CN103440986B - A kind of graphite oxide base transparent solid-state electrolyte preparation method - Google Patents
A kind of graphite oxide base transparent solid-state electrolyte preparation method Download PDFInfo
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- CN103440986B CN103440986B CN201310314479.1A CN201310314479A CN103440986B CN 103440986 B CN103440986 B CN 103440986B CN 201310314479 A CN201310314479 A CN 201310314479A CN 103440986 B CN103440986 B CN 103440986B
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Abstract
The present invention provides a kind of graphite oxide base transparent solid-state electrolyte preparation method, and described preparation method is as follows: be dispersed in deionized water or organic solvent by graphite oxide matrix, forms graphite oxide dispersion；Again toward graphite oxide dispersion is added inorganic ions conductor or the ion conductor containing the group that can become hydrogen bond with hydroxyl, carboxyl, by the complexing between the hydroxyl on graphite oxide, carboxyl and inorganic metal ion or and ion conductor group between hydrogen bond action make inorganic ions conductor or ion conductor dissolve to be distributed on graphite oxide matrix；Finally deionized water or organic solvent are evaporated, obtain graphite oxide base transparent solid-state electrolyte.Preparation method simple possible of the present invention also can obtain transparent solid electrolyte, all has broad application prospects in the transparent photoelectric chemical device particularly field such as sensitization solar battery and capacitor.
Description
[technical field]
The present invention relates to a kind of graphite oxide base transparent solid-state electrolyte preparation method.
[background technology]
The electrolyte of ionic conduction is the key component of the device such as sensitization solar battery and capacitor, to it
Performance and long-time stability play a decisive role.Traditional sensitization solar battery and capacitor mostly use
Liquid electrolyte.Complicated due to sealing technology in actual use, liquid electrolyte is easily from battery
Internal leakage is out.It addition, solvent is volatile under high temperature, it is also possible to other component reaction of device, because of
And the service life of sensitization solar battery or capacitor can be shortened.Additionally, the use of liquid electrolyte is also
The stability that can make device is greatly affected.Therefore, using non liquid state electrolyte is sensitization solar electricity
Practical key technology is moved towards in pond.Ion conductor is dissolved or is distributed to spy by a kind of effective method exactly
Determine in matrix, form all solid state electrolyte.The appearance of transparent devices in recent years, more requires that exploitation is transparent
These electrolyte are used in sensitization solar battery by electrolyte, can build the battery of double-side photic, energy
The utilization rate of sunlight is greatly improved, with in the capacitor, then can build transparent device, it is adaptable to right
Printing opacity has in the electronic product of particular/special requirement.Therefore, the exploitation of transparent electrolyte is significant.
In view of this, this process, on the basis of a series of research and test, develops one
Planting graphite oxide base transparent solid-state electrolyte preparation method, this case thus produces.
[summary of the invention]
The technical problem to be solved in the present invention, is to provide a kind of graphite oxide base transparent solid-state electrolyte
Preparation method, this preparation method simple possible also can obtain transparent solid electrolyte, in transparent optical electrification
Learn the device particularly field such as sensitization solar battery and capacitor all to have broad application prospects.
The present invention is achieved in that
A kind of graphite oxide base transparent solid-state electrolyte preparation method, described preparation method is as follows:
Graphite oxide matrix is dispersed in deionized water or organic solvent, forms graphite oxide dispersion；
Inorganic ions conductor is added or containing the group that can become hydrogen bond with hydroxyl, carboxyl again in graphite oxide dispersion
Ion conductor, made by complexation between the hydroxyl on graphite oxide, carboxyl and inorganic metal ion
With or and ion conductor group between hydrogen bond action make inorganic ions conductor or ion conductor molten
Solution is distributed on graphite oxide matrix；Finally deionized water or organic solvent are evaporated, obtain graphite oxide
Base transparent solid-state electrolyte.
Further, described graphite oxide matrix is, by hummer method, graphite is transformed into graphite oxide,
Obtain after centrifugal segregation impurity.
Further, described graphite oxide matrix carries out ultrasonic after being dispersed in deionized water or organic solvent
Vibration, makes graphite oxide matrix stripping become graphite oxide microplate or graphene oxide.
Further, the metal cation of described inorganic ions conductor can be described with hydroxyl, carboxyl complexation
Group contained by ion conductor is at least one in amino, hydroxyl, ether and carboxyl.
Further, at least during described organic solvent is methanol, ethanol, dimethyl sulfoxide, two formyls
Kind.
Further, described inorganic ions conductor is NaI, NaIx、LiI、Na2S、、Na2Sx、LiClO4
In at least one.
Further, described graphite oxide matrix and inorganic ions conductor or the mass ratio of ion conductor
It is 100/1～2/1.
Present invention have the advantage that
Using transparent solid-state electrolyte prepared by this method, technique is simple, and the electrical conductivity of electrolyte reaches
8～12mS/cm, sensitization solar battery can be met and capacitor uses requirement, it is seen that light light transmittance reaches
To 50～70%, transparent or semitransparent device can be obtained；For having certain transparency, energy double-side photic
Sensitization solar battery or transmittance is required, and the preparation of higher capacitor and practical offer are crucial
Component, and establish good basis.
[detailed description of the invention]
The present invention relates to a kind of graphite oxide base transparent solid-state electrolyte preparation method, described preparation method
As follows:
Graphite oxide matrix is dispersed in deionized water or organic solvent, forms graphite oxide dispersion；
Inorganic ions conductor is added or containing the group that can become hydrogen bond with hydroxyl, carboxyl again in graphite oxide dispersion
Ion conductor, made by complexation between the hydroxyl on graphite oxide, carboxyl and inorganic metal ion
With or and ion conductor group between hydrogen bond action make inorganic ions conductor or ion conductor molten
Solution is distributed on graphite oxide matrix；Finally deionized water or organic solvent are evaporated, obtain graphite oxide
Base transparent solid-state electrolyte.
Described graphite oxide matrix is, by hummer method, graphite is transformed into graphite oxide, and centrifugal segregation is miscellaneous
Obtain after matter.
Described graphite oxide matrix carries out sonic oscillation after being dispersed in deionized water or organic solvent, makes oxygen
Graphite matrix stripping becomes graphite oxide microplate or graphene oxide.
The metal cation of described inorganic ions conductor can be led with hydroxyl, carboxyl complexation, described organic ion
Group contained by body is at least one in amino, hydroxyl, ether and carboxyl.
Described organic solvent is at least one in methanol, ethanol, dimethyl sulfoxide, two formyls.
Described inorganic ions conductor is NaI, NaIx、LiI、Na2S、、Na2Sx、LiClO4In extremely
Few one.
Described graphite oxide matrix with the mass ratio of inorganic ions conductor or ion conductor is
100/1～2/1.
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment
First, the preparation of graphite oxide: first, pour 300 commercially available mesh graphite particulate 2g into 250mL
In beaker, under the conditions of ice-water bath, it is added thereto to 1g NaNO3Rear addition 46mL H2SO4And fully
Stirring, continuously adds 6g potassium permanganate and keeps solution reaction temperature at 20 DEG C of 5min, remove ice bath and make instead
Answer temperature to be increased to 35 DEG C and keep 30min, add 92mL deionized water afterwards, stir 15min,
Temperature is increased to 98 DEG C, continuously adds 80mL60 DEG C of 3vol.% hydrogen peroxide, and reactant liquor becomes brown.
Secondly, by the solution of brown in centrifuge with 3000 revs/min of centrifugal 10min, remove unreacted and anti-
Answer incomplete graphite particulate, by upper liquid again at 12000 revs/min of centrifugal 30min, precipitation is distributed to
In deionized water, high speed centrifugation again, obtain pure graphite oxide the most afterwards.
Second step, containing the preparation of graphite oxide liquid electrolyte: the pure oxidation stone first step obtained
Ink 20g, NaI3g, I25g is distributed in 500mL ethanol, and sonic oscillation 2h makes graphite oxide shell
From becoming graphite oxide microplate or graphene oxide, and ion conductor is made to be sufficiently mixed with graphite oxide.
3rd step, the preparation of transparent solid-state electrolyte: the liquid electrolyte 2mL that second step obtains is dropped in
On glass substrate, it is placed in heat treatment 1h in 60 DEG C of heating plates, then is placed in 60 DEG C of process in vacuum drying oven
12h, can obtain transparent solid-state electrolyte, or directly instillation area is 1cm2Sensitization solar electricity
In the device such as pond or capacitor, device is placed in heat treatment 1h in 60 DEG C of heating plates, then is placed in vacuum
In baking oven, 60 DEG C process 12h, can obtain the device being filled with transparent solid-state electrolyte.
The electrical conductivity of above-mentioned prepared transparent solid-state electrolyte is 9mS/cm；Visible light transmittance rate is 50%.
Using transparent solid-state electrolyte prepared by this method, technique is simple, and the electrical conductivity of electrolyte reaches
8～12mS/cm, sensitization solar battery can be met and capacitor uses requirement, it is seen that light light transmittance reaches
To 50～70%, transparent or semitransparent device can be obtained；For having certain transparency, energy double-side photic
Sensitization solar battery or transmittance is required, and the preparation of higher capacitor and practical offer are crucial
Component, and establish good basis.
Although the foregoing describing the detailed description of the invention of the present invention, but it is familiar with the technology people of the art
Member should be appreciated that our described specific embodiment is merely exemplary rather than for this
The restriction of bright scope, those of ordinary skill in the art are in the equivalence made according to the spirit of the present invention
Modify and change, all should contain in the scope of the claimed protection of the present invention.
Claims (6)
1. a graphite oxide base transparent solid-state electrolyte preparation method, it is characterised in that: described preparation method is as follows:
Graphite oxide matrix is dispersed in deionized water or organic solvent, forms graphite oxide dispersion；Again toward graphite oxide dispersion is added inorganic ions conductor or the ion conductor containing the group that can become hydrogen bond with hydroxyl, carboxyl, by the complexing between the hydroxyl on graphite oxide, carboxyl and inorganic metal ion or and ion conductor group between hydrogen bond action make inorganic ions conductor or ion conductor dissolve to be distributed on graphite oxide matrix；Finally deionized water or organic solvent are evaporated, obtain graphite oxide base transparent solid-state electrolyte；Described graphite oxide matrix is 100/1～2/1 with the mass ratio of inorganic ions conductor or ion conductor.
2. a kind of graphite oxide base transparent solid-state electrolyte preparation method as claimed in claim 1, it is characterised in that: described graphite oxide matrix is, by hummer method, graphite is transformed into graphite oxide, obtains after centrifugal segregation impurity.
3. a kind of graphite oxide base transparent solid-state electrolyte preparation method as claimed in claim 1, it is characterized in that: described graphite oxide matrix carries out sonic oscillation after being dispersed in deionized water or organic solvent, make graphite oxide matrix stripping become graphite oxide microplate or graphene oxide.
4. a kind of graphite oxide base transparent solid-state electrolyte preparation method as claimed in claim 1, it is characterized in that: the metal cation of described inorganic ions conductor can be with hydroxyl, carboxyl complexation, and group contained by described ion conductor is at least one in amino, hydroxyl, ether and carboxyl.
5. a kind of graphite oxide base transparent solid-state electrolyte preparation method as claimed in claim 1, it is characterised in that: described organic solvent is at least one in methanol, ethanol, dimethyl sulfoxide, two formyls.
6. a kind of graphite oxide base transparent solid-state electrolyte preparation method as claimed in claim 4, it is characterised in that: described inorganic ions conductor is NaI, NaIx、LiI、Na2S、Na2Sx、LiClO4In at least one.
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