CN110277550A - A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery - Google Patents

A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery Download PDF

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CN110277550A
CN110277550A CN201910548312.9A CN201910548312A CN110277550A CN 110277550 A CN110277550 A CN 110277550A CN 201910548312 A CN201910548312 A CN 201910548312A CN 110277550 A CN110277550 A CN 110277550A
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carbon cloth
ion battery
lithium
anode material
crystal form
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CN110277550B (en
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费杰
王娜
黄剑锋
曹丽云
许占位
李嘉胤
郑欣慧
李盟
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Shaanxi University of Science and Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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

Abstract

The present invention relates to the preparation methods that a kind of different valence state and crystal form sb oxide/carbon cloth make flexible anode material of lithium-ion battery, step 1: by SbCl3It is dissolved in dehydrated alcohol and obtains SbCl3Ethanol solution；Step 2:NaOH aqueous solution instills SbCl3In ethanol solution and adjusts its pH value and obtain mixed liquor；Step 3: the carbon cloth after activation processing being placed in mixed liquor and is impregnated；Step 4: by after dipping carbon cloth and mixed liquor go to hydro-thermal reaction in reaction vessel, different valence state and crystal form sb oxide/carbon cloth flexibility anode material of lithium-ion battery is made.The present invention prepares different valence state and crystal form sb oxide/carbon cloth flexibility anode material of lithium-ion battery by simply controlling the temperature of hydro-thermal reaction respectively；Its method and process is simple, and raw material is cheap, and products obtained therefrom crystal form is single, regular appearance, conducive to being grown in carbon cloth flexible substrates, has broad application prospects as sodium-ion battery flexibility cathode.

Description

A kind of different valence state and crystal form sb oxide/carbon cloth make flexible sodium-ion battery cathode The preparation method of material
Technical field
The invention belongs to flexible battery electrode material fields, and in particular to a kind of different valence state and crystal form sb oxide/carbon Cloth makees the preparation method of flexible anode material of lithium-ion battery.
Background technique
With various flexible, foldings and the appearance of frivolous electronic equipment, such as flexible electron display screen, flexible phone Deng the development of light and high-energy density flexible secondary cell obtains the attention of more scientific research personnel.Flexible electrode is high property One of the key factor of the flexible secondary cell development of energy.Sodium-ion battery is cheap since sodium element is resourceful, become after Most it is hopeful commercialized secondary cell after lithium ion secondary battery.As it can be seen that the research of sodium ion flexible electrode is with important Meaning.Material currently used for flexible electrode has graphene, carbon nanotube and carbon cloth etc..Wherein carbon cloth is due to good machine Carbon cloth carrying active substance is made flexible electrode material and has relevant report by tool performance and cheap.
Metal oxide makees the characteristic that second electrode negative electrode material has height ratio capacity, and metal oxide is generally polarity Oxide, and the combination of carbon cloth flexible electrode substrate are stronger, can be directly as sodium ion so carbon cloth is metal oxide-loaded Cell flexible negative electrode material.China's antimony is resourceful, and antimony element is located at the 5th main group, there is two kinds of valence states of positive trivalent and positive pentavalent, Trivalent is made battery electrode material and is had been reported that repeatly.Sb oxide synthetic method it is with the most use be wet process.Chinese patent Publication number CN10554066A and CN1072392A are related to a kind of method for preparing cubic crystal antimony trioxide, and this method is SbCl3 solution direct hydrolysis is prepared into aqueous slkali, but must be added to tartaric acid or its salt in hydrolyzate as crystal modifier. China Patent Publication No. CN104512926A is related to a kind of preparation method of rectangle antimony oxide, and this method is also in aqueous slkali It is middle to be prepared into SbCl3 solution direct hydrolysis, but must be added to triethanolamine in hydrolyzate.China Patent Publication No. CN101941737A is related to a kind of preparation method of antimony pentoxide dry powder, this method by antimony oxide, oxidant, water, It mixes according to a certain percentage, stirs, flows back, it is cooling, and inert porous material is added during the reaction, and core-shell structure copolymer has been made The antimony pentoxide of structure.
It can be seen that by must be added to oxidant, different crystal forms trivalent oxygen during Moist chemical synthesis pentavalent antimony oxide Certain crystal modifier need to be added in the synthesis for changing antimony.
Summary of the invention
The object of the present invention is to provide a kind of different valence states and crystal form sb oxide/carbon cloth to make flexible sodium-ion battery The preparation method of negative electrode material prepares orthorhombic forms Sb by control hydrothermal temperature and time respectively2O3/ carbon cloth, cube Crystal form Sb2O3/ carbon cloth and Sb2O5/ carbon cloth different valence state and crystal form sb oxide/carbon cloth flexibility anode material of lithium-ion battery.
In order to achieve the above objectives, the invention adopts the following technical scheme:
A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery, packet Include following steps:
Step 1: by the SbCl of 0.3~1.14g3It is added in 20~50mL dehydrated alcohol and dissolves to obtain SbCl3Solution；
Step 2: adjusting SbCl with NaOH aqueous solution3The pH value of solution obtains mixed liquor for 7~12；
Step 3: being placed in mixed liquor and impregnate after carbon cloth activation；
Step 4: carbon cloth and mixed liquor are gone into reaction vessel the hydro-thermal reaction at 120~180 DEG C, obtain different valence state and Crystal form sb oxide/carbon cloth flexibility anode material of lithium-ion battery.
Further, NaOH aqueous solution mass concentration is 0.6~1.2g/mL in step 2.
Further, carbon cloth activation is empty to carry out anodized, strong acid immersion treatment, low temperature to carbon cloth in step 3 One kind of gas oxidation processes.
Further, it is placed in mixed liquor after carbon cloth activation in step 3 and impregnates 20~40min.
Further, reaction vessel is polytetrafluoroethylkettle kettle in step 4；Carbon cloth and mixed liquor are gone in polytetrafluoroethylkettle kettle It is placed in 4~48h of hydro-thermal reaction in homogeneous reaction instrument.
Further, carbon cloth is hydrophilic carbon cloth, specification 32cm*16cm.
The beneficial effects of the present invention are embodied in:
The present invention provides a kind of different valence states and crystal form sb oxide/carbon cloth to make flexible anode material of lithium-ion battery Preparation method, using carbon cloth as substrate, by simply controlling, hydrothermal temperature prepares different valence state respectively and crystal form antimony aoxidizes Object/carbon cloth flexibility anode material of lithium-ion battery；Its simple process, raw material is cheap, and products obtained therefrom crystal form is single, regular appearance, Conducive to being grown in carbon cloth flexible substrates, have broad application prospects as sodium-ion battery flexibility cathode.
Detailed description of the invention
Fig. 1 is orthorhombic forms Sb prepared by embodiment 12O3The X-ray of/carbon cloth flexibility anode material of lithium-ion battery is spread out Penetrate map；
Fig. 2 is orthorhombic forms Sb prepared by embodiment 12O3The X-ray of/carbon cloth flexibility anode material of lithium-ion battery is spread out Penetrate map；
Fig. 3 is cubic Sb prepared by embodiment 22O3The X-ray of/carbon cloth flexibility anode material of lithium-ion battery is spread out Penetrate map；
Fig. 4 is cubic Sb prepared by embodiment 22O3The X-ray of/carbon cloth flexibility anode material of lithium-ion battery is spread out Penetrate map；
Fig. 5 is Sb prepared by embodiment 32O5The X-ray diffracting spectrum of/carbon cloth flexibility anode material of lithium-ion battery；
Fig. 6 is Sb prepared by embodiment 32O5The X-ray diffracting spectrum of/carbon cloth flexibility anode material of lithium-ion battery；
Fig. 7 is two kinds of valence state sb oxides/carbon cloth flexibility sodium-ion battery cathode prepared by embodiment 2 and embodiment 3 The electrochemistry cycle performance figure of material.
Specific embodiment
It elaborates with reference to the accompanying drawings and examples to the present invention.
Embodiment 1:
A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery, packet Include following steps:
Step 1: by the SbCl of 0.57g3It is added in 20mL dehydrated alcohol and dissolves to obtain SbCl3Solution；
Step 2: adjusting SbCl with the NaOH aqueous solution of 0.6g/mL3The pH to 8 of solution obtains mixed liquor；
Step 3: being placed in mixed liquor after carbon cloth progress anodized activation and impregnate 30min, wherein carbon cloth is hydrophilic Type carbon cloth and specification are 32cm*16cm；
Step 4: carbon cloth and mixed liquor being gone into polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument at 120 DEG C that hydro-thermal is anti- Orthorhombic forms Sb should be obtained for 24 hours2O3/ carbon cloth flexibility anode material of lithium-ion battery.
As shown in Figure 1, analyzing orthorhombic forms Sb with Rigaku D/max2000PCX- x ray diffractometer x2O3/ carbon cloth is flexible The Sb that anode material of lithium-ion battery, discovery sample and PDF number are 11-06892O3Structure is consistent, at 25.47 °, 28.38 °, 28.61 °, 43.96 °, 50.44 ° there is characteristic peak.As shown in Fig. 2, the field of sample FEI Co., U.S. S-4800 type is sent out It penetrates scanning electron microscope and carries out morphology observation, it is seen that obtained orthorhombic forms Sb2O3Particle is bulk, and size is larger, compared with Dispersion is grown on carbon cloth.
Embodiment 2:
A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery, packet Include following steps:
Step 1: by the SbCl of 1.14g3It is added in 40mL dehydrated alcohol and dissolves to obtain SbCl3Solution；
Step 2: adjusting SbCl with the NaOH aqueous solution of 1.2g/mL3The pH to 10 of solution obtains mixed liquor；
Step 3: being placed in mixed liquor after carbon cloth progress anodized activation and impregnate 30min, wherein carbon cloth is hydrophilic Type carbon cloth and specification are 32cm*16cm；
Step 4: carbon cloth and mixed liquor being gone into polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument at 150 DEG C that hydro-thermal is anti- Cubic Sb should be obtained for 24 hours2O3/ carbon cloth flexibility anode material of lithium-ion battery.
As shown in figure 3, analyzing cubic Sb with Rigaku D/max2000PCX- x ray diffractometer x2O3/ carbon cloth is flexible The Sb that anode material of lithium-ion battery, discovery sample and PDF number are 43-10712O3Structure is consistent, at 27.69 °, 32.08 °, 35.05 °, 46.00 °, 54.54 ° there is characteristic peak.As shown in figure 4, the field of sample FEI Co., U.S. S-4800 type is sent out It penetrates scanning electron microscope and carries out morphology observation, it is seen that cubic Sb2O3For spherical particle, and closely it is grown on carbon cloth.
Embodiment 3:
A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery, packet Include following steps:
Step 1: the SbCl3 of 0.57g being added in 20mL dehydrated alcohol and dissolves to obtain SbCl3Solution；
Step 2: adjusting SbCl with the NaOH aqueous solution of 0.6g/mL3The pH to 9 of solution obtains mixed liquor；
Step 3: being placed in mixed liquor after carbon cloth progress anodized activation and impregnate 40min, wherein carbon cloth is hydrophilic Type carbon cloth and specification are 32cm*16cm；
Step 4: carbon cloth and mixed liquor being gone into polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument at 180 DEG C that hydro-thermal is anti- Sb should be obtained for 24 hours2O5/ carbon cloth flexibility anode material of lithium-ion battery.
As shown in figure 5, analyzing orthorhombic forms Sb with Rigaku D/max2000PCX- x ray diffractometer x2O3/ carbon cloth is flexible The Sb that anode material of lithium-ion battery, discovery sample and PDF number are 11-06902O3Structure is consistent, at 14.87 °, 28.70 °, 30.00 °, 34.78 °, 50.05 °, 59.47 ° there is characteristic peak.As shown in fig. 6, by sample FEI Co., U.S. S-4800 type Field emission scanning electron microscope carry out morphology observation, it is seen that Sb2O5For spherical particle, and uniformly grown with monolayer In on carbon cloth, diameter about 50nm or so.
As shown in fig. 7, by cubic Sb prepared in embodiment 2 and embodiment 32O3/ carbon cloth and Sb2O5/ carbon cloth is soft Property anode material of lithium-ion battery be assembled into CR2032 type button cell respectively, and on blue electrical measurement test system carry out constant current fill Discharge cycle performance test, finds in 100mA.g-1Under current density, stable charging and discharging capacity is all shown, wherein Sb2O5/ carbon cloth is than cubic Sb2O3/ carbon cloth shows higher specific discharge capacity as anode material of lithium-ion battery, works as circulation When enclosing to 20, specific discharge capacity is respectively 1500mAh.g-1And 500mAh.g-1。
Embodiment 4:
A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery, packet Include following steps:
Step 1: by the SbCl of 0.3g3It is added in 20mL dehydrated alcohol and dissolves to obtain SbCl3Solution；
Step 2: adjusting SbCl with the NaOH aqueous solution of 0.6g/mL3The pH to 11 of solution obtains mixed liquor；
Step 3: being placed in mixed liquor after carbon cloth progress anodized activation and impregnate 30min, wherein carbon cloth is hydrophilic Type carbon cloth and specification are 32cm*16cm；
Step 4: carbon cloth and mixed liquor being gone into polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument at 120 DEG C that hydro-thermal is anti- 12h is answered, orthorhombic forms Sb is obtained2O3/ carbon cloth flexibility anode material of lithium-ion battery.
Orthorhombic forms Sb is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2O3/ carbon cloth flexibility sodium-ion battery The Sb that negative electrode material, discovery sample and PDF number are 11-06892O3Structure is consistent, at 25.47 °, 28.38 °, 28.61 °, 43.96 °, 50.44 ° there is characteristic peak.
Embodiment 5:
A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery, packet Include following steps:
Step 1: by the SbCl of 1.14g3It is added in 50mL dehydrated alcohol and dissolves to obtain SbCl3Solution；
Step 2: adjusting SbCl with the NaOH aqueous solution of 0.7g/mL3The pH to 10 of solution obtains mixed liquor；
Step 3: being placed in mixed liquor after carbon cloth progress anodized activation and impregnate 30min, wherein carbon cloth is hydrophilic Type carbon cloth and specification are 32cm*16cm；
Step 4: carbon cloth and mixed liquor being gone into polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument at 150 DEG C that hydro-thermal is anti- 10h is answered, cubic Sb is obtained2O3/ carbon cloth flexibility anode material of lithium-ion battery.
Cubic Sb is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2O3/ carbon cloth flexibility sodium-ion battery The Sb that negative electrode material, discovery sample and PDF number are 43-10712O3Structure is consistent, at 27.69 °, 32.08 °, 35.05 °, 46.00 °, 54.54 ° there is characteristic peak.
Embodiment 6:
A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery, packet Include following steps:
Step 1: by the SbCl of 0.57g3It is added in 20mL dehydrated alcohol and dissolves to obtain SbCl3Solution；
Step 2: adjusting SbCl with the NaOH aqueous solution of 1g/mL3The pH to 12 of solution obtains mixed liquor；
Step 3: being placed in mixed liquor after carbon cloth progress strong acid immersion treatment activation and impregnate 30min, wherein carbon cloth is hydrophilic Type carbon cloth and specification are 32cm*16cm；
Step 4: carbon cloth and mixed liquor being gone into polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument at 180 DEG C that hydro-thermal is anti- 48h is answered, Sb is obtained2O5/ carbon cloth flexibility anode material of lithium-ion battery.
Sb is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2O5/ carbon cloth flexibility anode material of lithium-ion battery, It was found that the Sb that sample and PDF number are 11-06902O5Structure is consistent, at 14.87 °, 28.70 °, 30.00 °, 34.78 °, 50.05 °, 59.47 ° there is characteristic peak.
Embodiment 7:
A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery, packet Include following steps:
Step 1: by the SbCl of 0.3g3It is added in 30mL dehydrated alcohol and dissolves to obtain SbCl3Solution；
Step 2: adjusting SbCl with the NaOH aqueous solution of 0.8g/mL3The pH value of solution to 7 mixed liquor；
Step 3: carbon cloth be placed in mixed liquor after low temperature air oxidation processing activation impregnating 30min, wherein carbon cloth is Hydrophilic carbon cloth and specification are 32cm*16cm；
Step 4: carbon cloth and mixed liquor being gone into polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument at 180 DEG C that hydro-thermal is anti- 4h is answered, orthorhombic forms Sb is obtained2O5/ carbon cloth flexibility anode material of lithium-ion battery.
Sb is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2O5/ carbon cloth flexibility anode material of lithium-ion battery, It was found that the Sb that sample and PDF number are 11-06902O5Structure is consistent, at 25.47 °, 28.38 °, 28.61 °, 43.96 °, 50.44 ° There is characteristic peak.
Embodiment 8:
A kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery, packet Include following steps:
Step 1: by the SbCl of 1.14g3It is added in 35mL dehydrated alcohol and dissolves to obtain SbCl3Solution；
Step 2: adjusting SbCl with the NaOH aqueous solution of 0.9g/mL3The pH value of solution to 10 mixed liquor；
Step 3: being placed in mixed liquor after carbon cloth progress anodized activation and impregnate 30min, wherein carbon cloth is hydrophilic Type carbon cloth and specification are 32cm*16cm；
Step 4: carbon cloth and mixed liquor being gone into polytetrafluoroethylkettle kettle and are placed in homogeneous reaction instrument at 120 DEG C that hydro-thermal is anti- 36h is answered, orthorhombic forms Sb is obtained2O3/ carbon cloth flexibility anode material of lithium-ion battery.
Orthorhombic forms Sb is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2O3/ carbon cloth flexibility sodium-ion battery The Sb that negative electrode material, discovery sample and PDF number are 11-06892O3Structure is consistent, at 25.47 °, 28.38 °, 28.61 °, 43.96 °, 50.44 ° there is characteristic peak.
In short, the present invention prepares orthorhombic forms using carbon cloth as substrate, by simply controlling hydrothermal temperature respectively Sb2O3/ carbon cloth, cubic Sb2O3/ carbon cloth and Sb2O5/ carbon cloth different valence state and crystal form sb oxide/carbon cloth flexibility sodium ion Cell negative electrode material.Different valence state provided by the invention and crystal form sb oxide/carbon cloth flexibility anode material of lithium-ion battery Preparation method, simple process, raw material is cheap, and products obtained therefrom crystal form is single, regular appearance, conducive to carbon cloth flexible substrates are grown on On, it has broad application prospects as sodium-ion battery flexibility cathode.

Claims (6)

1. a kind of different valence state and crystal form sb oxide/carbon cloth make the preparation method of flexible anode material of lithium-ion battery, special Sign is, comprising the following steps:
Step 1: by the SbCl of 0.3~1.14g3It is added in 20~50mL dehydrated alcohol and dissolves to obtain SbCl3Solution；
Step 2: adjusting SbCl with NaOH aqueous solution3The pH value of solution obtains mixed liquor for 7~12；
Step 3: being placed in mixed liquor and impregnate after carbon cloth activation；
Step 4: carbon cloth and mixed liquor being gone into reaction vessel the hydro-thermal reaction at 120~180 DEG C, obtain different valence state and crystal form Sb oxide/carbon cloth flexibility anode material of lithium-ion battery.
2. a kind of different valence state and crystal form sb oxide/carbon cloth flexibility anode material of lithium-ion battery according to claim 1 Preparation method, which is characterized in that in the step 2 NaOH aqueous solution mass concentration be 0.6~1.2g/mL.
3. a kind of different valence state and crystal form sb oxide/carbon cloth flexibility anode material of lithium-ion battery according to claim 1 Preparation method, which is characterized in that carbon cloth activation is carries out anodized, at strong acid immersion to carbon cloth in the step 3 Reason, one kind of low temperature air oxidation processing.
4. a kind of different valence state and crystal form sb oxide/carbon cloth flexibility anode material of lithium-ion battery according to claim 1 Preparation method, which is characterized in that in the step 3 carbon cloth activation after be placed in mixed liquor in impregnate 20~40min.
5. a kind of different valence state and crystal form sb oxide/carbon cloth flexibility anode material of lithium-ion battery according to claim 1 Preparation method, which is characterized in that in the step 4 reaction vessel be polytetrafluoroethylkettle kettle；Carbon cloth and mixed liquor go to poly- four 4~48h of hydro-thermal reaction in homogeneous reaction instrument is placed in vinyl fluoride kettle.
6. a kind of different valence state and crystal form sb oxide/carbon cloth flexibility anode material of lithium-ion battery according to claim 1 Preparation method, which is characterized in that the carbon cloth be hydrophilic carbon cloth, specification 32cm*16cm.
CN201910548312.9A 2019-06-24 2019-06-24 Preparation method of flexible sodium-ion battery cathode material made of antimony oxide/carbon cloth with different valence states and crystal forms Active CN110277550B (en)

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CN112038607A (en) * 2020-09-09 2020-12-04 陕西科技大学 Carbon cloth loaded flower-shaped Sb2O4@ polyhedral Sb2O5Composite self-supporting electrode material and preparation method thereof

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CN108400315A (en) * 2018-01-29 2018-08-14 北京航空航天大学 A kind of preparation method of the ion battery cathode material of carbon-coated antimony doping stannic oxide
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CN109546129A (en) * 2018-11-29 2019-03-29 陕西科技大学 Sodium-ion battery cathode C/SnO2The preparation method of/carbon cloth composite material
CN109786717A (en) * 2019-01-30 2019-05-21 陕西科技大学 A kind of sodium-ion battery cathode SnO2The preparation method of/carbon cloth composite material
CN109786716A (en) * 2019-01-30 2019-05-21 陕西科技大学 A kind of Sn/ carbon cloth composite material does the preparation method of sodium-ion battery cathode

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CN112038623A (en) * 2020-09-09 2020-12-04 陕西科技大学 Sb based on controllable construction of carbon cloth substrate2O4Self-supporting electrode material for sodium ion battery cathode and preparation method thereof
CN112038607A (en) * 2020-09-09 2020-12-04 陕西科技大学 Carbon cloth loaded flower-shaped Sb2O4@ polyhedral Sb2O5Composite self-supporting electrode material and preparation method thereof

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