CN108539144A - A kind of extra small metal organic frame is nanocrystalline and preparation method and application - Google Patents
A kind of extra small metal organic frame is nanocrystalline and preparation method and application Download PDFInfo
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- CN108539144A CN108539144A CN201810199024.2A CN201810199024A CN108539144A CN 108539144 A CN108539144 A CN 108539144A CN 201810199024 A CN201810199024 A CN 201810199024A CN 108539144 A CN108539144 A CN 108539144A
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The invention belongs to field of material preparation, specially a kind of extra small metal organic frame is nanocrystalline and preparation method and application.Step of the present invention is：The first homoepitaxial large scale metal-organic framework material in graphene oxide layer, then polymer wraps up metal-organic framework material by in-situ polymerization, it calcines in air, it is nanocrystalline to obtain super-small metal-organic framework material by the atomizing of heat auxiliary.Advantage of the present invention：Preparation method is simple, and raw material is cheap and easy to get, and low energy consumption for preparation process, the nanocrystalline size uniformity of metal-organic framework material of preparation（~5 nm）.When the material may be directly applied to lithium ion battery negative material, active material utilization is high, and the specific capacity based on entire electrode is big（1301 mAh g‑1）, have extended cycle life（Capacity retention ratio has 98.6% after 1000 circles）, it is expected to become next-generation lithium ion battery material.
Description
Technical field
The invention belongs to technical field of material, and in particular to a kind of extra small metal organic frame is nanocrystalline and preparation side
Method and application.
Background technology
The advantages that metal organic frame can easily be accommodated due to its big pore volume, higher specific surface area, pore size, can be with
It is widely used in gas separation and storage, catalyst and catalyst carrier, light absorption and conversion, ultracapacitor, secondary electricity
The multiple fields such as pond, pharmaceutical carrier.Meanwhile when a kind of scantling is reduced to nanoscale, physicochemical properties can be sent out
Life significantly changes, therefore people invent many methods and prepare extra small nano material, these conventional methods include：Laser synthesizing adds
Work, ultrasound or microwave treatment, quickly heating, atom or molecular-layer deposition etc..But on the one hand unsuitable prepare of these methods surpasses
Small metal-organic framework material, because of the unstability of metal-organic framework material under some extreme conditions, on the other hand,
In certain method preparation process it is comparatively laborious, it is expensive, be unfavorable for preparing on a large scale.Therefore, inventing a kind of low cost can be big
Scale prepares the nanocrystalline method of extra small metal organic frame with regard to particularly important.
Invention content
The object of the present invention is to provide a kind of simple, quick, safety extra small metal organic frame is nanocrystalline and its prepare
Methods and applications.
Extra small metal organic frame nanometer crystal preparation method provided by the present invention, is as follows：
（1）Prepare graphene oxide presoma：
It is prepared using Hummers methods are improved, that is, takes 1 ~ 3g, 325 mesh graphite powders, the sodium nitrate powder and 40 ~ 120 of 1 ~ 2g is added
The ml concentrated sulfuric acids are slowly added to 3 ~ 9 g potassium permanganate under cold bath, in 30 ~ 40 DEG C of 0.5 h of stirred in water bath, then it is added 50 ~
100 ml water, the reaction was continued 10 ~ 30 min add the water of 200 ~ 400 ml, react 5 ~ 20 min, are then added 10 ~ 30
3% hydrogen peroxide of ml to solution becomes golden yellow；
Decantation removes supernatant liquor after solution left standstill is settled, and the hydrochloric acid that mass concentration is 10% is added, is distributed into centrifuge tube
High speed centrifugation discards supernatant liquor, and 10000 ~ 12000 r/min of high speed centrifugation rotating speed is then washed with deionized water to neutrality, will
Collection of products after washing, is added deionized water ultrasonic disperse, and low-speed centrifugal takes supernatant to obtain graphene oxide（GO）It is water-soluble
Liquid, 2000 ~ 5000 r/min of low-speed centrifugal rotating speed；
（2）Prepare graphene oxide/metal organic frame/high molecular compound：
Cobalt chloride and sodium ferricyanide solution are configured first；0.4 ~ 2 mg/mL graphene oxide water solutions are added in cobalt chloride solution
In, stirring ultrasound；Above-mentioned solution is added in sodium ferricyanide solution, 0.5 ~ 1.5h is stirred, it is organic that graphene oxide/metal can be obtained
Frame compound；Then ammonium persulfate and pyrrole monomer are sequentially added, continues stirring 8 ~ 12 hours, centrifugation, washing can be obtained
Graphene oxide/metal organic frame/high molecular compound；By freeze-drying, so that it may to obtain composite aerogel；
（3）It is nanocrystalline to prepare extra small metal organic frame
By step（2）The composite aerogel of gained is calcined in air atmosphere has machine frame to get to carbon-coated extra small metal
The nanocrystalline aeroge of frame.
Step of the present invention（1）In, a concentration of 0.4 ~ 2 mg/mL of graphene oxide water solution.
Step of the present invention（2）In, the sodium ferricyanide and cobalt chloride concentration are 0.1 ~ 1 mol/ml.
Step of the present invention（2）In, the freeze-drying of graphene oxide/metal organic frame/high molecular compound uses
Freeze dryer is put into before freeze dryer and first puts 1 ~ 3h in -20 ~ 0 DEG C of refrigerator, then freeze-drying time be 16 ~ for 24 hours.
Step of the present invention（3）In, calcination temperature is controlled at 150 ~ 400 DEG C.
The carbon-coated extra small nanocrystalline aeroge of metal organic frame of the present invention, can be not required to directly as negative material
Add additional conductive additive and binder.
Advantages of the present invention：By metal ion due to it is positively charged can be with adsorbed close in surface of graphene oxide, so
The metal organic frame particle that organic ligand can be obtained by even size distribution is added afterwards.It then can by in-situ polymerization
To obtain the metal organic frame particle of polymeric PTC materials；It calcines, is obtained by the atomization process of heat auxiliary extra small in air
Size metallic organic framework materials are nanocrystalline.Meanwhile preparation method of the present invention is simple, raw material is cheap and easy to get, the metal frame of preparation
The nanocrystalline size of frame material is small, and is evenly distributed（~5 nm）.As lithium ion battery negative material, active material utilization is high,
Specific capacity based on entire electrode is big（1301 mAh g-1）, have extended cycle life（Capacity retention ratio has 98.6% after 1000 circles）, have
Hoping becomes next-generation lithium ion battery material.
Description of the drawings
Fig. 1 is the transmission electron microscope picture of graphene oxide/metal organic frame/high molecular compound.
Fig. 2 is the nanocrystalline transmission electron microscope of the carbon-coated extra small metal organic frame that is formed after compound calcining in Fig. 1
Picture.
Fig. 3 is the Fourier transform infrared spectrum that the carbon-coated extra small organic metal framework that is formed is nanocrystalline after calcining.
Fig. 4 is that carbon-coated extra small metal organic frame nanocomposite object is assembled into half-cell with lithium piece, in different electricity
Charging and discharging curve under current density, specific capacity are calculated based on entire electrode quality.
Fig. 5 is that carbon-coated extra small metal organic frame is nanocrystalline is assembled into half-cell with lithium piece, in 5,10 A g-1Under
Cycle charge discharge capacitance keeps curve, and specific capacity is calculated based on entire electrode quality.
Specific implementation mode
Technical scheme of the present invention is further described with reference to embodiment, but is not limited to following embodiment,
It is every that technical solution of the present invention is modified or replaced equivalently, without departing from the range of technical solution of the present invention, belong to
The scope of protection of the invention.
A kind of preparation method that extra small metal organic frame is nanocrystalline, by Electrostatic Absorption and coordination in graphite oxide
Alkene surface homoepitaxial metal organic frame particle, it is then uniform in metal organic frame particle surface by in-situ polymerization mode
Wrap up high molecular material.Graphene oxide/metal organic frame/polymer aerogel is obtained by freeze-drying.It finally will be upper
It states aeroge and calcines that can be obtained carbon-coated extra small metal organic frame nanocrystalline in air atmosphere.
Embodiment 1：
（1）Prepare graphene oxide presoma：
It is prepared using Hummers methods are improved, that is, takes 325 mesh graphite powders of 3g, the sodium nitrate powder and the dense sulphur of 120 ml of 2g is added
Acid is slowly added to 9 g potassium permanganate under cold bath, and in 30 ~ 40 DEG C of 0.5 h of stirred in water bath, the water of 100ml is then added,
The reaction was continued 30 min add 400ml deionized waters, react 5 ~ 20 min, and 30 ml, 3% hydrogen peroxide is then added to molten
Liquid becomes golden yellow.
Decantation removes supernatant liquor after solution left standstill is settled, and 10% hydrochloric acid is added, and is distributed into the centrifugation of centrifuge tube high speed
Supernatant liquor is discarded, 10000 ~ 12000 r/min of high speed centrifugation rotating speed is then washed with deionized water to neutrality, will be produced after washing
Object is collected, and deionized water ultrasonic disperse is added, and low-speed centrifugal takes supernatant to obtain graphene oxide water solution, and low-speed centrifugal turns
2000 ~ 5000 r/min of speed.
（2）Prepare the compound of polymer/metal organic frame/graphene oxide：
1 mol/L cobalt chlorides and sodium ferricyanide solution are configured first.0.4 ~ 2 mg/mL oxidations are added in 0.2 ml cobalt chloride solutions
In graphene aqueous solution, stirring ultrasound；2ml sodium ferricyanide solution is continuously added, 1h is stirred, metal organic frame/oxygen can be obtained
Then graphite alkene compound sequentially adds ammonium persulfate and pyrrole monomer, continue stirring 8 ~ 12 hours, centrifugation, washing
Obtain the compound of polymer/metal organic frame/graphene oxide.Compound airsetting is can be obtained by by freeze-drying
Glue.
Fig. 1 is the transmission electron microscope picture of graphene oxide/metal organic frame/high molecular compound, shows that metal has
Machine frame frame material is coated on well in graphene oxide/macromolecule.
（3）It is nanocrystalline to prepare extra small metal organic frame
It will（2）The aeroge of gained calcines 2h in air atmosphere, at 350 DEG C and can be obtained by carbon-coated extra small metal and have
The nanocrystalline aeroge of machine frame.
Fig. 2 is the transmission electron microscope picture that the carbon-coated extra small metal organic frame that is formed is nanocrystalline after calcining, shows gold
It is nanocrystalline that category organic framework materials are divided into equally distributed extra small metal organic frame.Fig. 3 is carbon-coated extra small organic gold
Belong to the nanocrystalline Fourier transform infrared spectrum of frame, shows that the extra small metal organic frame for calcining formation in air is nanocrystalline
Component does not change, and there is no aoxidized.
（4）Using the carbon-coated extra small nanocrystalline aeroge of metal organic frame of gained as negative material and lithium piece in hand
Half-cell is assembled into casing, diaphragm is polypropylene（Celgard 2400）, electrolyte is 1 M LiPF6It is dissolved in carbonic acid second
Enester（EC）And dimethyl carbonate（DME）In mixed liquor（Volume ratio is 1:1）.Charge-discharge test is carried out after battery standing 12h,
Voltage range be 0.01 ~ 3V, specific capacity according to entire anode Mass Calculation.
Fig. 4 is half-cell under different current densities（0.1~40 A g-1）Under constant current charge-discharge curve, 0.1 A g-1Specific discharge capacity reaches 1301 mAh g-1.Fig. 5 is half-cell in 5 and 10 A g-1Under cycle charge discharge capacitance keep bent
Line, specific capacity retention rate is respectively 92.9% and 98.6% after 500 circle of cycle.
Embodiment 2：
1 mg/mL graphene oxide water solutions are obtained by the method in above-described embodiment 1, under stiring respectively by 0.2 ml's
Cobalt chloride（0.5 mol/L）And 2ml sodium ferricyanide solution（0.5 mol/L）It is added in graphene oxide water solution, stirs 30min
After stand 30 min, be centrifuged off supernatant, remaining solid is scattered in deionized water.120 microlitres of pyrroles are added to above-mentioned
Solution carries out in-situ polymerization, is then centrifuged for removing supernatant, remaining solid is scattered in deionized water.
For 24 hours by the freeze-drying of above-mentioned solution, graphene oxide/metal organic frame/macromolecule airsetting of self-supporting is obtained
Glue.The aeroge is calcined into 2h at 300 DEG C in air atmosphere and can be obtained the nanocrystalline material of the extra small metal organic frame of carbon coating
Material.
Embodiment 3：
0.5 mg/mL GO aqueous solutions are obtained by the method in above-described embodiment 1, under stiring respectively by the cobalt chloride of 0.2 ml
（0.5 mol/L）And 2ml sodium ferricyanide solution（0.5 mol/L）It is added in GO aqueous solutions, continues to stand 30 after stirring 30min
Min is centrifuged off supernatant, and remaining solid is scattered in deionized water, is uniformly dispersed.60 microlitres of pyrroles are added to above-mentioned molten
Liquid carries out in-situ polymerization, is then centrifuged for removing supernatant, remaining solid is scattered in deionized water.
By above-mentioned solution be freeze-dried 16 ~ for 24 hours, obtain graphene oxide/metal organic frame/macromolecule gas of self-supporting
Gel.The aeroge in air atmosphere at 350 DEG C is calcined 2h, and to can be obtained the extra small metal organic frame of carbon coating nanocrystalline
Material.
Claims (7)
1. a kind of preparation method that extra small metal organic frame is nanocrystalline, which is characterized in that be as follows：
（1）Prepare graphene oxide presoma：
It is prepared using Hummers methods are improved, that is, takes 1 ~ 3g, 325 mesh graphite powders, the sodium nitrate powder and 40 ~ 120 of 1 ~ 2g is added
The ml concentrated sulfuric acids are slowly added to 3 ~ 9 g potassium permanganate under cold bath, in 30 ~ 40 DEG C of 0.5 h of stirred in water bath, then it is added 50 ~
100 ml water, the reaction was continued 10 ~ 30 min add the water of 200 ~ 400 ml, react 5 ~ 20 min, are then added 10 ~ 30
3% hydrogen peroxide of ml to solution becomes golden yellow；
Decantation removes supernatant liquor after solution left standstill is settled, and the hydrochloric acid of mass concentration 10% is added, is distributed into centrifuge tube high speed
Centrifugation discards supernatant liquor, and 10000 ~ 12000 r/min of high speed centrifugation rotating speed is then washed with deionized water to neutrality, will wash
Collection of products afterwards, is added deionized water ultrasonic disperse, and low-speed centrifugal takes supernatant to obtain graphene oxide（GO）Aqueous solution is low
2000 ~ 5000 r/min of fast centrifugal rotational speed；
（2）Prepare graphene oxide/metal organic frame/high molecular compound：
Cobalt chloride and sodium ferricyanide solution are configured first；0.4 ~ 2 mg/mL graphene oxide water solutions are added in cobalt chloride solution
In, stirring ultrasound；Above-mentioned solution is added in sodium ferricyanide solution, 1h is stirred, it is multiple that graphene oxide/metal organic frame can be obtained
Close object；Then ammonium persulfate and pyrrole monomer are sequentially added, continues stirring 8 ~ 12 hours, centrifugation, washing can be obtained oxidation stone
Black alkene/metal organic frame/high molecular compound；By freeze-drying, composite aerogel is obtained；
（3）It is nanocrystalline to prepare extra small metal organic frame
By step（2）The composite aerogel of gained is calcined in air atmosphere has machine frame to get to carbon-coated extra small metal
The nanocrystalline aeroge of frame.
2. the nanocrystalline preparation method of extra small metal organic frame as described in claim 1, which is characterized in that step（1）
In, a concentration of 0.4 ~ 2 mg/mL of graphene oxide water solution.
3. the nanocrystalline preparation method of extra small metal organic frame as described in claim 1, which is characterized in that step（2）
In, the sodium ferricyanide and cobalt chloride concentration are 0.1 ~ 1 mol/ml.
4. the nanocrystalline preparation method of extra small metal organic frame as described in claim 1, which is characterized in that step（2）In,
The freeze-drying of graphene oxide/metal organic frame/high molecular compound use freeze dryer, before being put into freeze dryer, first-
Put 1 ~ 3h in 20 ~ 0 DEG C of refrigerator, then freeze-drying time be 16 ~ for 24 hours.
5. the nanocrystalline preparation method of extra small metal organic frame as described in claim 1, which is characterized in that step（3）In,
Calcination temperature is 150 ~ 400 DEG C.
6. the extra small metal organic frame being prepared according to the preparation method described in claim 1 ~ 5 is nanocrystalline.
7. the nanocrystalline application in lithium ion battery electrode material of extra small metal organic frame as claimed in claim 6.
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Cited By (7)
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| CN110085819A (en) * | 2019-04-16 | 2019-08-02 | 浙江大学 | One kind mixing sodium potassium base cyaniding frame composite material and its preparation method and application |
| CN110218406A (en) * | 2019-05-29 | 2019-09-10 | 上海利物盛纳米科技有限公司 | A kind of temp auto-controlled heating material and preparation method thereof based on metal organic framework |
| CN110483831A (en) * | 2019-08-19 | 2019-11-22 | 浙江大学 | A kind of MOF aeroge and preparation method thereof |
| CN111554929A (en) * | 2020-05-06 | 2020-08-18 | 青岛科技大学 | Uniformly dispersed ultra-small metal nano particle material and dispersing method thereof |
| CN112023893A (en) * | 2020-09-21 | 2020-12-04 | 桂林理工大学 | MOF material capable of adsorbing heavy metal ions and preparation method thereof |
| CN113479871A (en) * | 2021-07-30 | 2021-10-08 | 绍兴文理学院 | Preparation method of in-situ self-growth-based ultra-small metal oxide nanoparticle modified graphene |
| CN113611541A (en) * | 2021-06-17 | 2021-11-05 | 三峡大学 | V2C @ Ni-MOF/NF material and application thereof as electrode material of supercapacitor |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110085819A (en) * | 2019-04-16 | 2019-08-02 | 浙江大学 | One kind mixing sodium potassium base cyaniding frame composite material and its preparation method and application |
| CN110085819B (en) * | 2019-04-16 | 2020-12-04 | 浙江大学 | Sodium-potassium-doped cyaniding framework composite material and preparation method and application thereof |
| CN110218406A (en) * | 2019-05-29 | 2019-09-10 | 上海利物盛纳米科技有限公司 | A kind of temp auto-controlled heating material and preparation method thereof based on metal organic framework |
| CN110218406B (en) * | 2019-05-29 | 2021-02-05 | 上海利物盛纳米科技有限公司 | Self-temperature-control heating material based on metal organic framework and preparation method thereof |
| CN110483831A (en) * | 2019-08-19 | 2019-11-22 | 浙江大学 | A kind of MOF aeroge and preparation method thereof |
| CN110483831B (en) * | 2019-08-19 | 2020-09-04 | 浙江大学 | MOF aerogel and preparation method thereof |
| CN111554929A (en) * | 2020-05-06 | 2020-08-18 | 青岛科技大学 | Uniformly dispersed ultra-small metal nano particle material and dispersing method thereof |
| CN112023893A (en) * | 2020-09-21 | 2020-12-04 | 桂林理工大学 | MOF material capable of adsorbing heavy metal ions and preparation method thereof |
| CN112023893B (en) * | 2020-09-21 | 2022-05-03 | 桂林理工大学 | MOF material capable of adsorbing heavy metal ions and preparation method thereof |
| CN113611541A (en) * | 2021-06-17 | 2021-11-05 | 三峡大学 | V2C @ Ni-MOF/NF material and application thereof as electrode material of supercapacitor |
| CN113479871A (en) * | 2021-07-30 | 2021-10-08 | 绍兴文理学院 | Preparation method of in-situ self-growth-based ultra-small metal oxide nanoparticle modified graphene |
| CN113479871B (en) * | 2021-07-30 | 2023-03-28 | 绍兴文理学院 | Preparation method of in-situ self-growth-based ultra-small metal oxide nanoparticle modified graphene |
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