CN105908159B - A kind of g-C3N4The preparation method of/FTO compound transparent electricity conductive films - Google Patents

A kind of g-C3N4The preparation method of/FTO compound transparent electricity conductive films Download PDF

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CN105908159B
CN105908159B CN201610240304.4A CN201610240304A CN105908159B CN 105908159 B CN105908159 B CN 105908159B CN 201610240304 A CN201610240304 A CN 201610240304A CN 105908159 B CN105908159 B CN 105908159B
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李保家
祖伟
黄立静
曹海迪
任乃飞
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Jiangsu University
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C20/06—Coating with inorganic material, other than metallic material
    • C23C20/08—Coating with inorganic material, other than metallic material with compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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Abstract

The present invention relates to transparent conductive film material field, refers in particular to one kind using fluorine-doped tin dioxide (FTO) film as substrate, the self-assembling technique mutually adsorbed using positive and negative electrolyte ion realizes g C3N4Method prepared by/FTO compound transparent electricity conductive films, by varying solution in experimentation pH value can be prepared by flexible modulation laminated film photoelectric properties.

Description

A kind of g-C3N4The preparation method of/FTO compound transparent electricity conductive films
Technical field
The present invention relates to transparent conductive film material field, refers in particular to one kind using fluorine-doped tin dioxide (FTO) film as substrate, The self-assembling technique mutually adsorbed using positive and negative electrolyte ion realizes g-C3N4Side prepared by/FTO compound transparent electricity conductive films Method, by varying solution in experimentation pH value can be prepared by flexible modulation laminated film photoelectric properties.
Background technology
Because rare element indium is constrained be subject to low storage capacity and high price, FTO films gradually substitute tin-doped indium oxide (ITO) transparent conductive film, is widely used in the fields such as electronic liquid crystal display screen, photocatalysis, thin-film solar cells, its market needs Ask very big, it is studied attention for also giving height by scientific circles.FTO films have good suede structure, and production cost is low, But there is also the shortcomings of square resistance is big, light transmittance is relatively low.And carbon nitride films have as a kind of novel semiconductor material Highly thermally conductive, high atoms density, larger energy gap and excellent photoelectric properties, the defects of can exactly making up FTO films. Therefore prepared by research and development carbonitride/FTO compound transparent electricity conductive films and the new method of performance regulation and control is of great significance.
With deepening continuously for scientific research, some traditional coating techniques are continuously improving perfect, new film preparation Method also emerges in an endless stream.In the prior art, preparing the common method of carbon nitride films has electrochemical deposition method, vapour deposition Method, high temperature and high pressure method, magnetron sputtering method, pulsed laser deposition, ion beam deposition etc..Wang (king's grace brother) etc. is relatively early to be adopted Hot filament CVD is aided in be born on the basis of radio frequency and heated filament double action to Si substrates plus certain with biasing Bias, increases the density and energy of the electronics, especially Nitrogen ion of plasma, the chemism of intensified response group, is being protected Hold and be settled out carbon nitride films (referring to document in the Si substrates of certain temperature:E.G.Wang,Y.Chen,L.P Guo,and F.Chen.Science in China A 27(1998)49–53)；Peponas etc. utilizes rf magnetron sputtering system, with stone Ink is target, with Ar/N2Mixed gas is sputter gas, and Carbon Nitride Crystal film is successfully prepared in Si substrates (referring to text Offer:S.Peponas,M.Lejeune,S. Charvet,M.Guedda,and M.Benlahsen.Surface and Coatings Technology 212 (2012) 229-233), they, which are investigated, changes carbonitride of the deposition pressure to preparation The influence of organic thin-films and photoelectric properties, reference value is provided for follow-up study.But there are a system due to these methods The problem of row, if any the vacuum condition to experimental facilities have very high requirement, and need the target of high quality, manufacturing cost It is excessive；Some need, which adds some, not environmentally or to human body the additive of injury；Some preparation process are complicated, and The effective area and efficiency for preparing film are limited to a certain extent.Thus, it is proposed that a kind of g- compound in FTO substrates C3N4The straightforward procedure of/FTO films, the defects of effectively to overcome above-mentioned technology, it is final obtain photoelectric properties can flexible modulation g- C3N4/ FTO compound transparent electricity conductive films.
The content of the invention
The object of the present invention is to provide a kind of large area to prepare g-C3N4The method of/FTO compound transparent electricity conductive films, the party Method can obtain the g-C with different photoelectric properties by the control to solution ph used3N4/ FTO laminated films, operation letter It is single, it is energy saving, it is low without particular/special requirement, cost to equipment.
A kind of g-C3N4The preparation method of/FTO compound transparent electricity conductive films, it is characterised in that：By hydroxylated FTO films It is put into after being soaked in the ethanol solution of silane coupling agent and takes out, cleans, dries up, place into NaHSO4Immersion is so that FTO in solution Film sample surface produces positively charged amide proton, passes through the NaHSO to soaking FTO film samples4The control of solution ph System, realizes the regulation and control to compound film optoelectronic performance；G-C is immersed again3N4It is cloudy because of electrostatic force in anion electrolyte solution Ionic electrolytes absorption makes its negatively charged in positively charged substrate surface, then immerses the negatively charged substrate in surface again (C8H16NCl)nIn cationic polymer electrolyte solution, make its positively charged, FTO thin-film self-assemblings is adsorbed g-C3N4Layer, as needed Self assembly number of cycles operation, finally obtain g-C3N4/ FTO compound transparent electricity conductive films.
Further, concrete technical scheme of the present invention is as follows：
A kind of g-C3N4/ FTO compound transparent electricity conductive films prepare and the method for performance regulation and control, it is comprised the concrete steps that：
Step 1, will clean up and protect the FTO film samples in FTO film glasses face and be put into the ethanol solution of NaOH Middle ultrasonic cleaning, after rinsing well, immerses NH by FTO film samples3·H2O/H2O2/H2Heating water bath in the mixed solution of O, takes Go out the cleaning of FTO film samples, drying.
FTO film samples, be put into the ethanol solution of silane coupling agent after immersion and take out by step 2, cleans, dries up, then It is put into NaHSO4Immersion in solution is so that FTO film samples surface produces positively charged amide proton, by NaHSO4It is molten The control of liquid pH value, realizes the regulation and control to compound film optoelectronic performance.
Step 3, by surface amino groups protonate FTO film samples be put into g-C3N4Soaked in solution, rinse, blow after taking-up It is dry.
Step 4, step 3 is handled after FTO film samples be put into (C8H16NCl)nSoaked in solution, rinsed after taking-up, Drying.
Step 5, be repeated in operating procedure 3 and step 4, and number is 2~8 times, obtains g-C3N4/ FTO laminated films.
Further, it is described that FTO film samples are cleaned up into finger in step 1：First FTO film samples are being gone successively Respectively it is cleaned by ultrasonic 10min under ionized water, acetone, ethanol solution, then uses N2Drying, places into the drying that temperature is 45 DEG C 2h is dried in case, it is stand-by.
Further, in step 1, protect FTO film glasses face and refer to：FTO film samples are protected with resistance to acid and alkali adhesive tape Glass surface, prevent solution from adhering to the surface thereof.
Further, in step 1, the ethanol solution concentration of NaOH is 1mol/L, water and absolute ethyl alcohol volume ratio in solvent For 1:1, the ultrasonic cleaning time is 15min；Finger is rinsed well to be rinsed well with deionized water.
Further, in step 1, in the mixed solution, NH3·H2O、H2O2And H2The volume ratio of O is (1~3):1: 6, NH3·H2The mass percentage concentration of O is 28%, H2O2Mass percentage concentration be 30%；The temperature of the heating water bath is 50 DEG C, time 25min；Cleaning, which refers to be put into deionized water, to be cleaned by ultrasonic 3 times, and each time is 10min, and drying, which refers to, uses N2Blow It is dry.
Further, in step 2, in the ethanol solution of silane coupling agent, the volume of A-1130 silane coupling agents and ethanol Than for 1:9, soaking time 2h；Cleaning refers to is cleaned with acetone, and drying refers to and uses N2Drying.
Further, in step 2, NaHSO4The adjustable range of solution ph is 2~6, the NaHSO of configuration4Solution ph G-C that is bigger, obtaining3N4The light transmittance and square resistance of/FTO laminated films are bigger；Soaking time is 10 min.
Further, in step 3, g-C3N4The concentration of solution is 0.05~0.15mg/mL, soaking time 30min, is rushed Finger deionized water rinsing is washed, drying, which refers to, uses N2Drying.
Further, in step 4, (C8H16NCl)nThe mass percentage concentration of solution is 4%~15%, and soaking time is 30min, flushing refer to deionized water rinsing, and drying, which refers to, uses N2Drying.
Further, in step 5, operating procedure 3 and step 4 are repeated in, number is 4 times, obtains g-C3N4/ FTO is multiple Close film.
The present invention basic principle be：First by FTO film surface protonated aminos, make its positively charged, then immerse g- C3N4In anion electrolyte solution, because of electrostatic force, anion electrolyte absorption makes its band in positively charged substrate surface Negative electricity, then immerses (C again by the negatively charged substrate in surface8H16NCl)nIn cationic polymer electrolyte solution, make its positively charged, G-C is immersed again3N4In anion electrolyte solution, such circulate operation.G-C in solution3N4Molecule is spontaneously organized and gathered A stabilization, well-regulated composite membrane are integrated into, by NaHSO4The adjusting of solution ph, the light of controllable laminated film Electrical property.
Compared with prior art, the beneficial effects of the invention are as follows：
1) can in batch, large area prepare, cost is low.
2) g-C obtained3N4Adhesive force is stronger between each layer of/FTO laminated films, greatly improves thin film stability.
3) in whole process all it is the spontaneous progress under conditions of temperature requirement is not high, directly utilizes FTO film substrates New laminated film is prepared, easy to operate, reaction condition is gentle, and energy consumption is low, the equipment without special expensive.
4) find in an experiment, during FTO film samples surface amino groups protonate, the NaHSO of configuration4Solution ph G-C that is bigger, obtaining3N4The light transmittance and square resistance of/FTO laminated films are bigger；Therefore, the present invention can simply lead to Cross to NaHSO4The control of solution ph, realizes the regulation and control to compound film optoelectronic performance, so as to adapt to different application occasion It is required that.
Brief description of the drawings
Fig. 1 g-C3N4/ FTO compound transparent electricity conductive film preparation process schematic diagrames.
1FTO film samples, 2g-C3N4Solution, 3 glass containers, 4 (C8H16NCl)nSolution.
Fig. 2 g-C3N4The Zeta potential measurement figure of solution.
The g-C being prepared in Fig. 3 embodiments 13N4The SEM figures (a) and transmitted spectrum of/FTO compound transparent electricity conductive films (b)。
The g-C being prepared in Fig. 4 embodiments 23N4The SEM figures (a) and transmitted spectrum of/FTO compound transparent electricity conductive films (b)。
The g-C being prepared in Fig. 5 embodiments 33N4The SEM figures (a) and transmitted spectrum of/FTO compound transparent electricity conductive films (b)。
Embodiment
Fig. 1 is g-C3N4/ FTO compound transparent electricity conductive film preparation process schematic diagrames.FTO film samples 1 are located in advance by surface It is sequentially placed into after reason and surface amino groups protonation equipped with g-C3N4Solution 2 and (C8H16NCl)nIn the glass container 3 of solution 4, Its self assembly is set to adsorb g-C3N4Layer, the such circulate operation of self assembly number as needed, finally obtains g-C3N4/ FTO is compound Transparent conductive film, is washed with deionized water only after taking out sample every time, and uses N2Drying.
Fig. 2 is g-C3N4The Zeta potential measurement result of solution.It can be seen that g-C3N4The current potential of solution is -3.41 mV, Aobvious electronegativity, shows that it can directly be adsorbed in positively charged substrate surface.
The invention will now be described in further detail with reference to the accompanying drawings.
Embodiment 1：FTO film samples after cleaning up are put into the ethanol solution (body for the NaOH that concentration is 1mol/L Product is than being 1:1) it is cleaned by ultrasonic 15min, after deionized water rinsing is clean, it is 3 that FTO film samples are immersed volume ratio:1:6 NH3·H2O (28%)/H2O2(30%)/H2In the mixed solution of O, into the heating water bath that trip temperature is 50 DEG C, time 25min. Take out FTO film samples and be put into deionized water and be cleaned by ultrasonic 3 times, each time is 10min, then uses N2Drying.Then, will FTO film samples are put into volume ratio as 1:2h is soaked in the ethanol solution of 9 A-1130 silane coupling agents, after taking out sample, is used Acetone is cleaned, and uses N2Drying, then it is respectively put into the different NaHSO of pH value410min is soaked in solution.Finally, by surface The FTO film samples of protonated amino are sequentially placed into the g-C that concentration is 0.10mg/mL3N4Solution and mass fraction are 8% (C8H16NCl)nIn solution, 30min is soaked respectively, and repeats this operating process, and number is 4 times.
Fig. 3 (a) is the NaHSO using pH=44The g-C being prepared during solution3N4/ FTO compound transparent electricity conductive film tables Face SEM schemes, it can be seen that the g-C obtained on this condition3N4Layer is comparatively dense and uniform；Tested by Fig. 3 (b) and square resistance As a result understand, g-C3N4The light transmittance and square resistance of/FTO compound transparent electricity conductive films are with NaHSO4The increasing of solution ph Add and increase, work as NaHSO4When solution ph is respectively 2,4,6, g-C3N4The visible region average transmittance of/FTO laminated films (400~800nm) is respectively 71.54%, 72.35%, 73.03%, square resistance be respectively 7.32 Ω/sq, 8.48 Ω/sq, 9.66 Ω/sq, illustrate NaHSO4The pH value of solution is to g-C3N4There are the photoelectric properties of/FTO laminated films certain regulation and control to make With.
Embodiment 2：FTO film samples after cleaning up are put into the ethanol solution (body for the NaOH that concentration is 1mol/L Product is than being 1:1) it is cleaned by ultrasonic 15min, after deionized water rinsing is clean, it is 2 that FTO film samples are immersed volume ratio:1:6 NH3·H2O (28%)/H2O2(30%)/H2In the mixed solution of O, into the heating water bath that trip temperature is 50 DEG C, time 25min. Take out FTO film samples and be put into deionized water and be cleaned by ultrasonic 3 times, each time is 10min, then uses N2Drying.Then, will FTO film samples are put into volume ratio as 1:2h is soaked in the ethanol solution of 9 A-1130 silane coupling agents, after taking out sample, is used Acetone is cleaned, and uses N2Drying, places into the NaHSO of pH=2410min is soaked in solution.Finally, by surface amino groups matter The FTO film samples of sonization are sequentially placed into the g-C that concentration is 0.15mg/mL3N4Solution and mass fraction are 15% (C8H16NCl)nIn solution, 30 min are soaked respectively, and repeat this operating process, and number is 8 times.
Fig. 4 (a) is the g-C being prepared3N4/ FTO compound transparent electricity conductive films surface SEM schemes, it can be seen that in this condition Under obtained g-C3N4Layer is thicker, and uniformity is poor, and has local agglomeration.From Fig. 4 (b), wavelength for 400~ In the visible-range of 800nm, g-C3N4The average transmittance of/FTO laminated films is 71.11%.Test obtains laminated film Square resistance is 7.16 Ω/sq.
Embodiment 3：FTO film samples after cleaning up are put into the ethanol solution (body for the NaOH that concentration is 1mol/L Product is than being 1:1) it is cleaned by ultrasonic 15min, after deionized water rinsing is clean, it is 1 that FTO film samples are immersed volume ratio:1:6 NH3·H2O (28%)/H2O2(30%)/H2In the mixed solution of O, into the heating water bath that trip temperature is 50 DEG C, time 25min. Take out FTO film samples and be put into deionized water and be cleaned by ultrasonic 3 times, each time is 10min, then uses N2Drying.Then, will FTO film samples are put into volume ratio as 1:2h is soaked in the ethanol solution of 9 A-1130 silane coupling agents, after taking out sample, is used Acetone is cleaned, and uses N2Drying, places into the NaHSO of pH=6410min is soaked in solution.Finally, by surface amino groups matter The FTO film samples of sonization are sequentially placed into the g-C that concentration is 0.05mg/mL3N4Solution and mass fraction are 4% (C8H16NCl)nIn solution, 30 min are soaked respectively, and repeat this operating process, and number is 2 times.
Fig. 5 (a) is the g-C being prepared3N4/ FTO compound transparent electricity conductive films surface SEM schemes, it can be seen that in this condition Under obtained g-C3N4Layer distribution is more sparse.From Fig. 5 (b), in the visible-range that wavelength is 400~800nm, g- C3N4The average transmittance of/FTO laminated films is 72.86%.The square resistance that test obtains laminated film is 9.18 Ω/sq.
Above-described embodiment given by the present invention is only specifically described technical solution, and is not limited.In ability After the technical staff in domain has read the above, all it will be apparent for a variety of modifications and substitutions of the present invention.Therefore, Protection scope of the present invention should be limited to the appended claims.

Claims (9)

  1. A kind of 1. g-C3N4The preparation method of/FTO compound transparent electricity conductive films, it is characterised in that：By hydroxylated FTO films sample Product immerse NH3·H2O、H2O2And H2Heating water bath in the mixed solution of O, takes out and cleans, dries up, then by FTO film samples It is put into after being soaked in the ethanol solution of silane coupling agent and takes out, cleans, dries up, place into NaHSO4Immersion is so that FTO in solution Film sample surface produces positively charged amide proton, passes through the NaHSO to soaking FTO film samples4The control of solution ph System, realizes the regulation and control to compound film optoelectronic performance；G-C is immersed again3N4It is cloudy because of electrostatic force in anion electrolyte solution Ionic electrolytes absorption makes its negatively charged in positively charged substrate surface, then immerses the negatively charged substrate in surface again (C8H16NCl)nIn cationic polymer electrolyte solution, make its positively charged, FTO thin-film self-assemblings is adsorbed g-C3N4Layer, as needed Self assembly number of cycles operation, finally obtain g-C3N4/ FTO compound transparent electricity conductive films.
  2. A kind of 2. g-C as claimed in claim 13N4The preparation method of/FTO compound transparent electricity conductive films, it is characterised in that according to Following steps carry out：
    Step 1, by clean up and protect FTO film glasses face FTO film samples be put into the ethanol solution of NaOH surpass Sound cleans, and after rinsing well, FTO film samples are immersed NH3·H2O、H2O2And H2Heating water bath in the mixed solution of O, takes out The cleaning of FTO film samples, drying；
    FTO film samples, be put into the ethanol solution of silane coupling agent after immersion and take out by step 2, cleans, dries up, places into NaHSO4Immersion in solution is so that FTO film samples surface produces positively charged amide proton, by NaHSO4Solution ph Control, realize the regulation and control to compound film optoelectronic performance；
    Step 3, by surface amino groups protonate FTO film samples be put into g-C3N4Soaked in solution, rinse, dry up after taking-up；
    Step 4, step 3 is handled after FTO film samples be put into (C8H16NCl)nSoaked in solution, rinse, dry up after taking-up；
    Step 5, be repeated in operating procedure 3 and step 4, and number is 2~8 times, obtains g-C3N4/ FTO laminated films.
  3. A kind of 3. g-C as claimed in claim 23N4The preparation method of/FTO compound transparent electricity conductive films, it is characterised in that：Step It is described that FTO film samples are cleaned up into finger in rapid 1：First by FTO film samples successively in deionized water, acetone, absolute ethyl alcohol Respectively it is cleaned by ultrasonic 10min under solution, then uses N2Drying, places into the drying box that temperature is 45 DEG C and dries 2h, stand-by；Step In 1, protect FTO film glasses face and refer to：With the glass surface of resistance to acid and alkali adhesive tape protection FTO film samples, prevent solution from sticking On its surface；In step 1, the ethanol solution concentration of NaOH is 1mol/L, and water and absolute ethyl alcohol volume ratio are 1 in solvent:1, surpass Sound scavenging period is 15min；Finger is rinsed well to be rinsed well with deionized water.
  4. A kind of 4. g-C as claimed in claim 23N4The preparation method of/FTO compound transparent electricity conductive films, it is characterised in that：Step In rapid 1, in the mixed solution, NH3·H2O、H2O2And H2The volume ratio of O is (1~3):1:6, NH3·H2The quality percentage of O Concentration is 28%, H2O2Mass percentage concentration be 30%；The temperature of the heating water bath is 50 DEG C, time 25min；Cleaning Finger, which is put into deionized water, to be cleaned by ultrasonic 3 times, and each time is 10min, and drying, which refers to, uses N2Drying.
  5. A kind of 5. g-C as claimed in claim 23N4The preparation method of/FTO compound transparent electricity conductive films, it is characterised in that：Step In rapid 2, in the ethanol solution of silane coupling agent, the volume ratio of A-1130 silane coupling agents and ethanol is 1:9, soaking time is 2h；Cleaning refers to is cleaned with acetone, and drying, which refers to, uses N2Drying.
  6. A kind of 6. g-C as claimed in claim 23N4The preparation method of/FTO compound transparent electricity conductive films, it is characterised in that：Step In rapid 2, NaHSO4The adjustable range of solution ph is 2~6, the NaHSO of preparation4Solution ph is bigger, obtained g-C3N4/FTO The light transmittance and square resistance of laminated film are bigger；Soaking time is 10min.
  7. A kind of 7. g-C as claimed in claim 23N4The preparation method of/FTO compound transparent electricity conductive films, it is characterised in that：Step In rapid 3, g-C3N4The concentration of solution is 0.05~0.15mg/mL, soaking time 30min, and flushing refers to deionized water rinsing, Drying, which refers to, uses N2Drying.
  8. A kind of 8. g-C as claimed in claim 23N4The preparation method of/FTO compound transparent electricity conductive films, it is characterised in that：Step In rapid 4, (C8H16NCl)nThe mass percentage concentration of solution is 4%~15%, soaking time 30min, and flushing, which refers to, uses deionization Water rinses, and drying, which refers to, uses N2Drying.
  9. A kind of 9. g-C as claimed in claim 23N4The preparation method of/FTO compound transparent electricity conductive films, it is characterised in that：Step In rapid 5, operating procedure 3 and step 4 are repeated in, number is 4 times, obtains g-C3N4/ FTO laminated films.
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CN106848494B (en) * 2017-02-21 2019-06-28 陕西师范大学 A kind of simple preparation method of carbon auto-dope nano carbon nitride film electrode
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