CN109162141A - A kind of conductive nano paper and preparation method thereof and capacitor - Google Patents
A kind of conductive nano paper and preparation method thereof and capacitor Download PDFInfo
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- CN109162141A CN109162141A CN201811001496.9A CN201811001496A CN109162141A CN 109162141 A CN109162141 A CN 109162141A CN 201811001496 A CN201811001496 A CN 201811001496A CN 109162141 A CN109162141 A CN 109162141A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
-
- 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
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/07—Nitrogen-containing compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/005—Electrodes
Abstract
The invention discloses a kind of conductive nano paper and preparation method thereof and capacitor, the preparation method of the conductive nano paper includes: to obtain nano conductive film through vacuum filtration after being uniformly mixed nano-cellulose with conductive material；The nano conductive film is placed in the mixed aqueous solution of choline chloride and urea and is impregnated, then takes out drying.Conductive nano paper of the invention is by first obtaining nano conductive film through being filtered by vacuum after being uniformly mixed nano-cellulose with conductive material, then nano conductive film is placed in again in the mixed aqueous solution of choline chloride and urea after impregnating and is dried to obtain, not only transparency with higher, higher tensile strength and lower Young's modulus, and there is preferable electric conductivity, and it is also with good stability as the capacitor of key component building.
Description
Technical field
The present invention relates to flexible conducting material field, in particular to a kind of conductive nano paper and preparation method thereof and
Capacitor.
Background technique
In face of the growing energy consumption of modern society and very urgent environmental protection, researchers are constantly visited
Rope is renewable, the sustainable energy, such as solar battery, wind-force and thermal power generation clean energy resource, flexible electronic product and device
Important component of the part as information-intensive society should also walk environmentally protective, sustainable road.But in recent years, with various
The waste (such as PET) that electronic device is generated in being widely used for flexible products such as packaging, wearable devices to environment and
The threat of non-renewable energy resources is more and more very important.And lightweight capacitor is the significant components in flexible electronic device, because
This, it is very necessary for developing a kind of capacitor that raw material sources are abundant, renewable, biodegradable.
Paper is just playing the substitute effect of electronic product due to high yield and low cost and as renewable resource, in recent years
To show that the flexible capacitor with preferable electric property can be made using paper there are many report.But the one of traditional paper
A little disadvantages, such as micron-sized surface roughness, almost opaque, mechanical property is poor, limits paper base flexible conducting material
Application in terms of capacitor.
Summary of the invention
In view of this, a kind of conductive nano paper provided by the invention and preparation method thereof and capacitor, preferably overcome
The above-mentioned problems of the prior art and defect, the conductive nano paper by by nano-cellulose and conductive material after mixing
It is filtered by vacuum and first obtains nano conductive film, then nano conductive film is placed in the mixed aqueous solution of choline chloride and urea again
It is dried to obtain, not only transparency with higher, higher tensile strength and lower Young's modulus, and has preferable after immersion
Electric conductivity, and its as key component building capacitor it is also with good stability.In addition, conductive nano of the invention
The preparation method of paper is simple, convenient, easily industrializes, and can preferably be applied in capacitor.In addition, nanometer prepared by the present invention
Conductive paper also can be applied to the fields such as transparent electrode and electroluminescent material.
Specifically, the invention proposes embodiments in detail below:
A kind of preparation method of conductive nano paper, comprising:
Nano conductive film is obtained through vacuum filtration after nano-cellulose is uniformly mixed with conductive material；
The nano conductive film is placed in the mixed aqueous solution of choline chloride and urea and is impregnated, then takes out drying.
Further, the nano-cellulose by by hardwood pulp, eucalyptus pulp or softwood pulp through TEMPO/NaBr/
NaClO system carries out oxidation and homogenization obtains.
Further, the conductive material is nano-silver thread, poly- 3,4-ethylene dioxythiophene: poly styrene sulfonate, stone
One of nanometer powder of black alkene, carbon nanotube and conductive metal is a variety of.
Further, the dosage of the conductive material accounts for 0.5~2.5wt% of the quality of the nano-cellulose.
Further, the process that nano-cellulose is mixed with conductive material includes: by nano-cellulose and conduction
15~30min of ultrasonic vibration after material mixing.
Further, in the mixed aqueous solution of the choline chloride and urea: the mass ratio of choline chloride and urea is 1:
The gross mass of (1~3), choline chloride and urea and the mass ratio of water are (0.01~0.05): 1.
Further, the time of the immersion be 12~for 24 hours.
Further, the time of the drying is 2~3h；The temperature of the drying is 80~100 DEG C.
The present invention also provides a kind of conductive nano paper, are prepared by the preparation method of above-mentioned conductive nano paper.
The present invention also provides a kind of capacitors, including above-mentioned conductive nano paper.
Compared with prior art, the beneficial effect of a kind of conductive nano paper of the invention and preparation method thereof and capacitor
It is:
Conductive nano paper of the invention is first obtained by being filtered by vacuum after being uniformly mixed nano-cellulose with conductive material
To nano conductive film, then nano conductive film is placed in again in the mixed aqueous solution of choline chloride and urea dry after impregnating
It arrives, not only transparency with higher, higher tensile strength and lower Young's modulus, and there is preferable electric conductivity, and
It is also with good stability as the capacitor of key component building.In addition, the preparation side of conductive nano paper of the invention
Method is simple, convenient, easily industrializes, and can preferably be applied in capacitor.In addition, conductive nano paper prepared by the present invention can also
To be applied to the fields such as transparent electrode and electroluminescent material.
In conclusion the structure that the present invention is special, has the advantages that above-mentioned many and practical value, and in similar product
In there are no similar method and publish or use and really belong to innovation, produce handy and practical effect, more existing skill
Art has effects that the multinomial of enhancement, thus more suitable for practical, and there is extensive industrial value.
To enable the above objects, features and advantages of the present invention to be clearer and more comprehensible, preferred embodiment is cited below particularly, and cooperate
Appended attached drawing, is described in detail below.
Detailed description of the invention
Fig. 1 is the optics picture for stretching conductive nano paper of Examples 1 to 3 preparation；
Fig. 2 is the visible light transmittance curve of the conductive nano paper of Examples 1 to 5 preparation；
Fig. 3 is the scanning electron microscope (SEM) photograph of nano-cellulose prepared by embodiment 1；
Fig. 4 is the scanning electron microscope (SEM) photograph of conductive nano paper prepared by embodiment 1；
Fig. 5 is nano conductive film prepared by the conductive nano paper for preparing of Examples 1 to 5 and comparative example 1, comparative example 1 and pure
Stretching-inflection curves of nano-cellulose paper；
Fig. 6 is the Young's modulus figure of conductive nano paper and pure nano-cellulose paper prepared by Examples 1 to 5 and comparative example 1；
Fig. 7 is the cyclic voltammetry curve figure of conductive nano paper prepared by embodiment 1；
Fig. 8 is that the capacitor for the capacitor that conductive nano paper prepared by embodiment 1 is key component building retains test curve
Figure.
Specific embodiment
To facilitate the understanding of the present invention, conductive nano paper and preparation method thereof is carried out below with reference to relevant drawings more complete
The description in face.The embodiment of conductive nano paper and preparation method thereof is given in attached drawing.But conductive nano paper and its preparation side
Method can be realized in many different forms, however it is not limited to embodiment described herein.On the contrary, providing these embodiments
Purpose be to keep the disclosure to conductive nano paper and preparation method thereof more thorough and comprehensive.
Hereinafter, various embodiments of the present invention will be described more fully.The present invention can have various embodiments, and
It can adjust and change wherein.It should be understood, however, that: there is no various embodiments of the present invention are limited to spy disclosed herein
Determine the intention of embodiment, but should invention is construed as cover in the spirit and scope for falling into various embodiments of the present invention
All adjustment, equivalent and/or optinal plan.
Hereinafter, disclosed in the term " includes " that can be used in various embodiments of the present invention or " may include " instruction
Function, operation or the presence of element, and do not limit the increase of one or more functions, operation or element.In addition, such as existing
Used in various embodiments of the present invention, term " includes ", " having " and its cognate are meant only to indicate special characteristic, number
Word, step, operation, the combination of element, component or aforementioned item, and be understood not to exclude first one or more other
Feature, number, step, operation, element, component or aforementioned item combined presence or increase one or more features, number,
Step, operation, element, component or aforementioned item combination a possibility that.
In various embodiments of the present invention, statement " A or/and B " includes any combination or the institute of the text listed file names with
There is combination, such as, it may include A, it may include B or may include A and B both.
The statement (" first ", " second " etc.) used in various embodiments of the present invention can be modified in various implementations
Various constituent element in example, but respective sets can not be limited into element.For example, the above statement is not intended to limit the suitable of the element
Sequence and/or importance.The above statement is only used for the purpose for differentiating an element and other elements.For example, the first user fills
It sets and indicates different user device with second user device, although the two is all user apparatus.For example, of the invention each not departing from
In the case where the range of kind embodiment, first element is referred to alternatively as second element, and similarly, second element is also referred to as first
Element.
It should also be noted that in the present invention, unless otherwise specific regulation and definition, the arts such as " installation ", " connection ", " fixation "
Language shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection or being integrally connected；It can be machine
Tool connection, is also possible to be electrically connected；It can be and be directly connected to, and can be indirectly connected through an intermediary；It can be two
Connection inside element.For the ordinary skill in the art, above-mentioned term can be understood at this as the case may be
Concrete meaning in invention.
In the present invention, those skilled in the art are it is to be appreciated that indicating position or positional relationship in text
Term be orientation based on the figure or positional relationship, be merely for convenience of description of the present invention and simplification of the description, without
It is that the device of indication or suggestion meaning or element must have a particular orientation, be constructed and operated in a specific orientation, therefore
It is not considered as limiting the invention.
The term used in various embodiments of the present invention is used only for the purpose of describing specific embodiments and not anticipates
In limitation various embodiments of the present invention.Unless otherwise defined, otherwise all terms used herein (including technical term and
Scientific term) there is contain identical with the normally understood meaning of various embodiments of the present invention one skilled in the art
Justice.The term (term such as limited in the dictionary generally used) be to be interpreted as have in the related technical field
The identical meaning of situational meaning and Utopian meaning or meaning too formal will be interpreted as having, unless this
It is clearly defined in the various embodiments of invention.
The present invention provides a kind of preparation methods of conductive nano paper, comprising:
Nano conductive film is obtained through vacuum filtration after nano-cellulose is uniformly mixed with conductive material；
The nano conductive film is placed in the mixed aqueous solution of choline chloride and urea and is impregnated, then takes out drying.
Preferably, the nano-cellulose by by hardwood pulp, eucalyptus pulp or softwood pulp through TEMPO/NaBr/
NaClO system carries out oxidation and homogenization obtains.
It should be noted that TEMPO (2,2,6,6- tetramethyl piperidine -1- oxygen radical) is a kind of water-soluble piperidines nitrogen
Oxygen radical.TEMPO/NaBr/NaClO system is a kind of new selective oxidation system, TEMPO and NaBr as catalysis
Agent, NaClO is as oxidant.TEMPO/NaBr/NaClO system can be in the liquid phase environment that pH is 10~11, by aldehyde radical and carboxylic
Base effectively refers on cellulose surface, the position the C6 hydroxyl of cellulose surface is oxidized to carboxyl, through TEMPO/NaBr/NaClO
The cellulose of system oxidation, because its surface has carboxyl negative electrical charge, since intermolecular electrostatic repulsive interaction weakens intermolecular hydrogen bonding
Active force can be such that cellulose reduces and reunite under the action of mechanical shear stress.
By taking eucalyptus pulp prepares nano-cellulose as an example, the preparation method of the nano-cellulose includes:
(1) it samples in Eucalyptus pulpboard different location, with the water content of moisture teller measurement pulpboard, takes suitable exhausted
Dry pulp, is added a certain amount of deionized water, after soaked overnight, 3h is stirred with blender with the revolving speed of 500rpm/min, so that slurry
Expect fully dispersed in water.
(2) deionized water dissolving sodium bromide is used, bath temperature is to dissolve TEMPO at 50 DEG C, is then added scattered in advance
Slurry in, and be added deionized water adjusting, make the concentration 1% of slurry, continue stirring 30min, make aqueous sodium bromide and
TEMPO chemicals and slurry are sufficiently mixed uniformly.The amount of sodium bromide and TEMPO used is the dosage based on oven dry stock to calculate
, the dosage of sodium bromide is 10wt%, and the dosage of TEMPO is 1.6wt%.Sodium hypochlorite is added dropwise dropwise with rubber head dropper again, from
Sodium hypochlorite is added and starts calculating reacting time.Start in half an hour, reaction acutely, can use sodium hydroxide or salt acid for adjusting pH
Value keeps pH value to be in 10~11, and the time that entire reaction carries out is about 3~5h.
(3) slurry of above-mentioned steps (2) after the reaction was completed filter using Buchner funnel, deionized water and slurry bag and be washed
It washs, cleans repeatedly at least three times, until the chemicals in slurry all removes.Slurry after cleaning add it is suitable go from
Sub- water, diluted slurry concentration are 1% spare.Finally, the slurry diluted, which is transferred to nanometer Microfluidizer, carries out homogeneous
Processing, obtains gelatinous nano-cellulose.Nano-cellulose dispersion liquid obtained is placed under conditions of 4 DEG C and is stored for future use.
Certainly, the present invention is not intended to limit the source of nano-cellulose, can also for by by hardwood pulp, eucalyptus pulp or
Softwood pulp is obtained through acid-hydrolysis method or alkali hydrolysis method etc. is prepared.But using TEMPO/NaBr/NaClO system to broad-leaved
The nano-cellulose fiber that wood pulp, eucalyptus pulp or softwood pulp are obtained through being aoxidized, then using homogenization more evenly,
Energy consumption is lower.
Preferably, the conductive material is nano-silver thread (AgNWs), poly- 3,4-ethylene dioxythiophene: polystyrolsulfon acid
Salt (PEDOT:PSS), graphene (Graphene), carbon nanotube (CNT) and conductive metal one of nanometer powder or
It is a variety of.
Preferably, the dosage of the conductive material accounts for 0.5~2.5wt% of the quality of the nano-cellulose such as
0.5wt%, 1wt%, 1.5wt%, 2wt% or 2.5wt% etc..
Preferably, the process that nano-cellulose is mixed with conductive material includes: by nano-cellulose and conduction material
15~30min of ultrasonic vibration such as 15min, 20min, 25min or 30min etc. after material mixing.
Preferably, in the mixed aqueous solution of the choline chloride and urea: the mass ratio of choline chloride and urea is 1:(1
~3) such as 1:1,1:1.5,1:2,1:2.5 or 1:3；The mass ratio of the gross mass and water of choline chloride and urea be (0.01~
0.05): 1 such as 0.01:1,0.02:1,0.03:1,0.04:1 or 0.05:1.
Preferably, the time of the immersion be 12~such as 12h, 15h, 18h, 20h or for 24 hours for 24 hours.
It should be noted that the nano conductive film that is mixed with of nano-cellulose and conductive material by choline chloride/
The conductive nano paper obtained after the immersion treatment of aqueous solution of urea, can show preferable tensile property, and tensile deformation is reachable
17%, it is more than ten times of conductive nano paper and pure nano-cellulose paper that nano-cellulose and conductive material are mixed with.Reason
It is that-NH2 in choline chloride/urea aqueous solution on urea molecule can form intermolecular hydrogen bonding with the-OH on cellulosic molecule,
The intramolecular hydrogen bond between cellulose and cellulose is reduced, paper is made to show soft stretchable " elasticity " behavior.
Preferably, the time of the drying is 2~3h such as 2h, 2.5h or 3h etc..
Preferably, the temperature of the drying is 80~100 DEG C such as 80 DEG C, 90 DEG C or 100 DEG C；And glass is used in drying process
Glass plate will be soaking after conductive nano folder live, avoid paper from crimping.
The present invention also provides a kind of conductive nano paper, are prepared by the preparation method of above-mentioned conductive nano paper.
The present invention also provides a kind of capacitors, including above-mentioned conductive nano paper.
Conductive nano paper of the invention is first obtained by being filtered by vacuum after being uniformly mixed nano-cellulose with conductive material
To nano conductive film, then nano conductive film is placed in again in the mixed aqueous solution of choline chloride and urea dry after impregnating
It arrives, not only transparency with higher, higher tensile strength and lower Young's modulus, and there is preferable electric conductivity, and
It is also with good stability as the capacitor of key component building.In addition, the preparation side of conductive nano paper of the invention
Method is simple, convenient, easily industrializes, and can preferably be applied in capacitor.In addition, conductive nano paper prepared by the present invention can also
To be applied to the fields such as transparent electrode and electroluminescent material.
To facilitate the understanding of the present invention, below with reference to embodiment to further illustrate the technical scheme of the present invention.Applicant
Statement, detailed process equipment and process flow of the invention that the present invention is explained by the above embodiments, but the present invention not office
It is limited to above-mentioned detailed process equipment and process flow, that is, does not mean that the present invention should rely on above-mentioned detailed process equipment and technique stream
Cheng Caineng is implemented.It should be clear to those skilled in the art, any improvement in the present invention, to each original of product of the present invention
The equivalence replacement of material and addition, the selection of concrete mode of auxiliary element etc. all fall within protection scope of the present invention and open model
Within enclosing.
Embodiment 1
(1) it prepares transparent substrate nano-cellulose: leaf wood pulpboard being placed in deionized water and impregnates and then stirs to get
Slurry carry out oxidation processes through TEMPO/NaBr/NaClO system, then through homogenization, nano-cellulose is made.
(2) prepare conductive mixture: take step (1) prepare nano-cellulose and nano-silver thread according to 100:0.5 matter
For amount than mixing, ultrasonic vibration 30min is uniformly mixed the two, obtains conductive mixture.
(3) nano conductive film is prepared: the conductive mixture for taking step (2) to prepare, after vacuum filtration to get conductive nano
Film.
(4) prepare conductive nano paper: the nano conductive film for taking step (3) to prepare immerses in choline chloride/urea aqueous solution,
After impregnating 12h, taking-up is clamped with glass plate is placed in 80 DEG C of baking ovens dry 3h to get conductive nano paper；Wherein, choline chloride and
In the mixed aqueous solution of urea: the mass ratio of choline chloride and urea is 1:1；The matter of the gross mass and water of choline chloride and urea
Amount is than being 0.02:1.
Embodiment 2
(1) it prepares transparent substrate nano-cellulose: leaf wood pulpboard being placed in deionized water and impregnates and then stirs to get
Slurry carry out oxidation processes through TEMPO/NaBr/NaClO system, then through homogenization, nano-cellulose is made.
(2) prepare conductive mixture: take step (1) prepare nano-cellulose and nano-silver thread according to 100:1 quality
Than mixing, ultrasonic vibration 30min is uniformly mixed the two, obtains conductive mixture.
(3) nano conductive film is prepared: the conductive mixture for taking step (2) to prepare, after vacuum filtration to get conductive nano
Film.
(4) prepare conductive nano paper: the nano conductive film for taking step (3) to prepare immerses in choline chloride/urea aqueous solution,
After impregnating 12h, taking-up is clamped with glass plate is placed in 90 DEG C of baking ovens dry 2.5h to get conductive nano paper；Wherein, choline chloride
In the mixed aqueous solution of urea: the mass ratio of choline chloride and urea is 1:1；The gross mass and water of choline chloride and urea
Mass ratio is 0.02:1.
Embodiment 3
(1) it prepares transparent substrate nano-cellulose: leaf wood pulpboard being placed in deionized water and impregnates and then stirs to get
Slurry carry out oxidation processes through TEMPO/NaBr/NaClO system, then through homogenization, nano-cellulose is made.
(2) prepare conductive mixture: take step (1) prepare nano-cellulose and nano-silver thread according to 100:1.5 matter
For amount than mixing, ultrasonic vibration 30min is uniformly mixed the two, obtains conductive mixture.
(3) nano conductive film is prepared: the conductive mixture for taking step (2) to prepare, after vacuum filtration to get conductive nano
Film.
(4) prepare conductive nano paper: the nano conductive film for taking step (3) to prepare immerses in choline chloride/urea aqueous solution,
After impregnating 12h, taking-up is clamped with glass plate is placed in 100 DEG C of baking ovens dry 2h to get conductive nano paper；Wherein, choline chloride
In the mixed aqueous solution of urea: the mass ratio of choline chloride and urea is 1:1；The gross mass and water of choline chloride and urea
Mass ratio is 0.02:1.
Embodiment 4
(1) it prepares transparent substrate nano-cellulose: Eucalyptus pulpboard being placed in deionized water and impregnates and then stirs to get
Slurry carries out oxidation processes through TEMPO/NaBr/NaClO system, then through homogenization, nano-cellulose is made.
(2) prepare conductive mixture: take step (1) prepare nano-cellulose and carbon nanotube according to 100:2 quality
Than mixing, ultrasonic vibration 15min is uniformly mixed the two, obtains conductive mixture.
(3) nano conductive film is prepared: the conductive mixture for taking step (2) to prepare, after vacuum filtration to get conductive nano
Film.
(4) prepare conductive nano paper: the nano conductive film for taking step (3) to prepare immerses in choline chloride/urea aqueous solution,
After impregnating 18h, taking-up is clamped with glass plate is placed in 100 DEG C of baking ovens dry 2h to get conductive nano paper；Wherein, choline chloride
In the mixed aqueous solution of urea: the mass ratio of choline chloride and urea is 1:2；The gross mass and water of choline chloride and urea
Mass ratio is 0.03:1.
Embodiment 5
(1) it prepares transparent substrate nano-cellulose: Eucalyptus pulpboard being placed in deionized water and impregnates and then stirs to get
Slurry carries out oxidation processes through TEMPO/NaBr/NaClO system, then through homogenization, nano-cellulose is made.
(2) conductive mixture is prepared: the nano-cellulose and poly- 3,4-ethylene dioxythiophene for taking step (1) to prepare: polyphenyl
Vinyl sulfonate is mixed according to the mass ratio of 100:2, and ultrasonic vibration 20min is uniformly mixed the two, obtains conductive mixture.
(3) nano conductive film is prepared: the conductive mixture for taking step (2) to prepare, after vacuum filtration to get conductive nano
Film.
(4) prepare conductive nano paper: the nano conductive film for taking step (3) to prepare immerses in choline chloride/urea aqueous solution,
After impregnating for 24 hours, taking-up is clamped with glass plate is placed in 90 DEG C of baking ovens dry 2.5h to get conductive nano paper；Wherein, choline chloride
In the mixed aqueous solution of urea: the mass ratio of choline chloride and urea is 1:2.5；The gross mass and water of choline chloride and urea
Mass ratio be 0.05:1.
Embodiment 6
(1) it prepares transparent substrate nano-cellulose: leaf wood pulpboard being placed in deionized water and impregnates and then stirs to get
Slurry carry out oxidation processes through TEMPO/NaBr/NaClO system, then through homogenization, nano-cellulose is made.
(2) prepare conductive mixture: take step (1) prepare nano-cellulose and nano-silver thread according to 100:1.5 matter
For amount than mixing, ultrasonic vibration 15min is uniformly mixed the two, obtains conductive mixture.
(3) nano conductive film is prepared: the conductive mixture for taking step (2) to prepare, after vacuum filtration to get conductive nano
Film.
(4) prepare conductive nano paper: the nano conductive film for taking step (3) to prepare immerses in choline chloride/urea aqueous solution,
After impregnating 15h, taking-up is clamped with glass plate is placed in 100 DEG C of baking ovens dry 2h to get conductive nano paper；Wherein, choline chloride
In the mixed aqueous solution of urea: the mass ratio of choline chloride and urea is 1:1.5；The gross mass and water of choline chloride and urea
Mass ratio be 0.01:1.
Comparative example 1
(1) it prepares transparent substrate nano-cellulose: leaf wood pulpboard being placed in deionized water and impregnates and then stirs to get
Slurry carry out oxidation processes through TEMPO/NaBr/NaClO system, then through homogenization, nano-cellulose is made.
(2) prepare conductive mixture: take step (1) prepare nano-cellulose and nano-silver thread according to 100:0.5 matter
For amount than mixing, ultrasonic vibration 30min is uniformly mixed the two, obtains conductive mixture.
(3) prepare nano conductive film: the conductive mixture for taking step (2) to prepare obtains conductive nano after vacuum filtration
The nano conductive film is clamped with glass plate and is placed in 100 DEG C of baking ovens dry 2h, obtains conductive nano paper by film.
To the optical picture of conductive nano paper prepared in the above embodiments, visible light transmittance, the pattern of nano-cellulose, drawing
Stretch-deformation, soft or hard degree and electric conductivity detected, as a result as shown in Fig. 1~Fig. 6；And it prepared by the embodiment of the present invention
The capacitor stability of capacitor that constructs as key component of conductive nano paper detected, test structure is as shown in Figure 7.
Wherein, Fig. 1 is the embodiment of the present invention 1~3 respectively by the preparation of the mass ratio of different nano-celluloses and conductive material
Conductive nano paper optics picture.
Fig. 2 is the embodiment of the present invention 1~5 respectively by the nanometer of the mass ratio of different nano-celluloses and conductive material preparation
The visible light transmittance curve graph of conductive paper.
Fig. 3 is the scanning electron microscope (SEM) photograph of nano-cellulose prepared by embodiment 1.
Fig. 4 is the scanning electron microscope (SEM) photograph of conductive nano paper prepared by embodiment 1.
Fig. 5 is receiving for the different quality containing preparation that the embodiment of the present invention 1~5 is accounted for nano-cellulose by conductive material respectively
Stretching-inflection curves of rice conductive paper, conductive nano paper prepared by comparative example 1 and pure nano-cellulose paper.
Fig. 6 is receiving for the different quality containing preparation that the embodiment of the present invention 1~5 is accounted for nano-cellulose by conductive material respectively
The Young's modulus figure of rice conductive paper, conductive nano paper prepared by comparative example 1 and pure nano-cellulose paper.
Fig. 7 is the cyclic voltammetry curve figure of conductive nano paper prepared by the embodiment of the present invention 1.
Fig. 8 is the capacitor reservation for the capacitor that conductive nano paper prepared by the embodiment of the present invention 1 is constructed as key component
Test curve figure.
(1) from Fig. 1 and Fig. 2 result: as the mass ratio of nano-cellulose and conductive material is higher, obtained nanometer
The transparency of conductive paper is higher.
(2) shape appearance figure of nano-cellulose prepared by embodiment 1 can be turned out to be by Fig. 3 result；It should be noted that real
The pattern for applying the nano-cellulose of a 2-6 and the preparation of comparative example 1 is identical with the shape appearance figure.
(3) shape appearance figure of conductive nano paper prepared by embodiment 1 can be turned out to be by Fig. 4 result；It should be noted that real
The pattern for applying the nano-cellulose of a 2-6 and the preparation of comparative example 1 is identical with the shape appearance figure.
(4) from Fig. 5 result: the tensile strength of the conductive nano paper of preparation of the embodiment of the present invention is much higher than comparative example 1
The tensile strength of the conductive nano paper of preparation and pure nano-cellulose paper；Therefore, nano-cellulose and conductive material are mixed with
Nano conductive film in the conductive nano paper obtained after the immersion treatment of choline chloride/urea aqueous solution, can show
Preferable tensile property, tensile deformation up to 17%, be conductive nano paper that nano-cellulose and conductive material are mixed with and
More than ten times of pure nano-cellulose paper.Also, as the mass fraction that conductive material accounts for nano-cellulose is lower, i.e. conductive material
Dosage it is fewer, the tensile strength of obtained conductive nano paper is stronger.
(5) by Fig. 6 result it is found that the Young's modulus of the conductive nano paper of preparation of the embodiment of the present invention is far below comparative example 1
The Young's modulus of the conductive nano paper of preparation and pure nano-cellulose paper, the i.e. embodiment of the present invention preparation conductive nano paper it is soft
It is soft more preferable, also, as the mass fraction that conductive material accounts for nano-cellulose is lower, i.e. the dosage of conductive material is fewer, obtains
The Young's modulus of the conductive nano paper arrived is lower, and flexibility is more preferable.
(6) by Fig. 7 result it is found that conductive nano paper prepared by the embodiment of the present invention 1 has preferable electric conductivity；It needs
Bright, prepared by the electric conductivity and the embodiment of the present invention 1 of the conductive nano paper of 2-6 of embodiment of the present invention preparation conductive nano paper
Electric conductivity it is suitable.
(7) by Fig. 8 result it is found that the capacitor that conductive nano paper prepared by the embodiment of the present invention 1 is constructed as key component
Device has good capacitor stability；It should be noted that the conductive nano paper of 2-6 of embodiment of the present invention preparation is as crucial group
Conductive nano paper prepared by the capacitor and the embodiment of the present invention 1 of part building is protected as the capacitor for the capacitor that key component constructs
Stay test curve figure suitable, i.e. the capacitor that the conductive nano paper of 2-6 of embodiment of the present invention preparation is constructed as key component is also
It is with good stability.
To sum up, the conductive nano paper transparency with higher and higher tensile strength of preparation of the embodiment of the present invention, and
With preferable electric conductivity, and it is also with good stability as the capacitor of key component building.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of conductive nano paper, it is characterised in that: include:
Nano conductive film is obtained through vacuum filtration after nano-cellulose is uniformly mixed with conductive material；
The nano conductive film is placed in the mixed aqueous solution of choline chloride and urea and is impregnated, then takes out drying.
2. the preparation method of conductive nano paper according to claim 1, it is characterised in that: the nano-cellulose pass through by
Hardwood pulp, eucalyptus pulp or softwood pulp carry out oxidation through TEMPO/NaBr/NaClO system and homogenization obtains.
3. the preparation method of conductive nano paper according to claim 1, it is characterised in that: the conductive material is nano silver
Line, poly- 3,4-ethylene dioxythiophene: poly styrene sulfonate, graphene, carbon nanotube and conductive metal nanometer powder in
It is one or more.
4. the preparation method of conductive nano paper according to claim 1, it is characterised in that: the dosage of the conductive material is
0.5~2.5wt% of the quality of the nano-cellulose.
5. the preparation method of conductive nano paper according to claim 1, it is characterised in that: it is described by nano-cellulose with lead
The process of electric material mixing includes: 15~30min of ultrasonic vibration after mixing nano-cellulose with conductive material.
6. the preparation method of conductive nano paper according to claim 1, it is characterised in that: the choline chloride and urea
In mixed aqueous solution: the mass ratio of choline chloride and urea is 1:(1~3), the matter of the gross mass and water of choline chloride and urea
Amount is than being (0.01~0.05): 1.
7. the preparation method of conductive nano paper according to claim 1, it is characterised in that: the time of the immersion be 12~
24h。
8. the preparation method of conductive nano paper according to claim 1, it is characterised in that: the time of the drying be 2~
3h；The temperature of the drying is 80~100 DEG C.
9. a kind of conductive nano paper, it is characterised in that: its by conductive nano paper according to any one of claims 1 to 8 preparation
Method is prepared.
10. a kind of capacitor, it is characterised in that: including conductive nano paper as claimed in claim 9.
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