CN103440986A - Method for preparing graphite oxide base transparent solid electrolyte - Google Patents
Method for preparing graphite oxide base transparent solid electrolyte Download PDFInfo
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- CN103440986A CN103440986A CN2013103144791A CN201310314479A CN103440986A CN 103440986 A CN103440986 A CN 103440986A CN 2013103144791 A CN2013103144791 A CN 2013103144791A CN 201310314479 A CN201310314479 A CN 201310314479A CN 103440986 A CN103440986 A CN 103440986A
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- graphite oxide
- solid electrolyte
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- oxide base
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Abstract
The invention provides a method for preparing a graphite oxide base transparent solid electrolyte. The preparation method comprises the steps: dispersing graphite oxide base bodies in deionized water or an organic solvent, forming graphite oxide dispersion liquid, then adding inorganic ionic conductors or organic ion conductors containing groups which can form hydrogen bonds with hydroxide radicals and carboxyls into the graphite oxide dispersion liquid, dissolving and dispersing inorganic ionic conductors or the organic ion conductors in the graphite oxide base bodies through the complexing action between the hydroxide radicals and carboxyls on the graphite oxide and inorganic metal ions or the hydrogen bond action between the hydroxide radicals and carboxyls on the graphite oxide and the groups of the organic ion conductors, and fully evaporating the deionized water or the organic solvent so as to obtain the graphite oxide base transparent solid electrolyte. The preparation method is easy and feasible, can obtain the transparent solid electrolyte, and has wide application prospects in the fields of transparent photoelectrochemical devices, particularly sensitization solar cells, capacitors and the like.
Description
[technical field]
The present invention relates to the preparation method of the transparent solid electrolyte of a kind of graphite oxide base.
[background technology]
The electrolyte of ionic conduction is the key component of the devices such as sensitization solar battery and capacitor, and its performance and long-time stability are played a decisive role.Traditional sensitization solar battery and capacitor mostly adopt liquid electrolyte.Due to the sealing technology complexity, liquid electrolyte easily leaks out from inside battery in actual use.In addition, under high temperature, solvent is volatile, also may with other component reaction of device, thereby can shorten useful life of sensitization solar battery or capacitor.In addition, the use of liquid electrolyte also can make the stability of device be greatly affected.Therefore, using non liquid state electrolyte is that sensitization solar battery moves towards practical key technology.A kind of effective method dissolves ion conductor or be distributed in particular substrate exactly, forms all solid state electrolyte.The appearance of transparent devices in recent years, more require the transparent electrolyte of exploitation, these electrolyte are used in sensitization solar battery, can build the two-sided battery that is subject to light, can significantly improve the utilance of sunlight, be used in capacitor, can build transparent device, being applicable to has in the electronic product of specific (special) requirements printing opacity.Therefore, transparent electrolytical exploitation is significant.
In view of this, this process, on the basis through a series of research and test, is developed the preparation method of the transparent solid electrolyte of a kind of graphite oxide base, and this case produces thus.
[summary of the invention]
The technical problem to be solved in the present invention, be to provide the preparation method of the transparent solid electrolyte of a kind of graphite oxide base, this preparation method's simple possible also can obtain transparent solid electrolyte, in the transparent photoelectric chemical device, particularly all has broad application prospects in the field such as sensitization solar battery and capacitor.
The present invention is achieved in that
The preparation method of the transparent solid electrolyte of a kind of graphite oxide base, described preparation method is as follows:
The graphite oxide matrix is dispersed in deionized water or organic solvent, forms the graphite oxide dispersion liquid; Again toward adding the inorganic ions conductor in the graphite oxide dispersion liquid or containing becoming with hydroxyl, carboxyl the ion conductor of the group of hydrogen bond, by the complexing between the hydroxyl on graphite oxide, carboxyl and inorganic metal ion or and the ion conductor group between hydrogen bond action inorganic ions conductor or ion conductor are dissolved be distributed on the graphite oxide matrix; Finally, by deionized water or organic solvent evaporate to dryness, obtain the transparent solid electrolyte of graphite oxide base.
Further, described graphite oxide matrix is, by the hummer method, graphite is transformed into to graphite oxide, after centrifugal removal impurity, obtains.
Further, described graphite oxide matrix carries out sonic oscillation after being dispersed in deionized water or organic solvent, makes the graphite oxide matrix stripping become graphite oxide microplate or graphene oxide.
Further, the metal cation of described inorganic ions conductor can with hydroxyl, carboxyl complexing, the contained group of described ion conductor is at least one in amino, hydroxyl, ether and carboxyl.
Further, described organic solvent is at least one in methyl alcohol, ethanol, methyl-sulfoxide, two formyls.
Further, described inorganic ions conductor is NaI, NaI
x, LiI, Na
2s,, Na
2s
x, LiClO
4in at least one.
Further, the mass ratio of described graphite oxide matrix and inorganic ions conductor or ion conductor is 100/1～2/1.
The present invention has following advantage:
The transparent solid electrolyte that adopts this method to prepare, technique is simple, and electrolytical conductivity reaches 8～12mS/cm, can meet sensitization solar battery and capacitor instructions for use, and visible light transmittance rate reaches 50～70%, can obtain transparent or semitransparent device; For preparation and the practical key component that provides of certain transparency, the two-sided capacitor that is subject to the sensitization solar battery of light or light transmittance is had relatively high expectations of energy are provided, and establish good basis.
[embodiment]
The present invention relates to the preparation method of the transparent solid electrolyte of a kind of graphite oxide base, described preparation method is as follows:
The graphite oxide matrix is dispersed in deionized water or organic solvent, forms the graphite oxide dispersion liquid; Again toward adding the inorganic ions conductor in the graphite oxide dispersion liquid or containing becoming with hydroxyl, carboxyl the ion conductor of the group of hydrogen bond, by the complexing between the hydroxyl on graphite oxide, carboxyl and inorganic metal ion or and the ion conductor group between hydrogen bond action inorganic ions conductor or ion conductor are dissolved be distributed on the graphite oxide matrix; Finally, by deionized water or organic solvent evaporate to dryness, obtain the transparent solid electrolyte of graphite oxide base.
Described graphite oxide matrix is, by the hummer method, graphite is transformed into to graphite oxide, after centrifugal removal impurity, obtains.
Described graphite oxide matrix carries out sonic oscillation after being dispersed in deionized water or organic solvent, makes the graphite oxide matrix stripping become graphite oxide microplate or graphene oxide.
The metal cation of described inorganic ions conductor can with hydroxyl, carboxyl complexing, the contained group of described ion conductor is at least one in amino, hydroxyl, ether and carboxyl.
Described organic solvent is at least one in methyl alcohol, ethanol, methyl-sulfoxide, two formyls.
Described inorganic ions conductor is NaI, NaI
x, LiI, Na
2s,, Na
2s
x, LiClO
4in at least one.
The mass ratio of described graphite oxide matrix and inorganic ions conductor or ion conductor is 100/1～2/1.
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment
The first, the preparation of graphite oxide: at first, 300 commercially available order graphite particulate 2g are poured in the 250mL beaker, add wherein 1g NaNO under the ice-water bath condition
3after add 46mL H
2sO
4and fully stir, continue to add 6g potassium permanganate to keep the solution reaction temperature at 20 ℃ of 5min, removing ice bath makes reaction temperature be elevated to 35 ℃ of maintenance 30min, add afterwards the 92mL deionized water, stir 15min, temperature is elevated to 98 ℃, continues to add 80mL60 ℃ of 3vol.% hydrogen peroxide, and reactant liquor becomes brown.Secondly, by brown solution in centrifuge with 3000 rev/mins of centrifugal 10min, remove unreacted and react incomplete graphite particulate, by upper strata liquid again at 12000 rev/mins of centrifugal 30min, precipitation is distributed in deionized water, and high speed centrifugation, obtain pure graphite oxide after triplicate again.
Second step contains the preparation of graphite oxide liquid electrolyte: pure graphite oxide 20g, NaI3g, I that the first step is obtained
25g is distributed in 500mL ethanol, and sonic oscillation 2h makes graphite oxide peel off into graphite oxide microplate or graphene oxide, and ion conductor is fully mixed with graphite oxide.
The 3rd step, the preparation of transparent solid electrolyte: the liquid electrolyte 2mL that second step is obtained drops on glass substrate, is placed in heat treatment 1h on 60 ℃ of heating plates, then is placed in 60 ℃ of processing 12h of vacuum drying oven, can obtain transparent solid electrolyte, or directly to splash into area be 1cm
2sensitization solar battery or the device such as capacitor in, device is placed in to heat treatment 1h on 60 ℃ of heating plates, then is placed in 60 ℃ of vacuum drying ovens and processes 12h, can obtain the device that is filled with transparent solid electrolyte.
The conductivity of the above-mentioned transparent solid electrolyte made is 9mS/cm; Visible light transmittance rate is 50%.
The transparent solid electrolyte that adopts this method to prepare, technique is simple, and electrolytical conductivity reaches 8～12mS/cm, can meet sensitization solar battery and capacitor instructions for use, and visible light transmittance rate reaches 50～70%, can obtain transparent or semitransparent device; For preparation and the practical key component that provides of certain transparency, the two-sided capacitor that is subject to the sensitization solar battery of light or light transmittance is had relatively high expectations of energy are provided, and establish good basis.
Although more than described the specific embodiment of the present invention; but being familiar with those skilled in the art is to be understood that; our described specific embodiment is illustrative; rather than for the restriction to scope of the present invention; those of ordinary skill in the art are in modification and the variation of the equivalence of doing according to spirit of the present invention, all should be encompassed in the scope that claim of the present invention protects.
Claims (7)
1. the preparation method of the transparent solid electrolyte of graphite oxide base, it is characterized in that: described preparation method is as follows:
The graphite oxide matrix is dispersed in deionized water or organic solvent, forms the graphite oxide dispersion liquid; Again toward adding the inorganic ions conductor in the graphite oxide dispersion liquid or containing becoming with hydroxyl, carboxyl the ion conductor of the group of hydrogen bond, by the complexing between the hydroxyl on graphite oxide, carboxyl and inorganic metal ion or and the ion conductor group between hydrogen bond action inorganic ions conductor or ion conductor are dissolved be distributed on the graphite oxide matrix; Finally, by deionized water or organic solvent evaporate to dryness, obtain the transparent solid electrolyte of graphite oxide base.
2. the preparation method of the transparent solid electrolyte of a kind of graphite oxide base as claimed in claim 1, it is characterized in that: described graphite oxide matrix is, by the hummer method, graphite is transformed into to graphite oxide, after centrifugal removal impurity, obtains.
3. the preparation method of the transparent solid electrolyte of a kind of graphite oxide base 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, makes the graphite oxide matrix stripping become graphite oxide microplate or graphene oxide.
4. the preparation method of the transparent solid electrolyte of a kind of graphite oxide base as claimed in claim 1, it is characterized in that: the metal cation of described inorganic ions conductor can with hydroxyl, carboxyl complexing, the contained group of described ion conductor is at least one in amino, hydroxyl, ether and carboxyl.
5. the preparation method of the transparent solid electrolyte of a kind of graphite oxide base as claimed in claim 1, it is characterized in that: described organic solvent is at least one in methyl alcohol, ethanol, methyl-sulfoxide, two formyls.
6. the preparation method of the transparent solid electrolyte of a kind of graphite oxide base as claimed in claim 4, it is characterized in that: described inorganic ions conductor is NaI, NaI
x, LiI, Na
2s,, Na
2s
x, LiClO
4in at least one.
7. the preparation method of the transparent solid electrolyte of a kind of graphite oxide base as claimed in claim 1, it is characterized in that: the mass ratio of described graphite oxide matrix and inorganic ions conductor or ion conductor is 100/1～2/1.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102891335A (en) * | 2012-10-11 | 2013-01-23 | 同济大学 | Preparation method of full-solid-state nano composite polymer electrolyte |
| CN103187588A (en) * | 2011-12-27 | 2013-07-03 | 财团法人工业技术研究院 | Solid electrolyte, lithium battery with solid electrolyte and electrochemical carrier structure |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103187588A (en) * | 2011-12-27 | 2013-07-03 | 财团法人工业技术研究院 | Solid electrolyte, lithium battery with solid electrolyte and electrochemical carrier structure |
| CN102891335A (en) * | 2012-10-11 | 2013-01-23 | 同济大学 | Preparation method of full-solid-state nano composite polymer electrolyte |
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