CN109545965A - Electric storage material based on tannic acid and iron (III) coordination compound, preparation method thereof and electric storage device - Google Patents
Electric storage material based on tannic acid and iron (III) coordination compound, preparation method thereof and electric storage device Download PDFInfo
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having a potential-jump barrier or a surface barrier
- H10K10/20—Organic diodes
- H10K10/23—Schottky diodes
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/30—Coordination compounds
- H10K85/331—Metal complexes comprising an iron-series metal, e.g. Fe, Co, Ni
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Abstract
The invention discloses the preparation of electrical storage materials and devices based on tannic acid and iron (III) coordination compounds. Aiming at the problems that the existing preparation process is complex, organic compound molecules are not easy to form a film, the application of the organic compound molecules in a flexible device is limited, and the like, the invention utilizes the tannic acid and the iron (III) coordination compound to prepare the simple sandwich organic-electric memory device, and successfully realizes the organic-electric memory behavior. In the preparation experiment process, the synthesis of molecules and the preparation process of devices are realized, and the prepared flexible substrate device has great practical value on the application aspect of the organic electric storage in the future flexible devices, so that the application field of the organic electric storage device is greatly expanded.
Description
Technical field
The invention belongs to organic semiconducting materials technical fields, are related to tannic acid and iron (III) complex electricity storage material
The preparation of material, and the electrical storage device of more flexible substrates by organic matter complex material preparation.
Background technique
Recently as the explosive growth of information, traditional binary memory device is no longer satisfied current information storage
The requirement deposited promotes the development to Ultrahigh-Density Data Storage technology.Organic electrical storage device is due to, volume low with weight
Small, easy to process, structure is changeable at low cost and has received the advantages that easily realizing the write-in and reading of information on a molecular scale wide
General concern.But since organic coordination compounds intermolecular force is small, in conjunction with unstable, environmental pollution is serious, soft
It is not easy the problems such as forming a film in property substrate, this hinders application of the organic coordination compounds in terms of multi-system information storage significantly.
Summary of the invention
For above situation, the purpose of the present invention is intended to provide the electricity storage based on tannic acid and iron (III) complex
The preparation method of material, and the device prepared by this kind of method, compared with traditional device, the Organic Electricity in the present invention is deposited
The cut-in voltage of memory device is low, and V twiceth1And Vth2Fine differentiation is obtained.
To achieve the goals above, present invention employs following technical solutions:
The sediment of tannic acid and iron (III) complex is preparing the application in electric storage material or electrical storage device.
The preparation method of electric storage material of the one kind based on tannic acid and iron (III) complex, includes the following steps,
After tannic acid solution is mixed with Iron(III) chloride hexahydrate solution, alkali is added and obtains the heavy of tannic acid and iron (III) complex
Starch；Then organic matter film is made in the sediment of tannic acid and iron (III) complex, obtained based on tannic acid and iron
(III) the electric storage material of complex.
In above-mentioned technical proposal, can in existing substrate by the sediment of tannic acid and iron (III) complex at
Film.
The preparation method of electrical storage device of the one kind based on tannic acid and iron (III) complex, includes the following steps,
By in the mixed liquor of conductive substrates merging tannic acid solution and Iron(III) chloride hexahydrate solution, alkali is then added, in conductive substrates
Surface prepare the sediment of tannic acid and iron (III) complex；Then tannic acid and iron (III) complex will be had
The dry surface in conductive substrates of conductive substrates of sediment prepare organic matter film；Finally electricity is prepared on organic matter film surface
Pole obtains the electrical storage device based on tannic acid and iron (III) complex.
In the present invention, organic matter film with a thickness of 5~30nm, preferably 15~25nm；It can be controlled by sediment.
In the present invention, tannic acid, Iron(III) chloride hexahydrate mass ratio be 4: 1；The concentration of tannic acid solution is 0.4mg/
ML, the concentration of Iron(III) chloride hexahydrate solution are 0.1mg/mL.
In the present invention, alkali is sodium hydroxide.
It is dry to be dried in vacuo 8 hours for 50 DEG C by being dried to obtain organic matter film in the present invention.
In the present invention, conductive substrates include ito glass, gold-plated flexible substrates；It is preferred that the ito glass of surface hydroxyl modification,
For example surface hydroxyl modification is carried out to ito glass with the concentrated sulfuric acid and hydrogen peroxide configuration decorating liquid, tannic acid and iron can be improved
(III) growth film-formation result of the sediment of complex on its surface；Flexible substrates are existing product.
In the present invention, electrode with a thickness of 80~90nm, electrode material is aluminium, in the form of aluminium wire exist, pass through sand paper
It polishes aluminium wire surface.
Electrical storage device disclosed by the invention is ito glass device, flexible substrates device, and preparation method can be such that
The preparation of ito glass device:
1, ito glass substrate is cleaned using the method for ultrasonic cleaning；
2, ito glass substrate is modified by modifying solution, forms decorative layer, wherein decorative layer with a thickness of single layer
The thickness of polyhydroxylated molecule；
3, decorative layer modification ITO substrate on form organic matter film, wherein organic matter film with a thickness of 5 ~ 30nm；
4, electrode material is plated in organic matter film by vapour deposition method and forms electrode, wherein the electrode with a thickness of 80~
90nm finally obtains the organic compound material electrical storage device of the ito glass substrate based on decorative layer modification.
In the above preparation method, ultrapure water, dehydrated alcohol, acetone, anhydrous second are successively used in cleaning as described in step (1)
Alcohol is completed.
In the above preparation method, ito glass size of foundation base described in step (1) is 2 × 2cm2。
In the above preparation method, modification solution described in step (2) is 98% concentrated sulfuric acid and 30% hydrogen peroxide
It is formulated.
In above-mentioned preparation method, in step (3), the ITO substrate of decorative layer modification is placed in tannic acid solution and six
In the mixed liquor of trichloride hydrate ferrous solution, alkali is then added, prepares tannic acid and iron (III) coordination on the surface of conductive substrates
The sediment of compound；Then by the conductive substrates drying with the sediment of tannic acid and iron (III) complex in conduction
The surface of substrate prepares organic matter film.
The preparation of flexible substrates device:
In the above preparation method, in step (4), the electrode material is aluminium, exists in the form of aluminium wire, passes through sand paper pair
It polishes on aluminium wire surface.
Its key step is as follows:
1, nanogold sheath is made on the flexible substrates surface that dehydrated alcohol wipes using magnetron sputtering, wherein the nanometer sputtered
Gold ion layer is with a thickness of 80 rans；
2, form organic matter film on nanogold sheath, the organic matter film of formation with a thickness of 5~30nm；
3, electrode material is vaporized in organic matter film and forms electrode, wherein the electrode with a thickness of 80~90nm, finally
Obtain more base flexible organic compound material electricity storage molecule devices；
In the above preparation method, flexible substrates are respectively PET, PI, paper, leaf in step (1), and size is 2 ×
2cm2。
In the above preparation method, in step (3), flexible substrates is placed in tannic acid solution and Iron(III) chloride hexahydrate is molten
In the mixed liquor of liquid, alkali is then added, prepares the sediment of tannic acid and iron (III) complex on the surface of flexible substrates；
Then it prepared by the dry surface in flexible substrates of the conductive substrates with the sediment of tannic acid and iron (III) complex
Organic matter film.
In the above preparation method, in step (4), the electrode material is aluminium, exists in the form of aluminium wire, passes through sand
Paper polishes to aluminium wire surface.
It is a kind of to be stored according to the tannic acid and iron ion (III) complex material of above method preparation and more substrate electricity
The preparation of device.
The invention also discloses according to the preparation method based on tannic acid and the electric storage material of iron (III) complex
The electric storage material based on tannic acid and iron (III) complex of preparation；According to based on tannic acid and iron (III) ligand compound
The electrical storage device based on tannic acid and iron (III) complex of the preparation method preparation of the electrical storage device of object.
Compared with prior art, have as follows a little using the present invention of above-mentioned technical proposal:
(1) present invention is prepared for a series of organic electrical storage device of sandwich types, makes by modifying ito glass substrate
Preparation Method is simple, easily operated.
(2) compared with traditional device, the cut-in voltage of organic electrical storage device in the present invention is low, and V twiceth1With
Vth2Fine differentiation is obtained.
(3) molecule that organic compound material electrical storage device of the invention uses is good biocompatibility, nontoxic
Free of contamination organic molecule, and can form a film in most of substrates, it solves organic electrical storage device and is not easy into flexible device
Film is difficult to the problem applied, and has widened application of organic electrical storage device in terms of flexibility significantly.
Detailed description of the invention
Fig. 1 is untreated ito glass contact angle figure；
Fig. 2 is the contact angle phenogram modified after solution processing；
Fig. 3 is x-ray photoelectron spectroscopy (XPS) spectrogram of tannic acid and iron (III) complex；
Fig. 4 is the EDS energy spectrum diagram of tannic acid and iron (III) complex；
Fig. 5 is the AFM comparison diagram and Thickness Variation curve graph (a) of tannic acid and iron (III) complex difference frequency of depositing
10；(b)15；(c)20；(d)25；(e)30；(f) thickness with frequency of depositing change curve；
Fig. 6 is that the binary system of tannic acid and iron (III) complex and ternary electricity store；
Fig. 7 is the cut-in voltage comparison diagram of tannic acid and iron (III) complex modification front and back；
Fig. 8 is the yield variation diagram of tannic acid and iron (III) complex modification front and back；
Fig. 9 is tannic acid and iron (III) complex flexible substrates yield figure.
Specific embodiment
Below in conjunction with drawings and concrete examples to further illustrate the technical scheme of the present invention.Unless otherwise indicated, under
Reagent used in column embodiment, material, instrument can be obtained by commercial means.
Embodiment one: the preparation of tannic acid and iron (III) complex electrical storage device
Device is roughly divided into three layers, is that aluminium electrode layer, tannic acid and iron (III) complex material layer (have respectively from top to bottom
Machine object film), ito glass decorative layer, specific preparation process is as follows:
1, ultrapure water, dehydrated alcohol, acetone and washes of absolute alcohol ito glass substrate are successively used in supersonic wave cleaning machine；
2, ito glass substrate is modified by modifying solution, forms decorative layer, wherein the hydroxyl with a thickness of single layer of decorative layer
Then the thickness of base molecule elutes its surface with ultrapure water, then glass surface is dried up at normal temperature with hair dryer, stay
To spare, the decorative layer of modification solution processing is formed at this time；The modification solution is 98% concentrated sulfuric acid and 30% peroxidating
Hydrogen is formulated；
3, organic matter tannic acid and Iron(III) chloride hexahydrate are deposited by solution-deposition method, passes through different frequency of depositing
Form the molecular layer that 5~30nm is not waited.Its sedimentary condition are as follows: first 20mL ultrapure water is poured into culture dish, then tannin
Acid solution (0.4mg/mL) and Iron(III) chloride hexahydrate (0.1mg/mL) pour into culture dish in equal volume, are placed in the ITO glass of modification
The sodium hydroxide solution of 1mol/L is added dropwise in glass at once, controls PH=8.0 of solution, completes primary sedimentation；Aforesaid operations are repeated, are increased
Add frequency of depositing, the surface of conductive substrates prepares the sediment of tannic acid and iron (III) complex；It is put into vacuum drying again
Dry in case, keeping temperature is 50 DEG C, 8 hours, is cooled to room temperature, and the surface of conductive substrates prepares tannic acid and iron (III) coordination
The organic matter film of compound, for the electric storage material based on tannic acid and iron (III) complex；
4, aluminium electrode is vaporized on organic film, until aluminium electrode reaches 80nm, obtains corresponding organic compound material
Electrical storage device.Evaporation condition is as follows: 5 × 10-4Under Pa vacuum condition, the rate of vapor deposition is 2A/s.
Using unmodified ITO substrate as control, the contact angle test of modification front and back is determined respectively, result is as schemed
1, shown in Fig. 2, it can be seen that ito glass is after modification solution modification, contact angle be increased, and illustrate to have succeeded
ITO substrate is modified.From Fig. 3 and Fig. 4 it is found that all elements are both present on device, this illustrates tannic acid and iron (III) coordination
Compound film has been successfully prepared.The film thickness and film thickness of different frequency of depositing are with the variation of frequency of depositing as shown in figure 5, from figure
In it is found that the thickness of increasing with frequency of depositing, tannic acid and iron (III) complex film gradually increases.Such as Fig. 6 institute
Show, test shows that tannic acid and iron (III) complex mainly show the storage behavior of ternary electricity.
Embodiment two: the preparation of tannic acid and iron (III) complex electricity storage material
Device is roughly divided into three layers, is that aluminium electrode layer, tannic acid and iron (III) complex material layer (have respectively from top to bottom
Machine object film) and gold electrode layer (including flexible substrates), specific preparation process it is as follows:
1, different substrate, PET, PI, paper and leaf are wiped with dehydrated alcohol respectively, then naturally dry；
2, magnetic control sputtering device is used to sputter one layer of gold nano layer in PET, PI, paper and leaf flexible substrates respectively as conducting surface,
Then the flexible substrates sputtered are put into culture dish by solution-deposition method respectively, first pour into 20mL ultrapure water in culture dish
In, then tannic acid solution (0.4mg/mL) and Iron(III) chloride hexahydrate (0.1mg/mL) are poured into culture dish in equal volume, it is fast
The sodium hydroxide solution of 1mol/L is added dropwise in speed, controls PH=8.0 of solution.Aforesaid operations are repeated, frequency of depositing, conductive base are increased
The surface at bottom prepares the sediment of tannic acid and iron (III) complex.Dry, holding temperature is put into vacuum oven again
For 50 DEG C, 8 hours, it is cooled to room temperature, the surface of conductive substrates prepares the organic matter film of tannic acid and iron (III) complex,
For the electric storage material based on tannic acid and iron (III) complex；
3, in the organic matter film by vapour deposition method aluminium-vapour deposition to above-mentioned flexible substrates, until AM aluminum metallization thickness reaches 80nm；It steams
Plating condition is as follows: 5 × 10-4Under Pa vacuum condition, the rate of vapor deposition is 2A/s.
Embodiment three: the ternary device yield of different base is counted
Device is placed in 4200-SCS semi-conductor test instrument, at room temperature, adjusts voltage tester device from -5V~5V
Impedance variations.
The yield and ternary cut-in voltage for counting tannic acid and iron (III) complex device, such as Fig. 7 and Fig. 8 institute
Show, after being modified by decorative layer, since the surface of tannic acid and iron (III) complex film is more smooth, after modification
Cut-in voltage can be clearly separated, and device (embodiment one) yield improves a lot；Independent tannic acid can not form a film, and not deposit
Store up effect；According to the method for embodiment one, when tannic acid solution is 0.6mg/mL, when organic matter film thickness 20nm, device
Yield is 0.23, when tannic acid solution is 0.2mg/mL, when organic matter film thickness 20nm, and device yield 0.19.
The yield for counting tannic acid and iron (III) complex flexible device (embodiment two), as shown in figure 9, from figure
Know that tannic acid and iron (III) complex are suitable for the preparation of flexible device.
In conclusion being prepared for a series of sandwiches the present invention is based on tannic acid and iron (III) complex and organising
The electrical storage device for closing object material, obtain it is considerable have ternary device yield, solve that current ternary yield is lower to ask
Topic.In flexible device using upper, the present invention passes through the test to different flexible substrates, tannic acid and iron (III) ligand compound
Object molecule above shows very big application prospect in the application of flexible substrates.For the following flexible electrical field of storage, this hair
The bright flexible electrical storage device based on tannic acid and iron (III) organic compound material exists in following flexible electrical storage device
Potential application value.
Claims (10)
1. the sediment of tannic acid and iron (III) complex is preparing the application in electric storage material or electrical storage device.
2. application according to claim 1, which is characterized in that mix tannic acid solution with Iron(III) chloride hexahydrate solution
Afterwards, alkali is added and obtains the sediment of tannic acid and iron (III) complex；Then by tannic acid and iron (III) complex
Sediment organic matter film is made, obtain electric storage material.
3. application according to claim 1, which is characterized in that conductive substrates are placed in tannic acid solution and six hydration trichlorines
In the mixed liquor for changing ferrous solution, alkali is then added, prepares tannic acid and iron (III) complex on the surface of conductive substrates
Sediment；It then will the dry table in conductive substrates of the conductive substrates with the sediment of tannic acid and iron (III) complex
Wheat flour is for organic matter film；Electrode finally is prepared on organic matter film surface, obtains electrical storage device.
4. according to application described in claim 2 or 3, which is characterized in that organic matter film with a thickness of 5~30nm；Tannic acid,
The mass ratio of Iron(III) chloride hexahydrate is 4: 1；The concentration of tannic acid solution be 0.4mg/mL, Iron(III) chloride hexahydrate solution it is dense
Degree is 0.1mg/mL；Alkali is sodium hydroxide.
It, will 5. the preparation method of electric storage material of the one kind based on tannic acid and iron (III) complex, includes the following steps
After tannic acid solution is mixed with Iron(III) chloride hexahydrate solution, alkali is added and obtains the precipitating of tannic acid and iron (III) complex
Object；Then organic matter film is made in the sediment of tannic acid and iron (III) complex, obtained based on tannic acid and iron (III)
The electric storage material of complex.
It, will 6. the preparation method of electrical storage device of the one kind based on tannic acid and iron (III) complex, includes the following steps
Conductive substrates are placed in the mixed liquor of tannic acid solution and Iron(III) chloride hexahydrate solution, alkali are then added, in conductive substrates
Surface prepares the sediment of tannic acid and iron (III) complex；It then will be with tannic acid and iron (III) complex
The dry surface in conductive substrates of the conductive substrates of sediment prepares organic matter film；Electrode finally is prepared on organic matter film surface,
Obtain the electrical storage device based on tannic acid and iron (III) complex.
7. according to preparation method described in claim 5 or 6, which is characterized in that organic matter film with a thickness of 5~30nm；It is single
Peaceful sour, Iron(III) chloride hexahydrate mass ratio is 4: 1；The concentration of tannic acid solution is 0.4mg/mL, and Iron(III) chloride hexahydrate is molten
The concentration of liquid is 0.1mg/mL；Alkali is sodium hydroxide.
8. preparation method according to claim 6, which is characterized in that conductive substrates include ito glass, gold-plated flexible base
Bottom.
9. the electricity storage material based on tannic acid and iron (III) complex of preparation method preparation according to claim 5
Material.
10. the electric storage material based on tannic acid and iron (III) complex described in claim 9 is based on tannic acid in preparation
With the application in the electrical storage device of iron (III) complex.
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| CN114409916A (en) * | 2022-01-25 | 2022-04-29 | 汕头大学 | Nano tannin and preparation method and application thereof |
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