity of the voltage range of 2.0-4.5V
-1, be mainly corresponding to M
3+/ M
2+reversible chemical reaction between electron pair.Recently, relevant TiF
3and VF
3the report of material reversible chemical switching mechanism points out, in the voltage range of 0.02-4.3V, these materials can provide the g up to 500-600mAh
-1reversible capacity.In numerous transition metal, Fe element has cheap, and reserves are abundant, and advantages of environment protection, is one of first-selected element of electrode materials.Therefore, three ferric fluorides become one of preferred material of reversible chemical transformation mechanism material.When as positive electrode material, there are two kinds of different storage lithium mechanism in three ferric fluorides, in 2.5-4.5V voltage range, a lithium ion is at FeF in charge and discharge process
3the interior reversible embedding of crystalline structure/deviate from, is accompanied by Fe
3+/ Fe
2+transformation, be typical embedding, de-lithium mechanism, lithium storage content is 237mAh g
-1.At 1.5-2.5V voltage range, ferric fluoride can continue and two lithium ion generation electrochemical reducting reactions, forms Fe nanoparticle and LiF, is reversible chemical switching mechanism, and lithium storage content is 475mAh g
-1.FeF
3also exist the reversible capacity of material as electrode materials less, the problem such as cyclical stability is poor.This is mainly due to FeF
3the poor and charge and discharge process of electroconductibility in exist the institutes such as volumetric expansion to cause.For FeF
3these problems, main improved route is by FeF
3with the compound preparation nano composite material of conducting material, increase the conductivity of material.2003, Amatucci etc. were by FeF
3with carbon material (expanded graphite, carbon black and gac), prepare serial nano matrix material (F.Badway, N.Pereira with ball milled, F.Cosandey, G.G.Amatucci, J Electrochem.Soc., 2003,150A1209).In the voltage range of 2.0-4.5V, the initial discharge capacity 200mAh g of material
-1, corresponding to Fe
3+/ Fe
2+redox reaction.Subsequently, for same nano composite material, Amatucci etc. have studied its chemical property at 1.5-4.5V voltage range, and have reported based on Fe
3+/ Fe
0the reduction reaction of three electronics.In the time of 70 ℃, nano composite material has 500mAh g
-1reversible capacity.2009, Okada etc. utilized ball milled equally, prepare FeF
3/ carbon composite, has studied the charge-discharge performance (M.Nishijima, I.D.Gocheva, S.Okada, T.Doi, J.-i.Yamaki and T.Nishida, J.Power Sources, 2009,190,558) of material in 2.0-4.5V voltage range.Result shows, the existence of carbon material has improved the specific conductivity of matrix material and reduced the solubleness of fluorochemical in electrolyte solution.Except carbon material, investigator also passes through FeF
3carry out the compound chemical property that obtains nano composite material and improve material with conductive oxide and sulfide.2009, professor Wang Xianyou of University Of Xiangtan utilized ball milled, prepares FeF
3/ MoS
2, FeF
3/ V
2o
5nano composite material (W.Wu, X.Wang, X.Wang, S.Yang, X.Liu and Q.Chen, Mater.Lett., 2009,63,1788; W.Wu, Y.Wang, X.Wang, Q.Chen, X.Wang, S.Yang, X.Liu, J.Gao and Z.Yang, J.Alloys Compd., 2009,486,93).Result shows, at 2.0-4.5V voltage range, with respect to the FeF of pure phase
3material, the chemical property of matrix material has larger improvement.Although by carrying out compoundly can improving FeF with electro-conductive material
3conductivity, and improved to a certain extent FeF
3reversible capacity and cyclical stability, but its performance reaches far away actual application level, the FeF particularly using
3raw material particle size is larger, causes the FeF in the nano composite material of synthesized
3particle diameter is large and particle size distribution range is wide, and material structure consistence is poor, is the important factor that affects material application.
Preparation FeF at present
3main method be that ferric oxide or iron(ic) chloride and dry hydrogen fluoride gas effect are generated to amorphous FeF
3; At high temperature fluorine gas and metallic iron or ferric oxide effect are obtained to FeF
3.Recently there is bibliographical information to utilize the Fe (OH) of new system
3precipitation and hydrofluoric acid effect, then unnecessary water and the HF of evaporate to dryness obtains FeF
3.Also have bibliographical information to utilize ionic liquid to prepare FeF as solvent and fluorine source
3.But these methods also exist reaction process consumptive material high, gained FeF
3particle diameter is larger, needs the shortcomings such as poisonous fluorine source.Therefore, utilize low toxicity or nontoxic fluorochemical as fluorine source, synthesize by simple method the FeF that particle diameter is less
3material is for the development important in inhibiting that promotes height ratio capacity lithium-ion secondary cell.
Summary of the invention
Based on this, the present invention is directed to and in prior art, prepare FeF
3the deficiency of material, provides a kind of simple FeF
3the preparation method of nano material.
Three fluoridize a preparation method for ferrum nano material, comprise the following steps:
(1) inorganic molysite is dissolved in alcoholic solvent, obtains the alcoholic solution of iron content, in the alcoholic solution of described iron content, the concentration of iron ion is 1mM～0.2M;
(2) inorganic fluorine source is distributed to after the alcoholic solution of iron content of step (1), solution is transferred in hydrothermal reaction kettle; The iron ion of described inorganic molysite and NH
4hF
2the mol ratio of fluorion be 1: 2～4: 1;
(3) by hydrothermal reaction kettle in 40～140 ℃ of thermal treatments 1 hour to 7 days, naturally cooling, centrifugation, washing with alcohol, vacuum-drying at 40～80 ℃, to obtain final product.
In some embodiment therein, described in step (1), inorganic molysite is Fe (NO
3)
39H
2o, Fe
2(SO
4)
3or FeCl
3.
In some embodiment therein, described in step (1), alcoholic solvent is ethanol or propyl alcohol.
In some embodiment therein, in the alcoholic solution of the described iron content of step (1), the concentration of iron ion is 10mM～0.15M.
In some embodiment therein, described in step (2), the mol ratio of the iron ion of inorganic molysite and the fluorion of inorganic fluorine source is 1: 2.5～3.5: 1.
In some embodiment therein, in step (3), heat treated temperature is 60-120 ℃, and heat treatment time is 2 hours-3 days.
What the present invention also provided that above-mentioned preparation method prepares three fluoridizes ferrum nano material.
It is raw material that the preparation method of the present invention's three ferric fluorides does not need volatility fluorine source hydrofluoric acid, and the fluorochemical that utilizes low toxicity is fluorine source, and common molysite is source of iron, by simple solvent heat treatment, obtains the FeF containing minor amount of water
30.33H
2o nano material, preparation process is simple, and productive rate is high, and resulting materials degree of crystallinity is high.The inventive method is the preparation three one novelties of fluoridizing ferrum nano material, and practical operational path, is of very high actual application value.
Accompanying drawing explanation
Fig. 1 is FeF prepared by the embodiment of the present invention 1
30.33H
2the XRD spectra of O nano material;
Fig. 2 is FeF prepared by the embodiment of the present invention 1
30.33H
2the charging and discharging curve of O nano material.
Embodiment
Describe the present invention in detail below in conjunction with the drawings and specific embodiments.
Embodiment 1 three fluoridizes the preparation method of ferrum nano material
Comprise the following steps:
(1) by 0.1263g Fe (NO
3)
39H
2o is dissolved in 30mL dehydrated alcohol, obtains the alcoholic solution of the iron content of clarification, and in the alcoholic solution of this iron content, the concentration of iron ion is 10.4mM;
(2) under agitation condition, by 0.0267g NH
4hF
2be added in the alcoholic solution of above-mentioned iron content, until system becomes water white solution, solution transferred in the tetrafluoroethylene reactor that volume is 50mL; Described Fe (NO
3)
39H
2o and NH
4hF
2mol ratio be 1: 1.5 (mol ratio of iron ion and fluorion is 1: 3);
(3) by hydrothermal reaction kettle in 80 ℃ of thermal treatments 4 hours, naturally cooling, centrifugation, washing with alcohol 3 times, vacuum-drying 10h at 60 ℃, obtains FeF
30.33H
2o nano material.
Prepared by embodiment 1 to the FeF of gained
30.33H
2o nano material has been carried out the sign of some structures and character.Figure 1 shows that FeF
30.33H
2the XRD spectra of O nano material, diffraction peaks all in figure all belong to FeF
30.33H
2the characteristic diffraction peak of O, inclusion-free exists.The diffraction peak illustrative material of broadening is made up of nanoparticle, according to Scherrer formula (D=K λ/Bcos θ, wherein K is Scherrer constant, its value is 0.89; D is grain-size (nm); B is integration halfwidth degree) calculate particle diameter and be approximately 10-15 nanometer.
As shown in Figure 2, be the charging and discharging curve figure of the nano material of the present embodiment, as can be seen from Figure 2, the specific discharge capacity of the nano material of the present embodiment is 137mAh/g.
Embodiment 2 three fluoridizes the preparation method of ferrum nano material
Preparation method is with embodiment 1, just by Fe (NO
3)
39H
2the consumption of O becomes 0.606g (in the alcoholic solution of iron content, the concentration of iron ion is 50mM), by NH
4hF
2consumption become 0.1485g (Fe (NO
3)
39H
2o and NH
4hF
2mol ratio be 1: 1.5, the mol ratio of iron ion and fluorion is 1: 3), XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 130mAh/g.
Embodiment 3 three fluoridizes the preparation method of ferrum nano material
Preparation method is with embodiment 1, just by Fe (NO
3)
39H
2the consumption of O becomes 1.212g (in the alcoholic solution of iron content, the concentration of iron ion is 0.1M), by NH
4hF
2consumption become 0.297g (Fe (NO
3)
39H
2o and NH
4hF
2mol ratio be 1: 1.5, the mol ratio of iron ion and fluorion is 1: 3), XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 122mAh/g.
Embodiment 4 three fluoridizes the preparation method of ferrum nano material
Preparation method is with embodiment 1, just by Fe (NO
3)
39H
2the consumption of O becomes 1.818g (in the alcoholic solution of iron content, the concentration of iron ion is 0.15M), by NH
4hF
2consumption become 0.4455g (Fe (NO
3)
39H
2o and NH
4hF
2mol ratio be 1: 1.5, the mol ratio of iron ion and fluorion is 1: 3), XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 125mAh/g.
Embodiment 5 three fluoridizes the preparation method of ferrum nano material
Preparation method is with embodiment 1, just by Fe (NO
3)
39H
2the consumption of O becomes 2.424g (in the alcoholic solution of iron content, the concentration of iron ion is 0.2M), by NH
4hF
2consumption become 0.594g (Fe (NO
3)
39H
2o and NH
4hF
2mol ratio be 1: 1.5, the mol ratio of iron ion and fluorion is 1: 3), XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 115mAh/g.
Embodiment 6 three fluoridizes the preparation method of ferrum nano material
Preparation method is with embodiment 1, just by NH
4hF
2consumption become 0.0206g (Fe (NO
3)
39H
2o and NH
4hF
2mol ratio be 1: 1, the mol ratio of iron ion and fluorion is 1: 2), XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 110mAh/g.
Embodiment 7 three fluoridizes the preparation method of ferrum nano material
Preparation method is with embodiment 1, just by NH
4hF
2consumption become 0.0258g (Fe (NO
3)
39H
2o and NH
4hF
2mol ratio be 1: 1.25, the mol ratio of iron ion and fluorion is 1: 2.5), XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 128mAh/g.
Embodiment 8 three fluoridizes the preparation method of ferrum nano material
Preparation method is with embodiment 1, just by NH
4hF
2consumption become 0.00295g (Fe (NO
3)
39H
2o and NH
4hF
2mol ratio be 7: 1, the mol ratio of iron ion and fluorion is 3.5: 1), XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 122mAh/g.
Embodiment 9 three fluoridizes the preparation method of ferrum nano material
Preparation method is with embodiment 1, just by NH
4hF
2consumption become 0.00258g (Fe (NO
3)
39H
2o and NH
4hF
2mol ratio be 8: 1, the mol ratio of iron ion and fluorion is 4: 1), XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 105mAh/g.
Embodiment 10 3 fluoridizes the preparation method of ferrum nano material
Preparation method, with embodiment 4, just becomes 60 ℃ of thermal treatments 1 hour by step (3), and XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 118mAh/g.
Embodiment 11 3 fluoridizes the preparation method of ferrum nano material
Preparation method, with embodiment 4, just becomes 100 ℃ of thermal treatments 15 hours by step (3), and XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 132mAh/g.
Embodiment 12 3 fluoridizes the preparation method of ferrum nano material
Preparation method, with embodiment 4, just becomes 80 ℃ of thermal treatments 24 hours by step (3), and XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 122mAh/g.
Embodiment 13 3 fluoridizes the preparation method of ferrum nano material
Preparation method, with embodiment 4, just becomes 120 ℃ of thermal treatments 3 days by step (3), and XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 119mAh/g.
Embodiment 14 3 fluoridizes the preparation method of ferrum nano material
Preparation method, with embodiment 4, just becomes 80 ℃ of thermal treatments 6 days by step (3), and XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 108mAh/g.
Embodiment 15 3 fluoridizes the preparation method of ferrum nano material
Preparation method is with embodiment 1, just by the Fe (NO in step (1)
3)
39H
2o becomes Fe
2(SO
4)
3, XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 103mAh/g.
Embodiment 16 3 fluoridizes the preparation method of ferrum nano material
Preparation method is with embodiment 1, just by the Fe (NO in step (1)
3)
39H
2o becomes FeCl
3, XRD spectra shows to obtain equally FeF
30.33H
2o nano material.Particle diameter is approximately 10-15 nanometer, and the specific discharge capacity of material is 121mAh/g.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (4)
1. three preparation methods that fluoridize ferrum nano material, is characterized in that, comprise the following steps:
(1) inorganic molysite is dissolved in alcoholic solvent, obtains the alcoholic solution of iron content, in the alcoholic solution of described iron content, the concentration of iron ion is 10mM-0.15M;
(2) by NH
4hF
2be distributed to after the alcoholic solution of iron content of step (1), solution is transferred in hydrothermal reaction kettle; The iron ion of described inorganic molysite and NH
4hF
2the mol ratio of fluorion be 1:2～4:1;
(3) by hydrothermal reaction kettle in 40～140 ℃ of thermal treatments 1 hour to 7 days, naturally cooling, centrifugation, washing with alcohol, vacuum-drying, to obtain final product;
Described alcoholic solvent is ethanol.
2. as claimed in claim 1 three preparation methods that fluoridize ferrum nano material, is characterized in that, described in step (1), inorganic molysite is Fe (NO
3)
39H
2o, Fe
2(SO
4)
3or FeCl
3.
3. as claimed in claim 1 three preparation methods that fluoridize ferrum nano material, is characterized in that, iron ion and the NH of inorganic molysite described in step (2)
4hF
2the mol ratio of fluorion be 1:2.5～3.5:1.
4. as claimed in claim 1 three preparation methods that fluoridize ferrum nano material, is characterized in that: in step (3), heat treated temperature is 60-120`, and heat treatment time is 2 hours-3 days.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103151523B (en) * | 2013-02-28 | 2015-07-22 | 湘潭大学 | Preparation method of cuboid-shaped positive-pole FeF3(H2O)0.33 material |
| CN103165888B (en) * | 2013-03-02 | 2016-12-28 | 合肥国轩高科动力能源有限公司 | One has embedding lithium active Fe F3the preparation method of nanometer rods |
| CN103682340B (en) * | 2013-12-26 | 2016-03-23 | 中国科学院上海硅酸盐研究所 | A kind of iron-based fluoride nano material with hierarchy and its preparation method and application |
| CN103708565B (en) * | 2014-01-06 | 2015-06-03 | 贵州万方铝化科技开发有限公司 | Preparation method of FeF3 |
| CN103771534B (en) * | 2014-02-26 | 2015-06-03 | 贵州万方铝化科技开发有限公司 | Method and equipment for recycling fluoride in iron-containing compound production |
| CN104600301B (en) * | 2015-01-22 | 2017-02-01 | 中国工程物理研究院化工材料研究所 | Spherical cobaltous fluoride for battery positive material and preparation method of spherical cobaltous fluoride |
| CN105336946B (en) * | 2015-09-28 | 2018-09-11 | 中国船舶重工集团公司第七一二研究所 | A kind of preparation method of lithium ion battery ferric fluoride anode material |
| CN105958020A (en) * | 2016-05-26 | 2016-09-21 | 湘潭大学 | Method for preparing nanometer FeF<3>.0.33H<2>O by alcohol-thermal method |
| CN106099074B (en) * | 2016-08-19 | 2019-03-22 | 广东工业大学 | A kind of modified fluorinated iron nano composite anode material and its preparation method and application |
| CN110713242B (en) * | 2019-08-09 | 2020-12-01 | 中国科学院地理科学与资源研究所 | Zero-valent iron material Fe @ iron fluoride and preparation method thereof |
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