CN113621270A - Preparation method and application of nickel oxide nanocrystalline electrochromic ink - Google Patents
Preparation method and application of nickel oxide nanocrystalline electrochromic ink Download PDFInfo
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- CN113621270A CN113621270A CN202110994621.6A CN202110994621A CN113621270A CN 113621270 A CN113621270 A CN 113621270A CN 202110994621 A CN202110994621 A CN 202110994621A CN 113621270 A CN113621270 A CN 113621270A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/50—Sympathetic, colour changing or similar inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
- C09K9/02—Organic tenebrescent materials
Abstract
The invention discloses a preparation method and application of nickel oxide nanocrystalline electrochromic ink, wherein the method comprises the following steps: (1) mixing and heating the precursor, the solvent and the protective agent to a certain temperature under argon-oxygen mixed gas, and keeping the temperature for a period of time; (2) heating the reaction substance to a reaction temperature and preserving the temperature for a period of time to obtain a nickel oxide nanocrystal solution; (3) purifying the nickel oxide nanocrystalline solution obtained in the step (3); (4) and (4) carrying out ligand exchange on the nickel oxide nanocrystal obtained in the step (3) and dissolving the nickel oxide nanocrystal in a polar solvent to obtain the nickel oxide nanocrystal ink. The invention does not need a complex reaction system, and the nickel oxide nanocrystalline after ligand exchange can be dispersed in various polar solvents without adding extra additives, and is suitable for various film preparation processes such as ink-jet printing, spin coating, spraying method and the like.
Description
Technical Field
The invention relates to the field of electrochromic materials, in particular to a preparation method and application of nickel oxide nanocrystalline electrochromic ink.
Background
Electrochromism refers to a phenomenon that the optical properties of a material, such as reflectivity, transmittance and absorptivity, change in color stably and reversibly under the action of an applied electric field, and is visually represented as reversible changes in coloration and fading. Since the discovery of electrochromic materials, extensive research into electrochromic materials has been initiated due to their low power consumption, high coloring efficiency, and stable memory effect under open circuit conditions. The reflective mirror is widely applied to the fields of energy-saving glass, large-area displays, automobile skylights, military camouflage windows, intelligent reflectors and the like. Therefore, it is very promising to select electrochromic devices with long-term cycling stability, high coloring efficiency, large light modulation and short switching time at very low dc voltage for practical application.
The current preparation methods of electrochromic films include magnetron sputtering, solvothermal methods, chemical bath deposition, sol-gel methods, spray coating, ink-jet printing and the like. Among them, ink jet printing has received a great deal of attention as a novel process for preparing a thin film, and a process for preparing a conductive ink is an important part of the process for preparing a thin film. The main components of the conductive ink comprise a conductive substance, a solvent and various auxiliaries, wherein the auxiliaries comprise a dispersing agent, a binder, a defoaming agent and the like. The conductive ink has better fluid properties and film-forming properties due to the addition of the auxiliary agent, but the composition of the conductive ink becomes complicated. Most of the additives need to be removed at higher temperatures, which not only affects the performance of the conductive ink but also limits the development of flexible devices.
Disclosure of Invention
The invention aims to provide a preparation method and application of nickel oxide nanocrystal electrochromic ink, which realize the transfer of nickel oxide nanocrystals from a nonpolar solvent to a polar solvent under the action of a ligand exchanger, are suitable for various polar solvents, and have the advantages of simple and convenient operation, low manufacturing cost, small size and good monodispersity.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of nickel oxide nanocrystalline electrochromic ink comprises the following steps:
(1) mixing and heating nickel salt, a solvent and a protective agent to 50-150 ℃ under argon-oxygen mixed gas, and preserving heat for 10-45 minutes; preferably, the heating temperature is 80-100 ℃, and the heat preservation time is 25-35 minutes. Introducing argon-oxygen mixed gas into the atmosphere in the reaction system according to a certain proportion and continuing until the reaction is finished, so that reactants can fully react in the atmosphere, stirring is kept in the reaction process, and the control of nickel oxygen atoms of the nickel oxide nanocrystal can be realized in the oxygen-containing environment, so that the conductivity of the nickel oxide nanocrystal is improved;
(2) heating the substance obtained in the step (1) to a reaction temperature and preserving heat for a period of time to obtain a nickel oxide nanocrystal solution;
(3) purifying the nickel oxide nanocrystal solution to obtain nickel oxide nanocrystals, wherein the reaction mechanism is that nickel acetylacetonate and oleylamine carry out aminolysis reaction, and the chemical ratio of nickel oxide is adjusted by introducing flowing argon-oxygen mixed gas to participate in the reaction so as to improve the conductivity of nickel oxide;
(4) and dissolving the nickel oxide nanocrystal in n-hexane, then carrying out ligand exchange, and dissolving in a polar solvent to obtain the nickel oxide nanocrystal electrochromic ink.
Preferably, in the step (1), the solvent is oleylamine, the nickel salt is one of nickel stearate, nickel acetate and nickel acetylacetonate, and the protective agent is lithium stearate, so that excessive reduction of the nickel salt in the step (2) can be effectively prevented.
Preferably, the molar ratio of the nickel acetylacetonate to the lithium stearate is 2.5-3.6: 1, the amount of oleylamine is 10-15 ml.
Preferably, in the step (1), the flow ratio of argon to oxygen is 4: 1-1: 4, the flow of oxygen is 5-10 sccm, the flow of argon is 25-30 sccm, and a certain amount of oxygen atoms are ensured to be injected into the nickel oxide nanocrystals.
Preferably, in the step (2), the heating temperature of the substance is 150-300 ℃, the heat preservation time is 0.5-1.5 h, and further, the heating temperature is 200-250 ℃.
Preferably, the purification process in step (3) is as follows: and precipitating the nickel oxide nanocrystal solution with excessive ethanol, centrifuging, dissolving in n-hexane, adding hot methanol to obtain an upper layer solution, adding acetone to precipitate, and centrifuging to obtain the nickel oxide nanocrystal.
Preferably, the hot methanol is repeatedly washed for 4 times, so that the deep washing of the nickel oxide nanocrystals can be ensured.
Preferably, the ligand exchange process in the step (4) is specifically as follows: adding a ligand exchanger into acetonitrile, uniformly mixing, then adding a nickel oxide nanocrystal n-hexane solution, stirring, taking a lower layer solution, adding toluene, precipitating and centrifuging to obtain a nickel oxide nanocrystal after ligand exchange, and adding a polar solvent to obtain the nickel oxide nanocrystal electrochromic ink.
Preferably, the ligand exchanger is a Meerwein salt, including trimethyloxonium tetrafluoroborate (Me)3OBF4) Or triethyloxonium tetrafluoroborate (Et)3OBF4) And the polar solvent is one of DMF and NMP.
The nickel oxide nanocrystalline electrochromic ink prepared by the preparation method can be used for preparing a nickel oxide nanocrystalline electrochromic film.
The preparation method of the nickel oxide nanocrystalline electrochromic film comprises the following steps: ultrasonically cleaning the FTO glass by acetone, absolute ethyl alcohol and deionized water for 20 minutes respectively, and carrying out ozone treatment for 30 minutes after drying; the prepared nickel oxide nanocrystalline electrochromic ink is coated on FTO glass in a spin coating mode to form a film, then annealing and ozone treatment are carried out, and the prepared nickel oxide nanocrystalline film is prepared and has good electrochromic performance.
Preferably, the concentration of the nickel oxide nanocrystalline electrochromic ink subjected to spin coating is 25-100 mg/ml, the spin coating times are 4-8 times, the annealing temperature is 100-300 ℃, and the ozone treatment is carried out for 20-60 minutes.
Compared with the prior art, the invention has the beneficial effects that:
1) the nickel oxide nanocrystal prepared by the method has the characteristics of small and uniform size, good dispersibility and the like, and can be dispersed in various polar solvents after ligand exchange;
2) the chemical ratio of the nickel oxide is adjusted by introducing flowing argon-oxygen mixed gas to participate in the reaction, so that the conductivity of the nickel oxide, the response speed of the nickel oxide film and the coloring efficiency are improved;
3) the nickel oxide nanocrystalline electrochromic ink prepared by the invention has good dispersibility and stability, can be placed for several months to keep stable, and can form stable ink drops in ink-jet printing equipment. And is suitable for preparing films on various substrates by a spin coating method and a spraying method;
4) the nickel oxide nanocrystalline prepared by the method is only dispersed in a single solvent, and other additives are not used, so that the nickel oxide nanocrystalline ink still has good fluid property and film-forming property even if other additives are not used;
5) the transmittance of the nickel oxide in a fading state seriously influences the performance of an electrochromic device, the nickel oxide nanocrystalline film prepared by the invention has very high transmittance (up to 98%) in the fading state, can realize rapid reversible transformation of black, brown and transparent under different voltages, has good cycle stability, and can be applied to environment-friendly and energy-saving materials such as electrochromic intelligent windows and the like.
Drawings
FIG. 1 is an X-ray diffraction pattern of nickel oxide nanocrystals prepared in example 1;
FIG. 2 is an X-ray diffraction pattern of the nickel oxide nanocrystal prepared in example 2;
FIG. 3 is a transmission electron micrograph of nickel oxide nanocrystals prepared in example 2;
FIG. 4 is a scanning electron micrograph of the nickel oxide nanocrystalline thin film prepared in example 2;
FIG. 5 is a graph of electrochromic kinetics of the nickel oxide nanocrystalline thin film prepared in example 2 (550nm, -0.4v-1.1 v);
FIG. 6 is a graph of electrochromic spectral properties of the nickel oxide nanocrystalline thin film prepared in example 2;
fig. 7 is an ink drop perspective view of the nickel oxide nanocrystalline electrochromic ink prepared in example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of nickel oxide nanocrystalline electrochromic ink comprises the following specific steps:
(1) 6.5mmol of nickel acetylacetonate, 15ml of oleylamine and 1.8mmol of lithium stearate were placed in a three-necked flask, and a mixed gas of argon and oxygen was introduced at a flow ratio of 4:1 for 10 minutes, followed by heating to 100 ℃ and heat preservation for 30 minutes.
(2) The reaction was heated to 210 ℃ and incubated for 60 minutes.
(3) After cooling to room temperature, ethanol was added for precipitation, and after centrifugation, the precipitate was dissolved in n-hexane.
(4) Adding a certain amount of hot methanol of 50 deg.C, collecting the upper layer solution, and repeating for 4 times.
(5) Adding acetone for precipitation, centrifuging to obtain nickel oxide nanocrystal, and dissolving the nickel oxide nanocrystal in n-hexane according to the concentration of 10 mg/ml.
(6) 2ml of triethyloxonium tetrafluoroborate was dissolved in 30ml of acetonitrile, and a nickel oxide nanocrystalline n-hexane solution was added thereto and stirred for 12 hours, and toluene was added to the lower layer solution to precipitate. And after centrifugation, dissolving the precipitate in N-methyl pyrrolidone according to 100mg/ml to obtain the nickel oxide nanocrystalline electrochromic ink.
A preparation method of a nickel oxide nanocrystalline electrochromic film comprises the following steps:
(1) ultrasonically cleaning the FTO glass by acetone, absolute ethyl alcohol and deionized water for 20 minutes respectively, and carrying out ozone treatment for 30 minutes after drying;
(2) and spin-coating the prepared nickel oxide nanocrystalline electrochromic ink on FTO glass to form a film, carrying out annealing once at 150 ℃ every spin-coating, carrying out spin-coating for 4 times, and finally carrying out ozone treatment for 30 minutes to obtain the nickel oxide nanocrystalline electrochromic film.
Example 2
A preparation method of nickel oxide nanocrystalline electrochromic ink comprises the following specific steps:
(1) 4.5mmol of nickel acetylacetonate, 15ml of oleylamine and 1.8mmol of lithium stearate were placed in a three-necked flask, and a mixed gas of argon and oxygen was introduced at a flow ratio of 4:1 for 10 minutes, and then heated to 100 ℃ and kept warm for 30 minutes.
(2) The reaction was heated to 210 ℃ and incubated for 60 minutes.
(3) After cooling to room temperature, ethanol was added for precipitation, and after centrifugation, the precipitate was dissolved in n-hexane.
(4) Adding a certain amount of hot methanol of 50 deg.C, collecting the upper layer solution, and repeating for 4 times.
(5) Adding acetone for precipitation, centrifuging to obtain nickel oxide nanocrystal, and dissolving the nickel oxide nanocrystal in n-hexane according to the concentration of 10 mg/ml.
(6) Dissolving 2ml of triethyl oxytetrafluoroboric acid in 30ml of acetonitrile, adding a nickel oxide nanocrystalline n-hexane solution, stirring for 12 hours, taking the lower layer solution, and adding toluene for precipitation. And after centrifugation, dissolving the precipitate in N-methyl pyrrolidone according to 100mg/ml to obtain the nickel oxide nanocrystalline electrochromic ink.
A preparation method of a nickel oxide nanocrystalline electrochromic film comprises the following steps:
(1) ultrasonically cleaning the FTO glass by acetone, absolute ethyl alcohol and deionized water for 20 minutes respectively, and carrying out ozone treatment for 30 minutes after drying;
(2) and spin-coating the prepared nickel oxide nanocrystalline electrochromic ink on FTO glass to form a film, carrying out annealing once at 300 ℃ every spin-coating, carrying out spin-coating for 4 times, and finally carrying out ozone treatment for 30 minutes to obtain the nickel oxide nanocrystalline electrochromic film.
From the X-ray diffraction pattern of fig. 1-2 and the transmission electron microscope pattern of fig. 3, it is shown that the nickel oxide nanocrystal prepared by the invention has the characteristics of good crystallinity, good dispersibility, small particle size, uniform size and the like. The nickel oxide nanocrystalline ink prepared after ligand exchange has good stability and can be kept stable after being placed for several months. As can be seen from fig. 4, the nickel oxide nanocrystalline thin film prepared in example 2 has a dense structure, and the kinetic spectrum of fig. 5 and the spectral spectrum of fig. 6 show that the highest transmittance of the thin film reaches 98%, the electrochromic contrast reaches 40.3%, the coloring time is 1.1 seconds, and the fading time is 0.8 seconds. The prepared nickel oxide nanocrystalline electrochromic ink has the viscosity of 3.6mPa & s, the surface tension of 37.6mN/m and the density of 1.22g/cm3A stable drop was calculated to have an Ohnesorge number of 8.4. As shown in fig. 7, a stable ink droplet can be observed in the ink droplet observing function in the ink jet printing apparatus.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the present invention as defined in the accompanying claims.
Claims (10)
1. A preparation method of nickel oxide nanocrystalline electrochromic ink is characterized by comprising the following steps:
(1) mixing and heating nickel salt, a solvent and a protective agent to 50-150 ℃ under argon-oxygen mixed gas, and preserving heat for 10-45 minutes;
(2) heating the substance obtained in the step (1) to a reaction temperature and preserving heat for a period of time to obtain a nickel oxide nanocrystal solution;
(3) purifying the nickel oxide nanocrystal solution to obtain nickel oxide nanocrystals;
(4) and dissolving the nickel oxide nanocrystal in n-hexane, then carrying out ligand exchange, and dissolving in a polar solvent to obtain the nickel oxide nanocrystal electrochromic ink.
2. The method for preparing nickel oxide nanocrystalline electrochromic ink according to claim 1, characterized in that: in the step (1), the solvent is oleylamine, the nickel salt is one of nickel stearate, nickel acetate and nickel acetylacetonate, and the protective agent is lithium stearate.
3. The method for preparing nickel oxide nanocrystalline electrochromic ink according to claim 2, characterized in that: the molar ratio of the nickel acetylacetonate to the lithium stearate is 2.5-3.6: 1, the amount of oleylamine is 10-15 ml.
4. The method for preparing nickel oxide nanocrystalline electrochromic ink according to claim 1, characterized in that: in the step (1), the flow ratio of argon to oxygen is 4: 1-1: 4, the flow of oxygen is 5-10 sccm, and the flow of argon is 25-30 sccm.
5. The method for preparing nickel oxide nanocrystalline electrochromic ink according to claim 1, characterized in that: in the step (2), the heating temperature of the substance is 150-300 ℃, and the heat preservation time is 0.5-1.5 h.
6. The method for preparing the nickel oxide nanocrystalline electrochromic ink according to claim 1, wherein the purification process in the step (3) is specifically as follows: and precipitating the nickel oxide nanocrystal solution with excessive ethanol, centrifuging, dissolving in n-hexane, adding hot methanol to obtain an upper layer solution, adding acetone to precipitate, and centrifuging to obtain the nickel oxide nanocrystal.
7. The method for preparing nickel oxide nanocrystalline electrochromic ink according to claim 6, characterized in that: the hot methanol wash was repeated 4 times.
8. The method for preparing the nickel oxide nanocrystalline electrochromic ink according to claim 6, wherein the ligand exchange process in the step (4) is specifically as follows: adding a ligand exchanger into acetonitrile, uniformly mixing, then adding a nickel oxide nanocrystal n-hexane solution, stirring, taking a lower layer solution, adding toluene, precipitating and centrifuging to obtain a nickel oxide nanocrystal after ligand exchange, and adding a polar solvent to obtain the nickel oxide nanocrystal electrochromic ink.
9. The method for preparing nickel oxide nanocrystalline electrochromic ink according to claim 1, characterized in that: the ligand exchanger is Meerwein salt, and the polar solvent is one of DMF and NMP.
10. The application of the nickel oxide nanocrystalline electrochromic ink is characterized in that: the nickel oxide nanocrystalline electrochromic ink prepared according to the preparation method of any one of claims 1 to 9 can be used for preparing a nickel oxide nanocrystalline electrochromic film.
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