CN103950992B - The method of the transition metal oxide nano-slice of graphenic surface growing upright - Google Patents

The method of the transition metal oxide nano-slice of graphenic surface growing upright Download PDF

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CN103950992B
CN103950992B CN201410163843.3A CN201410163843A CN103950992B CN 103950992 B CN103950992 B CN 103950992B CN 201410163843 A CN201410163843 A CN 201410163843A CN 103950992 B CN103950992 B CN 103950992B
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CN103950992A (en
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丁书江
董碧桃
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Xian Jiaotong University
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    • 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
    • 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
    • Y02E60/13—Energy storage using capacitors

Abstract

The method of the transition metal oxide nano-slice of graphenic surface growing upright, first, ultrasonic separation is carried out with by the Graphene of oxidation, then use the method for oil bath in the transition-metal oxide nanometer sheet of surface of graphene oxide growing upright, in nitrogen, this material of transition-metal oxide nanometer sheet of graphenic surface growing upright finally after calcining, can be obtained; Feature of the present invention adopts simple chemosynthesis means, prepares easily separated, high-specific surface area, lithium electricity and ultracapacitor performance is better than general nano material electrochemical material.

Description

The method of the transition metal oxide nano-slice of graphenic surface growing upright
Technical field
The present invention relates to the preparation of graphene-based inorganic, metal oxide nano structural material, in particular to the method for the transition metal oxide nano-slice at graphenic surface growing upright for lithium ion battery and ultracapacitor, transition metal oxide comprises cobalt acid nickel, cobalt acid zinc, nickel oxide, cobalt oxide, zinc permanganate.
Technical background
Graphene-based nanostructure composite material shows the good potentiality as lithium ion battery negative material and electrode material for super capacitor, Graphene has excellent electrical properties, such as, good electroconductibility, the specific surface area of super large, light transmission and chemical stability and workability this make it become electrochemistry new forms of energy to transform and the electrode materials stored, not only effectively can improve the specific surface area of active ingredient using it as other nanoparticles carrier loaded, pure nanoparticle can also be solved and easily assemble this difficult problem.
In recent years, in numerous nano material, transition metal oxide is a class cheapness environment amenable transition metal oxide again, overall application is in fields such as electrocatalysis chemistry, ultracapacitor, lithium ion battery and magneticsubstances. and transition-metals and their oxides nano material, has that preparation is simple, morphology controllable and an electrochemical activity advantages of higher.Such as cobalt acid nickel has fabulous electroconductibility, and at least comparatively nickel oxide and high two orders of magnitude of cobalt oxide, also have higher electrochemical activity, can provide abundanter redox reaction (joint contribution of nickel ion and cobalt ion); Nickel oxide, cobalt oxide is because wide material sources, and easily prepare, lower-price characteristic is considered to alternative RuO 2ideal hyper capacitor material, people have also carried out large quantity research to it.Graphene and transition metal oxide be compounded with following advantage: first, the electric conductivity of transition metal oxide and high rate performance can reach obvious raising; Secondly, transition-metal oxide growth, on the surface of Graphene, prevents the reunion between transition metal oxide, substantially increases the electrochemically active specific surface area of electrode materials.Therefore, the chemical property of the matrix material of Graphene and transition metal oxide is better than simple transition-metal oxide usually.
Based on the potential using value of above-mentioned transition metal oxide, some researchists have synthesized different patterns and structure as nano wire, nanometer sheet and nano particle etc., but this matrix material is all generally the surface being laid in Graphene, such appearance structure can not make the outstanding chemical property of transition metal oxide better play.
Summary of the invention
In order to overcome the defect of the transition metal oxide nano-slice material of above-mentioned graphenic surface growth, the object of the present invention is to provide the method for the transition metal oxide nano-slice of graphenic surface growing upright, by the upright metal oxide nano-sheet that growth composition, structure and crystal formation on graphenic surface are controlled, the specific surface area greatly improving integral material with contact site, also improve the utilization ratio of material, universality simultaneously, thus improve performance.
In order to achieve the above object, technical scheme of the present invention is:
The method of the transition metal oxide nano-slice of graphenic surface growing upright, comprises the following steps:
The first step: the stannic oxide/graphene nano sheet taking 10 ~ 500mg, joins in the deionized water of 10 ~ 500mL, ultrasonic disperse 1 ~ 60 minute, described ultrasonic power is 250W; Then add the transition metal salt compounds of at least one 10 ~ 1000mg successively, 5 ~ 100mg Trisodium Citrate and 10 ~ 500mg hexamethylenetetramine, then stirring reaction 2 ~ 12 hours at 80 ~ 90 DEG C, stirring velocity is 400r/m; By the product centrifugation obtained, then use ethanol eccentric cleaning 1 ~ 10 time, drying for standby; Described transition metal salt compounds comprises Nickelous nitrate hexahydrate, Cobaltous nitrate hexahydrate, zinc nitrate hexahydrate and manganese nitrate hexahydrate.
Second step: by the product in the first step in nitrogen tube furnace 250 DEG C ~ 450 DEG C calcining 1 ~ 4 hour, temperature rise rate is 1 ~ 5 DEG C of min -1; The powder obtained is the transition metal oxide nano-material of growing upright on Graphene.
X-ray diffraction shows that product is made up of Graphene and transition-metal oxide.
On the Graphene utilizing the present invention to prepare, the transition-metal oxide nano material of growing upright has a little following: 1 higher specific surface area, thus can provide more active reaction sites, thus improves chemical property; 2 upright nanometer sheet can fully and electrolyte contacts; 3 can improve the utilization ratio of material in graphenic surface growing upright nanometer sheet, thus improve chemical property.
Embodiment
Embodiment one
The present embodiment comprises the following steps:
The first step: the stannic oxide/graphene nano sheet taking 10mg, joins in the deionized water of 40mL, ultrasonic disperse 5 minutes, described ultrasonic power is 250W; Then 97.3mgNi (NO is added successively 3) 26H 2o, 150mgCo (NO 3) 26H 2o, 7.7mg Trisodium Citrate and 35.3mg hexamethylenetetramine, then stirring reaction 3 hours at 90 DEG C, stirring velocity is 400r/m; By the product centrifugation obtained, then use ethanol eccentric cleaning 5 times, drying for standby;
Second step: by the product in the first step in nitrogen tube furnace 300 DEG C calcining 2 hours, temperature rise rate is 1 DEG C of min -1; The powder obtained is the cobalt acid nickel nano material of growing upright on Graphene.
X-ray diffraction shows that product is made up of Graphene and cobalt acid nickel.Tested by super capacitor, on Graphene, the cobalt acid nickel nano material of growing upright is 10Ag in current density -1lower ratio capacitance reaches 1500C.
Embodiment two
The present embodiment comprises the following steps:
The first step: the stannic oxide/graphene nano sheet taking 5mg, joins in the deionized water of 40mL, ultrasonic disperse 10 minutes, described ultrasonic power is 250W; Then 75mgZn (NO is added successively 3) 26H 2o, 150mgCo (NO 3) 26H 2o, 7.25mg Trisodium Citrate and 35mg hexamethylenetetramine, then stirring reaction 5 hours at 90 DEG C, stirring velocity is 400r/m; By the product centrifugation obtained, then use ethanol eccentric cleaning 5 times, drying for standby;
Second step: by the product in the first step in nitrogen tube furnace 400 DEG C calcining 2 hours, temperature rise rate is 2 DEG C of min -1; The powder obtained is the cobalt acid zinc nano material of growing upright on Graphene.
X-ray diffraction shows that product is made up of Graphene and cobalt acid zinc.Tested by lithium ion battery, on Graphene, the cobalt acid zinc nano material of growing upright is 100mAg in current density -1lower ratio capacitance reaches 1300mAhg -1.
Embodiment three
The present embodiment comprises the following steps:
The first step: the stannic oxide/graphene nano sheet taking 20mg, joins in the deionized water of 80mL, ultrasonic disperse 15 minutes, described ultrasonic power is 250W; Then 194.6mgNi (NO is added successively 3) 26H 2o, 15.4mg Trisodium Citrate and 70.6mg hexamethylenetetramine, then stirring reaction 6 hours at 90 DEG C, stirring velocity is 400r/m; By the product centrifugation obtained, then use ethanol eccentric cleaning 5 times, drying for standby;
Second step: by the product in the first step in nitrogen tube furnace 450 DEG C calcining 3 hours, temperature rise rate is 3 DEG C of min -1; The powder obtained is the nickel oxide nano material of growing upright on Graphene.
X-ray diffraction shows that product is made up of Graphene and nickel oxide.Tested by super capacitor, on Graphene, the nickel oxide nano material of growing upright is 10Ag in current density -1lower ratio capacitance reaches 1000C.
Embodiment four
The first step: the stannic oxide/graphene nano sheet taking 50mg, joins in the deionized water of 200mL, ultrasonic disperse 25 minutes, described ultrasonic power is 250W; Then 750mgCo (NO is added successively 3) 26H 2o, 38.5mg Trisodium Citrate and 176.5mg hexamethylenetetramine, then stirring reaction 6 hours at 90 DEG C, stirring velocity is 400r/m; By the product centrifugation obtained, then use ethanol eccentric cleaning 5 times, drying for standby;
Second step: by the product in the first step in nitrogen tube furnace 450 DEG C calcining 4 hours, temperature rise rate is 4 DEG C of min -1; The powder obtained is the cobalt oxide nano material of growing upright on Graphene.
X-ray diffraction shows that product is made up of Graphene and cobalt oxide.Tested by lithium ion battery, on Graphene, the cobalt oxide nano material of growing upright is 200mAg in current density -1lower ratio capacitance reaches 879mAhg -1.
Embodiment five
The present embodiment comprises the following steps:
The first step: the stannic oxide/graphene nano sheet taking 10mg, joins in the deionized water of 400mL, ultrasonic disperse 40 minutes, described ultrasonic power is 250W; Then 63mgMn (NO is added successively 3) 26H 2o, 150mgZn (NO 3) 26H 2o, 77mg Trisodium Citrate and 353mg hexamethylenetetramine, then stirring reaction 8 hours at 90 DEG C, stirring velocity is 400r/m; By the product centrifugation obtained, then use ethanol eccentric cleaning 10 times, drying for standby;
Second step: by the product in the first step in nitrogen tube furnace 350 DEG C calcining 2 hours, temperature rise rate is 5 DEG C of min -1; The powder obtained is the zinc permanganate nano material of growing upright on Graphene.
X-ray diffraction shows that product is made up of Graphene and zinc permanganate.Tested by lithium ion battery, on Graphene, the cobalt oxide nano material of growing upright is 200mAg in current density -1lower ratio capacitance reaches 785mAhg -1.

Claims (6)

1. the method for the transition metal oxide nano-slice of graphenic surface growing upright, is characterized in that, comprises the following steps:
The first step: the stannic oxide/graphene nano sheet taking 10 ~ 500mg, joins in the deionized water of 10 ~ 500mL, ultrasonic disperse 1 ~ 60 minute, described ultrasonic power is 250W; Then add the transition metal salt compounds of at least one 10 ~ 1000mg successively, 5 ~ 100mg Trisodium Citrate and 10 ~ 500mg hexamethylenetetramine, then stirring reaction 2 ~ 12 hours at 80 ~ 90 DEG C, stirring velocity is 400r/m; By the product centrifugation obtained, then use ethanol eccentric cleaning 1 ~ 10 time, drying for standby; Described transition metal salt compounds comprises Nickelous nitrate hexahydrate, Cobaltous nitrate hexahydrate, zinc nitrate hexahydrate and manganese nitrate hexahydrate;
Second step: by the product in the first step in nitrogen tube furnace 250 DEG C ~ 450 DEG C calcining 1 ~ 4 hour, temperature rise rate is 1 ~ 5 DEG C of min -1; The powder obtained is the transition metal oxide nano-material of growing upright on Graphene.
2. the method for the transition metal oxide nano-slice of graphenic surface growing upright according to claim 1, is characterized in that, comprise the following steps:
The first step: the stannic oxide/graphene nano sheet taking 10mg, joins in the deionized water of 40mL, ultrasonic disperse 5 minutes, described ultrasonic power is 250W; Then 97.3mgNi (NO is added successively 3) 26H 2o, 150mgCo (NO 3) 26H 2o, 7.7mg Trisodium Citrate and 35.3mg hexamethylenetetramine, then stirring reaction 3 hours at 90 DEG C, stirring velocity is 400r/m; By the product centrifugation obtained, then use ethanol eccentric cleaning 5 times, drying for standby;
Second step: by the product in the first step in nitrogen tube furnace 300 DEG C calcining 2 hours, temperature rise rate is 1 DEG C of min -1; The powder obtained is the cobalt acid nickel nano material of growing upright on Graphene.
3. the method for the transition metal oxide nano-slice of graphenic surface growing upright according to claim 1, is characterized in that, comprise the following steps:
The first step: the stannic oxide/graphene nano sheet taking 5mg, joins in the deionized water of 40mL, ultrasonic disperse 10 minutes, described ultrasonic power is 250W; Then 75mgZn (NO is added successively 3) 26H 2o, 150mgCo (NO 3) 26H 2o, 7.25mg Trisodium Citrate and 35mg hexamethylenetetramine, then stirring reaction 5 hours at 90 DEG C, stirring velocity is 400r/m; By the product centrifugation obtained, then use ethanol eccentric cleaning 5 times, drying for standby;
Second step: by the product in the first step in nitrogen tube furnace 400 DEG C calcining 2 hours, temperature rise rate is 2 DEG C of min -1; The powder obtained is the cobalt acid zinc nano material of growing upright on Graphene.
4. the method for the transition metal oxide nano-slice of graphenic surface growing upright according to claim 1, is characterized in that, comprise the following steps:
The first step: the stannic oxide/graphene nano sheet taking 20mg, joins in the deionized water of 80mL, ultrasonic disperse 15 minutes, described ultrasonic power is 250W; Then 194.6mgNi (NO is added successively 3) 26H 2o, 15.4mg Trisodium Citrate and 70.6mg hexamethylenetetramine, then stirring reaction 6 hours at 90 DEG C, stirring velocity is 400r/m; By the product centrifugation obtained, then use ethanol eccentric cleaning 5 times, drying for standby;
Second step: by the product in the first step in nitrogen tube furnace 450 DEG C calcining 3 hours, temperature rise rate is 3 DEG C of min -1; The powder obtained is the nickel oxide nano material of growing upright on Graphene.
5. the method for the transition metal oxide nano-slice of graphenic surface growing upright according to claim 1, is characterized in that, comprise the following steps:
The first step: the stannic oxide/graphene nano sheet taking 50mg, joins in the deionized water of 200mL, ultrasonic disperse 25 minutes, described ultrasonic power is 250W; Then 750mgCo (NO is added successively 3) 26H 2o, 38.5mg Trisodium Citrate and 176.5mg hexamethylenetetramine, then stirring reaction 6 hours at 90 DEG C, stirring velocity is 400r/m; By the product centrifugation obtained, then use ethanol eccentric cleaning 5 times, drying for standby;
Second step: by the product in the first step in nitrogen tube furnace 450 DEG C calcining 4 hours, temperature rise rate is 4 DEG C of min -1; The powder obtained is the cobalt oxide nano material of growing upright on Graphene.
6. the method for the transition metal oxide nano-slice of graphenic surface growing upright according to claim 1, is characterized in that, comprise the following steps:
The first step: the stannic oxide/graphene nano sheet taking 10mg, joins in the deionized water of 400mL, ultrasonic disperse 40 minutes, described ultrasonic power is 250W; Then 63mgMn (NO is added successively 3) 26H 2o, 150mgZn (NO 3) 26H 2o, 77mg Trisodium Citrate and 353mg hexamethylenetetramine, then stirring reaction 8 hours at 90 DEG C, stirring velocity is 400r/m; By the product centrifugation obtained, then use ethanol eccentric cleaning 10 times, drying for standby;
Second step: by the product in the first step in nitrogen tube furnace 350 DEG C calcining 2 hours, temperature rise rate is 5 DEG C of min -1; The powder obtained is the zinc permanganate nano material of growing upright on Graphene.
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CN104599851A (en) * 2014-12-31 2015-05-06 江苏江大环保科技开发有限公司 Application of 3D coralline graphene/NiCo2O4 composite material
CN105225844B (en) * 2015-09-09 2017-10-31 南京航空航天大学 The preparation method of the sour zinc composite of nitrogen-doped graphene/nitrogen-doped carbon nanometer pipe/cobalt and application
CN106158418B (en) * 2016-07-14 2019-02-05 江苏大学 A kind of preparation method of NiO/ nitrogen-doped graphene composite nano-electrode material
CN106783210B (en) * 2017-02-06 2018-11-06 江苏大学 The preparation method of the hollow super electric material of nucleocapsid ZnCo2O4-RGO flexibilities
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CN107014952A (en) * 2017-02-28 2017-08-04 济南大学 A kind of rGO/ZnCo2O4The preparation method of/Au tri compound room temperature gas sensitive
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