CN106910638A - A kind of is carbon material and its preparation method and application of template based on Zr MOFs composites - Google Patents
A kind of is carbon material and its preparation method and application of template based on Zr MOFs composites Download PDFInfo
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- CN106910638A CN106910638A CN201710157272.6A CN201710157272A CN106910638A CN 106910638 A CN106910638 A CN 106910638A CN 201710157272 A CN201710157272 A CN 201710157272A CN 106910638 A CN106910638 A CN 106910638A
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- carbon material
- carboxylated graphene
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for 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
- Y02E60/13—Energy storage using capacitors
Abstract
It is the carbon material of template based on Zr MOFs composites that the present invention is provided a kind of, by amino terephthalic acid (TPA), ZrCl4With carboxylated Graphene, after hydro-thermal method synthesizes, heating carbonization treatment is prepared from, and the specific surface area scope of gained carbon material is in 1000 ~ 1973 m2g‑1.Its preparation method includes：（1）By amino terephthalic acid (TPA), ZrCl4With carboxylated Graphene and mixing, ultrasound；（2）By the NH of hydro-thermal method synthetic composite material UiO 662/ carboxylated graphene composite material；（3）Heating carbonization treatment is carried out, product is obtained；（4）Product is washed, is dried, you can obtain porous carbon material.Gained carbon material through electrochemical property test, as electrode material for super capacitor application when, when current density is 0.15Ag‑1, specific capacitance value scope is in 150 ~ 300 F g‑1.Therefore, in carbon material, particularly ultracapacitor field has broad application prospects the present invention.
Description
Technical field
The present invention relates to carbon material technical field, and in particular to a kind of is the carbon materials of template based on Zr-MOFs composites
Material and its preparation method and application.
Background technology
Ultracapacitor, is called double layer capacitor, is a kind of novel energy storage apparatus.It has that the charging interval is short, uses
The features such as long lifespan, good temp characteristic, energy saving and environmental protection.Material as capacitor have porous carbon-based, Graphene,
The transition metal oxide such as conducting polymer and ruthenium, iridium, manganese, nickel, vanadium.Porous carbon materials are a kind of with low density, height
Surface area, big pore volume, heat endurance and chemical stability feature high, are one of most attractive and important materials,
Because they have very wide application in many important technology fields, such as in terms of adsorbing separation, lithium battery, ultracapacitor
Application.
MOFs has been applied to gas storage and has separated, and is catalyzed and photoelectric magnetic property, the aspect such as medicament slow release and sensor.Cause
To possess orderly, uniform adjustable structure, the features such as specific surface area high, have than conventional porous materials more common with preceding
Scape.But because the MOFs of less stable has very big limit in terms of practice is used with development.For more common profit
The use of MOFs materials is promoted with the labile feature of MOFs material at high temperature, it is carbonized at high temperature prepares the nanometer of stabilization
Porous carbon materials.The carbon material of this local graphite possesses specific surface area higher and has preferable electric conductivity, chemically stable
Property, there is good prospect of the application in terms of electrochemistry.It is reported that after HKUST-1, MOF-5, Al-PCP high temperature cabonization
When the carbon material obtained through hydrofluoric acid treatment is as electrode material for super capacitor, in 100 mA g-1Current density under, specific volume
Amount is up to 232.8Fg-1, specific capacity it is relatively low [Applied Surface Science 2014, 308, 306-310.]。
The content of the invention
The purpose of the present invention be it is a kind of be carbon material and preparation method thereof of template and should based on Zr-MOFs composites
With, it is combined with MOFs materials by by Graphene, further enhance stability using both synergies, improve conductance
Rate, is applied to electrode material for super capacitor.
In order to realize foregoing invention purpose, the technical solution adopted by the present invention is：
Be the carbon material of template based on Zr-MOFs composites, by prepare the amino terephthalic acid (TPA) of certain mol proportion with
ZrCl4Mixture, then by carboxylated Graphene and mixture press certain mass than mixing ultrasonic mixing, by hydro-thermal method synthesize
Composite UiO-66-NH2/ carboxylated graphene composite material, by gained UiO-66-NH2/ carboxylated graphene composite material
It is placed in heating furnace, after carrying out heating carbonization treatment in an inert atmosphere, washing is dried.The specific surface area model of gained carbon material
It is trapped among 1000 ~ 1973 m2g-1。
Based on Zr-MOFs composites for the preparation method of the carbon material of template is comprised the following steps：
Step（1）, prepare the amino terephthalic acid (TPA) and ZrCl of certain mol proportion4Mixture, then by carboxylated Graphene and
Mixture presses certain mass than mixing, ultrasound, the amino terephthalic acid (TPA) and ZrCl4Mixture mol ratio be 1:1, institute
The mass ratio for stating carboxylated Graphene and mixture is 1：200；
Step（2）, will mix, the good sample of ultrasound passes through hydro-thermal method synthetic composite material UiO-66-NH2/ carboxylated Graphene
Composite,；
Step（3）, by UiO-66-NH2/ carboxylated graphene composite material is heated in an inert atmosphere in being put into heating furnace
Carbonization treatment, obtains product, and the temperature range of the heating carbonization treatment is 600 ~ 900 DEG C, and time range is 5 ~ 500min；
Step（4）, product is first used into hydrofluoric acid wash, then filtered with deionized water cyclic washing, then the sample collected is existed
Dried at a temperature of 120 DEG C, you can obtain porous carbon material.
Based on the carbon material that Zr-MOFs composites are template as the application of electrode material for super capacitor, work as electric current
Density is 0.15A g-1When, specific capacitance value scope is in 150 ~ 300 F g-1。
The nitrogen adsorption desorption performance test of carbon material of the present invention is the Quantachrome in U.S.'s Quanta instrument manufacturings
Carried out on ASIQM0002-4 type physical adsorption appearances, test result shows：The typical IV nitrogen adsorption desorption of the materials show is bent
Line, with abundant micropore and mesopore orbit structure, there is a specific surface area higher, the specific surface area scope of material 1000 ~
1973 m2g-1。
The electrochemical property test of carbon material of the present invention is carried out on electrochemical workstation（Chenhua Co. Ltd.,
Shanghai, China）Use three electrode test systems.Test result shows：Under different sweep speeds, circulation volt
Peace curve keeps good similar to rectangular shape and has response current higher, with preferable electric double layer capacitance behavior with
In electrochemical reversibility, and the test of constant current charge-discharge, under different current densities, the carbon material has shown a mirror
As symmetrical triangular shaped, illustrate that there is preferable charge-discharge performance, when current density is 0.15Ag-1When, specific capacitance value model
It is trapped among 150 ~ 300 F g-1。
The present invention relative to prior art, with advantages below：
1. carboxylated Graphene and amino terephthalic acid (TPA) and ZrCl are utilized in the present invention4Mixture by hydro-thermal method synthesize
Zr-MOFs composites, gained composite is carried out in an inert atmosphere heat the carbon material prepared of carbonization treatment has
Uniform and stable structure, and the structure of original graphite alkene is still maintain, be conducive to improving material conductivity and chemical stability；
2. carbon material is prepared for template based on Zr-MOFs composites, stencil-chosen simple and efficient with preparation means
Property variation, the features such as the controllability of carbon material duct；
3. the specific surface area highest of carbon material of the present invention has reached 1973 m2g-1, and with excellent stability；
4th, carbon material of the present invention has specific capacitance high, when current density is 0.15Ag-1When, specific capacitance value reaches 234 Fg-1.,
Can be widely applied to the electrode material of ultracapacitor.
Therefore, in electrode material, particularly ultracapacitor field has broad application prospects the present invention.
Brief description of the drawings：
Fig. 1 is the low temperature nitrogen adsorption isothermal curve of specific embodiment 1；
Fig. 2 is the electric capacity cyclic voltammogram of carbon material prepared by specific embodiment 1；
Fig. 3 is the capacitor charge and discharge performance plot of the carbon material of specific embodiment 1；
Fig. 4 is the low temperature nitrogen adsorption isothermal curve of specific embodiment 2；
Fig. 5 is the electric capacity cyclic voltammogram of carbon material prepared by specific embodiment 2；
Fig. 6 is the capacitor charge and discharge performance plot of the carbon material of specific embodiment 2.
Specific embodiment
The present invention is described in further detail, but be not right with reference to Figure of description by embodiment to present invention
Limitation of the invention.
Embodiment 1
The present invention is based on Zr-MOFs composites for the concrete operation step of the carbon materials preparation method for material of template is as follows：
Step（1）, quality is taken for (1.0mmol) ZrCl4With amino terephthalic acid (TPA)（H2BDC, 1.0mmol）With 20 mL's
Both DMF solvent ultrasound arrangement mixed solutions, take the carboxylated Graphene that quality is said mixture 0.5%, with the N of 15 mL,
Dinethylformamide（DMF）Solvent supersonic configures graphene solution, and all solution ultrasonic mixings that will be prepared afterwards are uniform；
Step（2）, all solution that will be prepared are transferred in stainless steel cauldron, by reactor be placed in advance temperature control at 120 DEG C
Baking oven in react, be incubated 48 h, the precipitation of gained carries out centrifuge washing, filtering with DMF, is dried at 120 DEG C and obtained
Sample；
Step（3）, the sample that will be obtained is put into tube furnace, in N2Heating carbonization treatment, the heating are carried out under inert atmosphere
The temperature of carbonization treatment is 800 DEG C, and the time is 5 ~ 500min；
Step（4）, product is first used into hydrofluoric acid wash, then filtered with deionized water cyclic washing, then the sample collected is existed
Dried at a temperature of 120 DEG C, you can porous carbon material needed for obtaining.
The low temperature nitrogen isothermal adsorption desorption performance test conditions of carbon material of the present invention deaerate 8 hours under the conditions of 200 DEG C, so
Isothermal nitrogen adsorption desorption test is carried out under the conditions of 77 K afterwards.Test result is as shown in figure 1, specific surface area is 1973m2g-1。
Carbon material of the present invention as electrode material for super capacitor application, the performance test of its electrochemistry is in electrochemistry work
Carried out on standing.Including cyclic voltammetry curve, test result as shown in Fig. 2 under different sweep speeds, cyclic voltammetry curve
Keep good similar to rectangular shape, show with preferable electric double layer capacitance behavior and electrochemical reversibility.Constant current fills
Discharge test, test result are as shown in figure 3, current density is 0.15Ag-1When, specific capacitance value is up to 234 Fg-1。
Embodiment 2
Not specified step is same as Example 1, and difference is：Step（3）, the temperature of heating carbonization treatment be
900℃。
The low temperature nitrogen isothermal adsorption performance test conditions of carbon material of the present invention are to be deaerated 8 hours under the conditions of 200 DEG C, so
Isothermal nitrogen adsorption desorption test is carried out under the conditions of 77 K afterwards.Result is as shown in figure 4, the resulting materials specific surface area of embodiment 2 reaches
To 1315 m2g-1。
Carbon material of the present invention as electrode material for super capacitor application, the performance test of its electrochemistry is in electrochemistry work
Carried out on standing.Including cyclic voltammetry curve, test result as shown in figure 5, under different sweep speeds, cyclic voltammetry curve
Keep good similar to rectangular shape, show with preferable electric double layer capacitance behavior and electrochemical reversibility.Constant current fills
Discharge test, test result are as shown in fig. 6, under different current densities, shown a triangle shape for specular
Shape, illustrates there is the performance of preferable electrochemistry.Current density is 0.15Ag-1When, specific capacitance value reaches 150 Fg-1。
Claims (7)
1. a kind of is the carbon material of template based on Zr-MOFs composites, it is characterised in that：The carbon material is by amino to benzene two
Formic acid, ZrCl4With carboxylated Graphene, by hydro-thermal method synthetic composite material UiO-66-NH2/ carboxylated graphene composite material
Afterwards, it is placed in heating furnace, after carrying out heating carbonization treatment in an inert atmosphere, is washed, dries and obtain.
2. carbon material according to claim 1, it is characterised in that：The specific surface area scope of described carbon material 1000 ~
1973 m2g-1。
3. the preparation method of carbon material according to claim 1, it is characterised in that comprise the following steps：
Step（1）, prepare the amino terephthalic acid (TPA) and ZrCl of certain mol proportion4Mixture, then by carboxylated Graphene and mixed
Compound presses certain mass than mixing, ultrasound；
Step（2）, will mix, the good sample of ultrasound passes through hydro-thermal method synthetic composite material UiO-66-NH2/ carboxylated Graphene is answered
Condensation material；
Step（3）, by UiO-66-NH2/ carboxylated graphene composite material is heated in an inert atmosphere in being put into heating furnace
Carbonization treatment, obtains product；
Step（4）, product is first used into hydrofluoric acid wash, then filtered with deionized water cyclic washing, then the sample collected is existed
Dried at a temperature of 120 DEG C, you can obtain porous carbon material.
4. preparation method according to claim 3, it is characterised in that：The step（1）Amino terephthalic acid (TPA) and ZrCl4
Mixture mol ratio be 1:1.
5. preparation method according to claim 3, it is characterised in that：The step（1）Carboxylated Graphene and mixture
Mass ratio be 1：200.
6. preparation method according to claim 3, it is characterised in that：The step（3）Heat the temperature model of carbonization treatment
It is 600 ~ 900 DEG C to enclose, and time range is 5 ~ 500min.
7. carbon material according to claim 1 as electrode material for super capacitor application, it is characterised in that：Work as electric current
Density is 0.15A g-1When, specific capacitance value scope is in 150 ~ 300 F g-1。
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| CN107578927A (en) * | 2017-09-07 | 2018-01-12 | 陕西科技大学 | A kind of preparation method of polyaniline MOF nano composite material flexible super capacitors |
| CN108328706A (en) * | 2018-01-15 | 2018-07-27 | 浙江工业大学 | A kind of MOF derives the preparation and application of porous carbon/graphene combination electrode material |
| GB2565044A (en) * | 2017-07-05 | 2019-02-06 | Zewail City Of Science And Tech | Composite |
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| CN110305331A (en) * | 2019-07-02 | 2019-10-08 | 南开大学 | The method that ligand selection reservation method constructs multi-stage porous MOF |
| CN110931271A (en) * | 2019-12-24 | 2020-03-27 | 桂林电子科技大学 | Preparation and application of hydrophobic Schiff base cobalt @ β cyclodextrin-graphene porous carbon composite material |
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| CN116081686A (en) * | 2023-02-13 | 2023-05-09 | 中国人民解放军国防科技大学 | Nano ZrO 2 C heat-resistant wave-absorbing material and preparation method thereof |
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| CN110931271B (en) * | 2019-12-24 | 2021-04-13 | 桂林电子科技大学 | Preparation and application of hydrophobic Schiff base cobalt @ beta cyclodextrin-graphene porous carbon composite material |
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| CN114652306A (en) * | 2022-03-17 | 2022-06-24 | 电子科技大学 | MOFs-based fingertip contact type noninvasive sweat glucose sensor and method |
| CN116081686A (en) * | 2023-02-13 | 2023-05-09 | 中国人民解放军国防科技大学 | Nano ZrO 2 C heat-resistant wave-absorbing material and preparation method thereof |
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