CN110127654A - A kind of preparation method of uniform micron pore size three-dimensional carbon network - Google Patents
A kind of preparation method of uniform micron pore size three-dimensional carbon network Download PDFInfo
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- CN110127654A CN110127654A CN201910467743.2A CN201910467743A CN110127654A CN 110127654 A CN110127654 A CN 110127654A CN 201910467743 A CN201910467743 A CN 201910467743A CN 110127654 A CN110127654 A CN 110127654A
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- sodium chloride
- dimensional carbon
- carbon network
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- glucose
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
Abstract
The present invention relates to a kind of preparation methods of uniform micron pore size three-dimensional carbon network, including the following steps: 1) prepares salt template.2) it prepares presoma: glucose is dissolved in dehydrated alcohol, glucose and proportion of ethanol are no more than 1g/100mL, step 1) are added, sodium chloride crystal powder is made, and water-bath heat is dry, obtains the sodium chloride presoma of surface cladding glucose.3) it prepares three-dimensional carbon network: precursor powder made from step 2) is calcined under inert gas and hydrogen mixed gas atmosphere, obtain carbonized product, by draining for several times, is dried later to get micron pore size three-dimensional carbon network material is arrived again after carbonized product water-soaked.
Description
Technical field
The invention belongs to the preparation technical fields of nano material, and in particular to a kind of uniform micron pore size three-dimensional carbon network with
And the preparation of carried metal nanoparticle three-dimensional carbon nanometer network in situ.
Background technique
With well crystalline three-dimensional carbon network due to its big specific surface area, excellent electrical and thermal conductivity, excellent machine
Tool intensity, microwave absorbing property etc., in electrochemical material, the fields such as structural material are with a wide range of applications, and its is huge
Application potential is still under development.For example, in electrochemical field, three-dimensional carbon network is good load due to pore structure abundant
Body is usually used in the preparation of high-performance electrode capacitance material；In structural material field, good carbon backbone structure is composite material
Excellent reinforcement has critically important status in field of compound material.
Three-dimensional carbon network structure is generally completed by template, using gaseous state, liquid, solid-state carbon source, passes through hydro-thermal, solvent
Dry, freeze-drying of heat, heat etc. obtains presoma, recycles the technologies high temperature cabonizations such as chemical vapor deposition, finally again removes template.Three
The pore size for tieing up carbon network, is highly dependent on the particle size of template, and the catalysis of the crystallinity and template itself of carbon network is living
Property is related.Therefore, it is most important as template to choose a kind of material appropriate.Common template has two classes: the first kind is porous
Metal, granular metal, grain silicon etc., the catalytic activity that this class template has had itself, but the cost of template itself is very high, and
And the later period goes removing template to need to carry out chemical attack using acid solution or other corrosive liquids, increases preparation cost；Second class template
It is inorganic salts, generally inorganic salts is dissolved in the water together with carbon source, the means such as, freeze-drying dry by heat saltouts carbon source with inorganic
Out, then high temperature cabonization is carried out, goes removing template only to need to clean in water due to the later period, greatly reduces preparation cost.
But due to the crystallization property of inorganic salts, the unified particle of partial size is hardly resulted in precipitation process, is difficult to regulate and control as template
The pore size of three-dimensional carbon network, the material typically resulted in are difficult to accomplish that whole pore size is uniform.
Summary of the invention
In view of the shortcomings of the prior art, the invention proposes a kind of micron pore size three-dimensional carbon networks integrally having good uniformity
Preparation method, aperture is controllable, thickness is controllable, entirety is uniform, process is quick and easy, low in cost, yield is big, is suitble to extensive
Industrial output.The present invention utilizes the inorganic salts feature that the dissolubility in different solvents is different from carbon source, is first prepared inorganic
Then salt particle disperses as template in the solvent that carbon source is solvable, inorganic salts are insoluble, keep form stable, obtain carbon source packet
The presoma of template, subsequent high temperature cabonization are covered, last water washes off salt template and obtains three-dimensional carbon network material.Technical solution of the present invention
It is as follows:
A kind of preparation method of uniform micron pore size three-dimensional carbon network, including the following steps:
1) salt template is prepared
Sodium chloride solution is prepared, dehydrated alcohol is added, sodium chloride is precipitated, it is consistent by filtering and drying obtained partial size
Sodium chloride crystal powder is collected spare.
2) presoma is prepared
Glucose is dissolved in dehydrated alcohol, glucose and proportion of ethanol are no more than 1g/100mL, and step 1) is added and is made
Sodium chloride crystal powder, water-bath heat is dry, obtains the sodium chloride presoma of surface cladding glucose.
3) three-dimensional carbon network is prepared
Precursor powder made from step 2) is calcined under inert gas and hydrogen mixed gas atmosphere, carbonization is obtained and produces
Object, by draining for several times, is dried later to get micron pore size three-dimensional carbon network material is arrived again after carbonized product water-soaked.
Another way in step 2), in dehydrated alcohol, while being added and has deliquescent metal nitrate.It is described
Metal nitrate be copper nitrate, nickel nitrate or zinc nitrate.
Preferably, precursor powder made from step 2) is placed in tube furnace under argon gas and hydrogen mixed gas atmosphere, with 10
DEG C/min is warming up to 700-800 DEG C.
In conclusion technological core of the invention is chosen suitable molten using inorganic salts and the deliquescent difference of carbon source
Agent, inorganic salts, carbon source, do not destroy template, are made using inorganic salts as the presoma of template.Such as dehydrated alcohol, sodium chloride, grape
Sugar, the insoluble characteristic of sodium chloride using glucose slightly soluble in ethyl alcohol are made carbon source and coat sodium chloride presoma.It is solvent, inorganic
Salt, carbon source can select other types.Compared with prior art, advantage of the process is that
1) inorganic salts of size tunable are made as template, realize the uniform pore diameter of three-dimensional carbon network entirety
2) it using inorganic salts and the deliquescent difference of carbon source, does not destroy under the precursor of template, realizes carbon source for template
Uniform cladding, obtain presoma
3) carried metal nano particle in situ can be carried out to three-dimensional carbon network during preparing presoma
4) present invention process process time-consuming is short, low in cost, green non-pollution, large-scale production easy to accomplish
Detailed description of the invention
Fig. 1 is the SEM image of sodium chloride crystal template prepared by the present invention
Fig. 2 is the SEM image that glucose prepared by the present invention coats sodium chloride template presoma
Fig. 3 is SEM image of the presoma prepared by the present invention after high temperature reduction is carbonized
Fig. 4 is SEM image of the Copper-cladding Aluminum Bar presoma prepared by the present invention after high temperature reduction is carbonized
Fig. 5 is the SEM image of the three-dimensional carbon network surface topography prepared by the present invention after washing drying
Fig. 6 is the SEM image of the three-dimensional carbon network surface topography of the Copper-cladding Aluminum Bar prepared by the present invention after washing drying
Fig. 7 is the Raman map of three-dimensional carbon network prepared by the present invention
The present invention does not address place and is suitable for the prior art.
The specific implementation embodiment of preparation method of the present invention is given below.Embodiment is only used for further illustrating system of the present invention
Preparation Method is not intended to limit the protection scope of the claim of this application.
Embodiment 1
According to the solubility of sodium chloride at room temperature, 29g sodium chloride is dissolved in 100mL deionized water, 20min is to equal for stirring
It is even, it takes 150mL dehydrated alcohol in beaker, is quickly poured into sodium chloride solution, precipitation obtains a micron sodium chloride powder.It can observe
It is largely precipitated from solution to milky sodium chloride crystal, is filtered using micropore ethyl alcohol filter membrane, ethyl alcohol is washed 3-5 times, transfer chlorine
Change sodium powder end in culture dish, 60 DEG C of drying 2h collect powder spare.
0.37g DEXTROSE ANHYDROUS is taken to be dissolved in 150mL dehydrated alcohol, above-mentioned sodium chloride powder is added to uniform in stirring 20min
6g continues to stir 20min, is transferred to 80 DEG C of stirred in water bath heat and does, obtains precursor powder.During heat is dry, sodium chloride
It is always maintained at powder morphology, glucose will be precipitated and be uniformly wrapped on sodium chloride surface.
Precursor powder is placed in rectangular mould and is flattened, is placed in tube furnace, at argon gas (flow 200mL/min)
Under hydrogen (flow 50mL/min) mixed atmosphere, 10 DEG C/min is warming up to 750 DEG C, keeps the temperature 120min, after be cooled to room temperature,
Obtain carbonized product.
Carbonized product is placed in a beaker, water logging 60min (can not be stirred strongly during water logging, be prevented from causing product
Destroy), it pulls out, is placed in draining on filter paper, continue water logging 10min, draining, be repeated 5 times, be placed in 60 DEG C of drying 12h, obtain three-dimensional
Carbon networking products.
Embodiment 2
29g sodium chloride is dissolved in 100mL deionized water, 20min is to uniform for stirring, and take 150mL dehydrated alcohol in beaker,
It is quickly poured into sodium chloride solution, precipitation obtains a micron sodium chloride powder.It can be observed that milky sodium chloride crystal is from molten
It is largely precipitated in liquid, is filtered using micropore ethyl alcohol filter membrane, ethyl alcohol is washed 3-5 times, shifts sodium chloride powder in culture dish, 60 DEG C of bakings
Dry 2h, powder is collected spare.
Take 0.55g DEXTROSE ANHYDROUS, 0.4gCu (NO3)2It is dissolved in 150mL dehydrated alcohol, stirring 20min is to uniform, in addition
Sodium chloride powder 6g is stated, continues to stir 20min, 80 DEG C of stirred in water bath heat is transferred to and does, obtain the precursor powder of Copper-cladding Aluminum Bar.
During heat is dry, sodium chloride is always maintained at powder morphology, glucose and Cu (NO3)2It will be precipitated and be uniformly wrapped on sodium chloride table
Face.
Precursor powder is placed in rectangular mould and is flattened, is placed in tube furnace, at argon gas (flow 200mL/min)
Under hydrogen (flow 50mL/min) mixed atmosphere, 10 DEG C/min is warming up to 750 DEG C, keeps the temperature 120min, after be cooled to room temperature,
Obtain carbonized product.
Carbonized product is placed in a beaker, water logging 60min (can not be stirred strongly during water logging, be prevented from causing product
Destroy), it pulls out, is placed in draining on filter paper, continue water logging 10min, draining, be repeated 5 times, be placed in 60 DEG C of drying 12h, loaded
The three-dimensional carbon networking products of copper nano particles.
Embodiment 3
29g sodium chloride is dissolved in 100mL deionized water, 20min is to uniform for stirring, and take 150mL dehydrated alcohol in beaker,
It is quickly poured into sodium chloride solution, precipitation obtains a micron sodium chloride powder.It can be observed that milky sodium chloride crystal is from molten
It is largely precipitated in liquid, is filtered using micropore ethyl alcohol filter membrane, ethyl alcohol is washed 3-5 times, shifts sodium chloride powder in culture dish, 60 DEG C of bakings
Dry 2h, powder is collected spare.
Take 0.55g DEXTROSE ANHYDROUS, 0.4gNi (NO3)2It is dissolved in 150mL dehydrated alcohol, stirring 20min is to uniform, in addition
Sodium chloride powder 6g is stated, continues to stir 20min, 80 DEG C of stirred in water bath heat is transferred to and does, obtain the precursor powder of nickel doping.
During heat is dry, sodium chloride is always maintained at powder morphology, glucose and Ni (NO3)2It will be precipitated and be uniformly wrapped on sodium chloride table
Face.
Precursor powder is placed in rectangular mould and is flattened, is placed in tube furnace, at argon gas (flow 200mL/min)
Under hydrogen (flow 50mL/min) mixed atmosphere, 10 DEG C/min is warming up to 750 DEG C, keeps the temperature 120min, after be cooled to room temperature,
Obtain carbonized product.
Carbonized product is placed in a beaker, water logging 60min (can not be stirred strongly during water logging, be prevented from causing product
Destroy), it pulls out, is placed in draining on filter paper, continue water logging 10min, draining, be repeated 5 times, be placed in 60 DEG C of drying 12h, loaded
The three-dimensional carbon networking products of nano nickel particles.
Claims (4)
1. a kind of preparation method of uniform micron pore size three-dimensional carbon network, including the following steps:
1) salt template is prepared
Sodium chloride solution is prepared, dehydrated alcohol is added, sodium chloride is precipitated, by filtering and drying the consistent chlorination of obtained partial size
Sodium crystal powder is collected spare.
2) presoma is prepared
Glucose is dissolved in dehydrated alcohol, glucose and proportion of ethanol are no more than 1g/100mL, step 1) are added, chlorination is made
Sodium crystal powder, water-bath heat is dry, obtains the sodium chloride presoma of surface cladding glucose.
3) three-dimensional carbon network is prepared
Precursor powder made from step 2) is calcined under inert gas and hydrogen mixed gas atmosphere, carbonized product is obtained, by carbon
Changing product water-soaked, draining for several times, is dried later to get micron pore size three-dimensional carbon network material is arrived again later.
2. preparation method according to claim 1, which is characterized in that in step 2), in dehydrated alcohol, while tool is added
There is deliquescent metal nitrate.
3. preparation method according to claim 1, which is characterized in that the metal nitrate is copper nitrate, nickel nitrate
Or zinc nitrate.
4. preparation method according to claim 1, which is characterized in that precursor powder made from step 2) is placed in tubular type
In furnace under argon gas and hydrogen mixed gas atmosphere, 700-800 DEG C is warming up to 10 DEG C/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113380991A (en) * | 2020-03-10 | 2021-09-10 | 广州汽车集团股份有限公司 | Silicon-carbon composite and preparation method thereof, negative electrode material, negative electrode plate, lithium ion battery and application thereof |
| CN113651993A (en) * | 2021-08-25 | 2021-11-16 | 江南大学 | Phenolic resin nanosheet with parallel columnar mesopores and preparation method thereof |
| CN115477548A (en) * | 2022-09-01 | 2022-12-16 | 天津大学 | Preparation method of self-supporting three-dimensional porous carbon foam |
| CN116425138A (en) * | 2022-11-23 | 2023-07-14 | 中国石油大学(北京) | Heavy oil derived carbon-based electromagnetic wave absorbing material and preparation method thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6680013B1 (en) * | 1999-04-15 | 2004-01-20 | Regents Of The University Of Minnesota | Synthesis of macroporous structures |
| US20130299417A1 (en) * | 2011-01-17 | 2013-11-14 | Eth Zurich | Porous polymer membranes |
| CN104308172A (en) * | 2014-08-11 | 2015-01-28 | 常州大学 | Method for preparing hollow cubic micro-nano metal |
| CN105006374A (en) * | 2015-08-20 | 2015-10-28 | 东南大学 | Preparation of porous nitrogen carbon composite by using salt template method and application of porous nitrogen carbon composite in super capacitor |
| CN105525124A (en) * | 2016-02-02 | 2016-04-27 | 天津大学 | Preparation method for in-situ synthesis of three-dimensional graphene-reinforced copper-based composite material |
| CN106311219A (en) * | 2016-09-08 | 2017-01-11 | 江苏大学 | Preparation method and application of carbon doped silicon dioxide composite material |
| CN106669756A (en) * | 2016-06-29 | 2017-05-17 | 南京理工大学 | Method for preparing nano layered g-C3N4/Ag@AgCl composite photocatalytic material |
| CN106876702A (en) * | 2017-02-08 | 2017-06-20 | 大连理工大学 | A kind of sodium-ion battery negative pole coal tar pitch resin base amorphous carbon coats the preparation method and application of few layer molybdenum disulfide nano box |
| CN108172848A (en) * | 2018-01-31 | 2018-06-15 | 成都新柯力化工科技有限公司 | The catalyst layer and preparation method of a kind of fuel cell N doping copper/nickel alloy |
-
2019
- 2019-05-31 CN CN201910467743.2A patent/CN110127654A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6680013B1 (en) * | 1999-04-15 | 2004-01-20 | Regents Of The University Of Minnesota | Synthesis of macroporous structures |
| US20130299417A1 (en) * | 2011-01-17 | 2013-11-14 | Eth Zurich | Porous polymer membranes |
| CN104308172A (en) * | 2014-08-11 | 2015-01-28 | 常州大学 | Method for preparing hollow cubic micro-nano metal |
| CN105006374A (en) * | 2015-08-20 | 2015-10-28 | 东南大学 | Preparation of porous nitrogen carbon composite by using salt template method and application of porous nitrogen carbon composite in super capacitor |
| CN105525124A (en) * | 2016-02-02 | 2016-04-27 | 天津大学 | Preparation method for in-situ synthesis of three-dimensional graphene-reinforced copper-based composite material |
| CN106669756A (en) * | 2016-06-29 | 2017-05-17 | 南京理工大学 | Method for preparing nano layered g-C3N4/Ag@AgCl composite photocatalytic material |
| CN106311219A (en) * | 2016-09-08 | 2017-01-11 | 江苏大学 | Preparation method and application of carbon doped silicon dioxide composite material |
| CN106876702A (en) * | 2017-02-08 | 2017-06-20 | 大连理工大学 | A kind of sodium-ion battery negative pole coal tar pitch resin base amorphous carbon coats the preparation method and application of few layer molybdenum disulfide nano box |
| CN108172848A (en) * | 2018-01-31 | 2018-06-15 | 成都新柯力化工科技有限公司 | The catalyst layer and preparation method of a kind of fuel cell N doping copper/nickel alloy |
Non-Patent Citations (3)
| Title |
|---|
| TANG，YUXIN ET AL: ""Efficient Ag@AgCl Cubic Cage Photocatalysts Profit from Ultrafast Plasmon-Induced Electron Transfer Processes"", 《ADVANCED FUNCTIONAL MATERIALS》 * |
| 石亚茹: ""生物质多孔碳材料制备及电性能研究"", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
| 赵乃勤 等: ""多维度碳纳米相增强铝基复合材料研究进展"", 《金属学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113380991A (en) * | 2020-03-10 | 2021-09-10 | 广州汽车集团股份有限公司 | Silicon-carbon composite and preparation method thereof, negative electrode material, negative electrode plate, lithium ion battery and application thereof |
| CN113651993A (en) * | 2021-08-25 | 2021-11-16 | 江南大学 | Phenolic resin nanosheet with parallel columnar mesopores and preparation method thereof |
| CN115477548A (en) * | 2022-09-01 | 2022-12-16 | 天津大学 | Preparation method of self-supporting three-dimensional porous carbon foam |
| CN115477548B (en) * | 2022-09-01 | 2023-11-17 | 天津大学 | Preparation method of self-supporting three-dimensional porous carbon foam |
| CN116425138A (en) * | 2022-11-23 | 2023-07-14 | 中国石油大学(北京) | Heavy oil derived carbon-based electromagnetic wave absorbing material and preparation method thereof |
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