CN108467033B - A kind of preparation method of bionic laminar nano composite film - Google Patents
A kind of preparation method of bionic laminar nano composite film Download PDFInfo
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- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
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- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/117—Esters of phosphoric acids with cycloaliphatic alcohols
Abstract
The invention belongs to high-strength light composite nano materials preparation technical fields, are related to a kind of preparation method of bionic laminar nano composite film.A kind of high intensity, high tenacity bionic laminar nano composite film has been prepared with simple mechanical package method by " brick-mud " microstructure of imitation shellfish material in this method.Specific method is that (1) prepares certain density graphene oxide and plant acid solution respectively at room temperature;(2) above-mentioned solution is mixed according to certain mass percent, is sufficiently stirred, form transparent uniform mixed solution;(3) at room temperature, mixed solution is subjected to mechanical package, removed, finally obtain high-intensitive, high tenacity bionic laminar nano composite film.The advantages that present invention has intensity high, and light-weight, convenient transportation, it is simple and direct, firm to construct, and not creep, designability is good, insulation, heat-resisting cold-resistant, anticorrosion.
Description
Technical field
The invention belongs to high-strength light technical field of nanometer material preparation, it is related to a kind of preparing that high-intensitive, high tenacity is compound
The preparation method of thin-film material.
Background technique
With the development of modern science and technology, made rapid progress especially in fields such as Aeronautics and Astronautics, national defence, for material
The requirement of material is higher and higher.The quality that material how is reduced while improving the strength of materials, is save the cost, improves production effect
The key point of rate, while being also the key issues of present material area research.
In recent years, biomaterial, such as cellulose tissue (timber, bamboo), collagen tissue (tendon, ligament), mineralising group
It knits (bone, shell) and causes the great interest of scientist.Their light weights, outstanding mechanical performance are not only as, it is heavier
What is wanted is that researcher passes through the heterogeneous microstructure for imitating the multilevel of its biomaterial, and it is compound to can be realized preparation high-performance
Material substitutes existing traditional performance materials.For example, multilevel, natural seashell (mother-of-pearl) material of micro-/ nano heterojunction structure
Material is passed through orderly by two-dimentional aragonite (calcium carbonate) micron chip and soft biological organic molecule layer (polysaccharide and albumen) of hard
It is piled into " brick-cement " layer structure, has very outstanding mechanical performance.The two dimension of many material science Household hards is thin
Piece and soft polymer molecule imitate shell stratiform " brick-cement " structure, (such as based on the strong molecular force of the heterogeneous interface
Hydrogen bond, ionic bond and covalent bond), construct high-strength light laminar composite.Although these materials can show certain excellent
Elegant mechanical property, but it is difficult to have both high-intensitive and high tenacity, in addition, its preparation process is cumbersome, expensive and highly energy-consuming, and system
Standby scantling is smaller, is highly detrimental to Lightweight high-strength composite material production application.
Carbon Materials include that carbon fiber, graphite, graphene and graphene oxide in light-weight high-strength material field have important answer
With by taking graphene oxide as an example, with outstanding mechanical property.How by the stratified material of the type, pass through simple interface
Strengthening design, preparation have both high-intensitive and high tenacity, large-sized composite material, and it is huge to be that investigation of materials field still suffers from
Challenge.
Thus the preparation method for developing a kind of bionic laminar nano composite film need be needed at present come on overcoming
State defect.
Summary of the invention
Had outstanding mechanical property and phytate molecule in biomaterial by " brick-cement " micro-structure of shell mother of pearl
In strong chelation common inspiration, in view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to utilize simple mechanical group
Dress method uses the graphene oxide conveniently obtained and biological organic molecule for raw material, based on the biomolecule in graphite oxide
Alkene strong interface bond and effect provide high intensity a kind of easy to operate, environmentally protective, high tenacity bionic laminar composite material
Preparation method.Composite film material prepared by this method has light weight, intensity big, high tenacity, scantling, and thickness is micro-
The features such as structure-controllable.Specific preparation method the following steps are included:
Step 1: based on modified Hummer method, preparing graphene oxide, used as reserve materials;
Step 2: weighing the graphene oxide reserve materials powder of 3-5g in step 1, be configured to the oxygen of 1-3mg/ml concentration
Graphite alkene colloidal sol dispersion liquid, ultrasonic disperse are used as stock solution;
Step 3: the phytic acid weak solution of configuration 0.3-1.0wt% concentration is used as stock solution;
Step 4: measuring the stock solution of a certain amount of step 2 and step 3 respectively, being configured to volume ratio is the mixed of 95:0.2-1.0
It closes solution 30-50ml and forms stable graphene oxide/phytic acid first to its sonic oscillation 30-60min, then magnetic agitation 5-7h
Mixing dispersion solution;
Step 5: the graphene oxide for the 30-50ml that step 4 is obtained/phytic acid mixing dispersion solution utilizes miillpore filter
Mechanical-assisted assemble method, is assembled.Different-thickness (5-20 μm) based on thin-film material, usually needing built-up time is 6-
48h etc.;It is aperture is 0.22 μm that the described miillpore filter mechanical-assisted assembling, which is by multilayer filter membrane, the mixing of 3-8cm size
Cellulose filter membrane carries out overlapping assembling.
Step 6: finishing (solvent completely removes) to the thin-film material assembling in step 5, removed to get to accordingly
High-intensitive, high tenacity bionic laminar composite film material.
Further, the concrete operations that graphene oxide is prepared in the step 1 are as follows: the concentrated sulfuric acid being taken to be added to reaction
In device, reactor is placed in water-bath and controls temperature less than 2 DEG C;Natural flake graphite is chosen, with the matter of natural flake graphite
Natural flake graphite is added in the reactor for filling the concentrated sulfuric acid by the proportionate relationship that amount and the volume ratio of the concentrated sulfuric acid are 1:33, is stirred
25-35min is mixed, water bath temperature is increased to 10-15 DEG C, with KMnO4With NaNO3The proportionate relationship that mass ratio is 6:1 is added
KMnO4And NaNO325-35min is stirred, and water bath temperature is increased to 30-40 DEG C, continues to stir 1-3h, be mixed
Liquid;Water is added for the proportionate relationship of 1:46 with the quality of natural flake graphite and the volume of water in mixed liquor, by water-bath
Temperature is increased to 90-100 DEG C, stirs 25-35min;Reactor is removed into water-bath, water is added, with H2O2With the volume ratio of HCl
H is added for the proportionate relationship of 15:22O2And HCl, washing, until supernatant liquor is in neutrality, drying obtains oxidation stone for centrifugation
Ink.
In the present invention, available graphene oxide is mainly synthesized by modified Hummer method, but is not only limited to this.
Preferably, solution system used in step (1)-(3) is deionized water system.
Preferably, graphene oxide powder used with a thickness of 0.5-1nm.
Preferably, it is 0.22 μm that filter membrane described in step (5), which is aperture, the cellulose mixture filter membrane of 3-8cm size.
The present invention, prepared bionic laminar nano composite film have the size of 3-8cm, 5-30 μm of thickness.
The present invention, prepared bionic laminar nano composite film have the wrong orderly laminar microstructure of height heap,
It is between layers 1nm hereinafter, macroscopical color is sepia.
The present invention, the tensile strength position 140-300Mpa of prepared bionic laminar nano composite film, Young mould
Amount is 10-14Gpa, work to break 5-8MJ/m-3。
In the present invention, if be not particularly described, used solution is all prepared under normal conditions, such as
Substance dissolution is prepared in aqueous solution at room temperature.
In the present invention, if be not particularly described, used device, instrument, material, technique, method, step, system
Standby condition etc. is all that this field routinely uses or those of ordinary skill in the art can according to the technology that this field routinely uses
With what is be easy to get.
In the present invention, available crystalline flake graphite is 200 mesh, but is not only limited to this.
Relative to the preparation of existing high-strength light composite film material, the present invention is had a characteristic that
(1) raw material used in preparation process of the present invention is simple and easy to get, and cost is relatively low, and there are no pollution to the environment, technique
Simply, easy to operate;
(2) the features such as bionic laminar composite film material prepared by the present invention, structure is uniform, light weight, intensity is big, and
Its size and thickness, the wrong orderly layered microstructure of heap also can control;
(3) gained composite film material is easily prepared due to its outstanding mechanical performance, and potential electronics and thermal conductivity can seep
The features such as permeability, biocompatibility, filters in the biological and chemical of biological gas sensitive device, bio-pharmaceuticals, separating film, nano-pore
Device, interface thermal control etc. have good application prospect.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is mechanical package of the present invention;
Fig. 2 is the digital photograph of the high intensity of preparation of the embodiment of the present invention, high tenacity bionic laminar nano composite film
Piece (a) and its laminar microstructure scanning electron microscope microscope photo (b, c, d);
Fig. 3 is that the present invention implements prepared high intensity, the X-ray of high tenacity bionic laminar nano composite film
Diffraction maximum shows the wrong orderly layer structure of its heap.
Fig. 4 is high intensity, high tenacity bionic laminar nano composite film mechanical property prepared by present example 1,2,3
It can comparison.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
This high-intensitive, high tenacity bionic laminar composite film material preparation is specifically described with implementation with reference to the accompanying drawing
Method.It is to be understood that these embodiments are only intended to illustrate the present invention, and the protection not limiting the invention in any way
Range.
Embodiment 1
A kind of preparation method of bionic laminar nano composite film (maximum proportion)
1, step 1: the concentrated sulfuric acid is taken to be added in reactor based on modified Hummer method, reactor is placed in water-bath
Control temperature is less than 2 DEG C in pot;3 parts of natural flake graphite are chosen, with the volume ratio of the quality of natural flake graphite and the concentrated sulfuric acid
Natural flake graphite is added in the reactor for filling the concentrated sulfuric acid for the proportionate relationship of 1:33,25-35min is stirred, by water-bath
Pot temperature is increased to 10-15 DEG C, with KMnO4With NaNO3KMnO is added in the proportionate relationship that mass ratio is 6:14And NaNO3Stirring
25-35min, and water bath temperature is increased to 30-40 DEG C, continue to stir 1-3h, obtains mixed liquor;With natural in mixed liquor
Water is added in the proportionate relationship that the quality of crystalline flake graphite and the volume of water are 1:46, and the temperature of water-bath is increased to 90-100 DEG C,
Stir 25-35min;Reactor is removed into water-bath, water is added, with H2O2The proportionate relationship that volume ratio with HCl is 15:2 adds again
Enter H2O2And Hcl, washing, until supernatant liquor is in neutrality, drying obtains graphene oxide reserve materials powder 2.5 for centrifugation
Part.
Step 2: weighing the graphene oxide reserve materials powder of 200mg in step 1, be configured to the oxygen that concentration is 1mg/ml
Graphite alkene colloidal sol dispersion liquid 100ml, ultrasonic disperse 60min are used as stock solution;
Step 3: measuring a certain amount of plant acid solution and being configured to 50ml concentration is that 0.5wt% weak solution makes as stock solution
With;
Step 4: measuring the graphene oxide solution (step 2) of 29.987ml and the phytic acid (step 3) of 12.563 μ l respectively
Mass percent (95:0.2) mixing, first to its sonic oscillation 30min, then magnetic agitation 5h, formed the phytic acid of stable 30ml/
Graphene oxide mixing dispersion solution (such as Fig. 1);
Step 5: the 30ml graphene oxide that step 4 is obtained/phytic acid mixing dispersion solution carries out miillpore filter machinery group
Dress, built-up time is about 42h;
Step 6: in step 5 thin-film material assembling finish (solvent completely removes), remove to get arrive with a thickness of
12 μm, the composite film material (Fig. 2 a) having a size of 4cm.Scanning electron microscope displaing micro picture and X-ray diffraction peak show that Qi Duicuo has
The layer structure (Fig. 2 b and Fig. 3) of sequence, and stronger mechanical property is showed, tensile strength is 143.5 ± 10.3Mpa, fracture
Function is 3.5 ± 0.6MJ/m-3, maximum Young's modulus is 5.7 ± 0.8Gpa (Fig. 4).
Embodiment 2
A kind of preparation method (optimization) of bionic laminar nano composite film
Step 1: based on modified Hummer method, weighs the concentrated sulfuric acid and be added in reactor, reactor is placed in water-bath
Control temperature is less than 2 DEG C in pot;3 parts of natural flake graphite are chosen, with the volume ratio of the quality of natural flake graphite and the concentrated sulfuric acid
Natural flake graphite is added in the reactor for filling the concentrated sulfuric acid for the proportionate relationship of 1:33,30min is stirred, by water-bath pot temperature
Degree is increased to 15 DEG C, with KMnO4With NaNO3KMnO is added in the proportionate relationship that mass ratio is 6:14And NaNO330min is stirred, and
Water bath temperature is increased to 35 DEG C, continues to stir 2h, obtains mixed liquor;In mixed liquor with the quality of natural flake graphite with
Water is added in the proportionate relationship that the volume of water is 1:46, and the temperature of water-bath is increased to 95 DEG C, stirs 30min;Reactor is moved
Water is added, with H in water-bath out2O2The proportionate relationship that volume ratio with HCl is 15:2 adds H2O2And Hcl, washing, centrifugation are straight
It is in neutrality to supernatant liquor, it is dry, that is, obtain 2.5 parts of graphene oxide reserve materials powder;
Step 2: weighing the graphene oxide reserve materials powder of 200mg in step 1, be configured to the oxygen that concentration is 1mg/ml
Graphite alkene colloidal sol dispersion liquid 100ml, ultrasonic disperse 45min are used as stock solution;
Step 3: measuring a certain amount of plant acid solution and being configured to 50ml concentration is that 0.5wt% weak solution makes as stock solution
With;
Step 4: measuring the graphene oxide solution (step 2) of 29.975ml and the phytic acid (step 3) matter of 25.1 μ l respectively
Percentage (95:0.4) mixing is measured, first to its sonic oscillation 45min, then magnetic agitation 6h, forms phytic acid/oxygen of stable 30ml
Graphite alkene mixing dispersion solution (Fig. 1);
Step 5: the 30ml graphene oxide that step 4 is obtained/phytic acid mixing dispersion solution carries out miillpore filter machinery group
Dress, built-up time is about 48h;
Step 6: in step 5 thin-film material assembling finish (solvent completely removes), remove to get arrive with a thickness of
12.5 μm, the composite film material (Fig. 2 a) having a size of 4cm.Scanning electron microscope displaing micro picture and X-ray diffraction peak show Qi Duicuo
Orderly layer structure (Fig. 2 c and Fig. 3), and maximum mechanical property is shown, tensile strength is 266.2 ± 26.4Mpa,
Work to break is 5.9 ± 0.8MJ/m-3, maximum Young's modulus is 11.5 ± 0.4Gpa.
Embodiment 3
A kind of preparation method of bionic laminar nano composite film (minimum proportion)
Step 1: based on modified Hummer method, the crystalline flake graphite for weighing 3g prepares the graphene oxide powder of 2.5g
End is used as reserve materials;
Step 2: weighing the graphene oxide reserve materials powder of 200mg in step 1, be configured to the oxygen that concentration is 1mg/ml
Graphite alkene colloidal sol dispersion liquid 100ml, ultrasonic disperse 45min are used as stock solution;
Step 3: measuring a certain amount of plant acid solution and being configured to 50ml concentration is that 0.5wt% weak solution makes as stock solution
With;
Step 4: measuring the graphene oxide solution (step 2) of 29.937ml and the phytic acid (step 3) matter of 62.7 μ l respectively
Percentage (95:1.0) mixing is measured, first to its sonic oscillation 60min, then magnetic agitation 7h, forms phytic acid/oxygen of stable 30ml
Graphite alkene mixing dispersion solution;
Step 5: the 30ml graphene oxide that step 4 is obtained/phytic acid mixing dispersion solution carries out miillpore filter machinery group
Dress, built-up time is about 54h;
Step 6: in step 5 thin-film material assembling finish (solvent completely removes), remove to get arrive with a thickness of
13 μm, the bionic laminar composite film material having a size of 4cm,
Step 6: in step 5 thin-film material assembling finish (solvent completely removes), remove to get arrive with a thickness of
13 μm, the composite film material (Fig. 2 a) having a size of 4cm.Scanning electron microscope displaing micro picture and X-ray diffraction peak show that Qi Duicuo has
The layer structure (Fig. 2 d and Fig. 3) of sequence, and outstanding mechanical property is shown, tensile strength is 162.1 ± 7.3Mpa, fracture
Function is 4.5 ± 0.4MJ/m-3, Young's modulus is 4.8 ± 1.6Gpa.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For device disclosed in embodiment
For, since it is corresponded to the methods disclosed in the examples, so being described relatively simple, related place is said referring to method part
It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (8)
1. a kind of preparation method of bionic laminar nano composite film, which comprises the following steps:
Step (1): based on modified Hummer method, graphene oxide powder is prepared;
Step (2): the graphene oxide powder in step (1) is weighed, adds water to carry out in Xiang Suoshu graphene oxide powder
Ultrasonic disperse is configured to the graphene oxide colloidal sol dispersion liquid of 1-3mg/ml concentration;
Step (3): the phytic acid weak solution of configuration 0.3-1.0wt% concentration;
Step (4): graphene oxide colloidal sol dispersion liquid and phytic acid weak solution, graphene oxide colloidal sol dispersion liquid are measured respectively
It is 95:0.2~95:0.1 with phytic acid weak solution volume ratio, successively carries out sonic oscillation, magnetic agitation forms stable oxidation stone
Black alkene/phytic acid mixing dispersion solution;
Step (5): the graphene oxide that step (4) are obtained/phytic acid mixes dispersion solution and carries out miillpore filter mechanical package;
Step (6): finishing to the miillpore filter mechanical package in step (5), until graphene oxide/phytic acid mixing dispersion solution
In solution completely remove, by the removing of the film of formation to get to it is corresponding it is high-intensitive, the bionic laminar of high tenacity is nano combined
Thin-film material.
2. a kind of preparation method of bionic laminar nano composite film according to claim 1, which is characterized in that institute
State prepared in step (1) graphene oxide concrete operations it is as follows: take the concentrated sulfuric acid to be added in reactor, reactor be placed in water
In bath;Natural flake graphite is chosen, it is proportional with the volume of the quality of natural flake graphite and the concentrated sulfuric acid, by natural squama
Piece graphite is added in the reactor for filling the concentrated sulfuric acid, is stirred for the first time, with KMnO4With NaNO3The proportionate relationship of certain mass ratio
KMnO is added4And NaNO3Second of stirring, and water bath temperature is increased to 30-40 DEG C, third time stirs, and is mixed
Liquid;Water is added with the proportionate relationship of certain volume ratio of natural flake graphite and water in mixed liquor, by the temperature of water-bath
It is increased to 90-100 DEG C, the 4th stirring;Reactor is removed into water-bath, water is added, with H2O2With certain volume ratio of HC l
Proportionate relationship add H2O2With HC l, washing, until supernatant liquor is in neutrality, dry is to obtain graphite oxide powder for centrifugation.
3. a kind of preparation method of bionic laminar nano composite film according to claim 1, which is characterized in that institute
Graphene oxide with a thickness of 0.5-1nm.
4. a kind of preparation method of bionic laminar nano composite film according to claim 1, which is characterized in that step
Suddenly in (5), it is 6-48h that miillpore filter mechanical-assisted, which assembles built-up time,.
5. a kind of preparation method of bionic laminar nano composite film according to claim 1, which is characterized in that step
Suddenly it is 0.22 μm that filter membrane described in (5), which is aperture, the cellulose mixture filter membrane of 3-8cm size.
6. a kind of preparation method of bionic laminar nano composite film according to claim 1, which is characterized in that step
Suddenly the stock solution for measuring a certain amount of step (2) and step (3) in (4) respectively is configured to the mixed solution that volume ratio is 95:0.4,
First to its sonic oscillation 60min, then magnetic agitation 7h, stable phytic acid/graphene oxide mixing dispersion solution is formed.
7. a kind of preparation method of bionic laminar nano composite film according to claim 2, which is characterized in that institute
Stating and preparing time for stirring for the first time described in the concrete operations of graphene oxide in step (1) is 25-35min, described second
The time of secondary stirring is 25-35mi n, and the time of the third time stirring is 1-3h, and the time of the 4th stirring is 25-
35min。
8. a kind of preparation method of bionic laminar nano composite film according to claim 2, which is characterized in that institute
It states and prepares the quality of natural flake graphite described in the concrete operations of graphene oxide in step (1) and the volume ratio of the concentrated sulfuric acid is
1:33;The KMnO4With NaNO3Certain mass ratio is 6:1;The quality of the natural flake graphite and the volume of water are 1:46;
The H2O2It is 15:2 with HC l certain volume ratio.
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