CN112608730B - One-way color-changing nano material and preparation method and application thereof - Google Patents
One-way color-changing nano material and preparation method and application thereof Download PDFInfo
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Abstract
The invention is suitable for the technical field of nano functional materials, and provides a unidirectional color-changing nano material, a preparation method and application thereof, wherein the preparation method comprises the following steps: adding an inducer into the prepared acid solution, and obtaining a first mixed solution after the inducer is completely dissolved; the inducer is one or more of tyrosine, tryptophan, valine, serine, glycine and glutamic acid at any ratio; adding the first mixed solution into the prepared molybdenum salt solution, and uniformly stirring to obtain a second mixed solution; and transferring the second mixed solution to a hydrothermal reaction kettle for hydrothermal reaction, and washing and drying after the reaction is finished to obtain the one-way color-changing nano material. The preparation method provided by the invention is characterized in that amino in inducer molecules is protonated and positively charged in strong acid atmosphere and reacts with MoO 4 2‑ The combination induction forms a nano material crystal nucleus, a metastable phase nano rod is formed in the hydrothermal process, the structure of the final product becomes more uniform under the Oswald curing effect, and the light sensitivity is strong.
Description
Technical Field
The invention belongs to the technical field of nano functional materials, and particularly relates to a unidirectional color-changing nano material, and a preparation method and application thereof.
Background
In the research and application of functional materials, color-changing materials always occupy a considerable proportion, and are always the focus of attention. The photochromic material can be generally divided into an inorganic photochromic material and an organic photochromic material, and compared with the organic photochromic material, the inorganic photochromic material has the advantages of high photochromic reaction rate, strong ageing resistance, high mechanical strength, stable property, long photochromic duration, good thermal stability and the like, and has been partially applied in practice. At present, the most important research on inorganic photochromism is the photochromism glass material, the photochromism crystal material and the photochromism composite film material, and the most important research at present is the photochromism powder material, and by means of the 'size effect' of nano materials, the inorganic and organic photochromism materials are combined in the future, so that the photochromism performance of the photochromism material is obviously enhanced.
Molybdenum is a typical transition metal, and when molybdenum oxide is irradiated by light, electrons in a valence band are excited to a conduction band to generate electron-hole pairs having reduction and oxidation effects, and then photogenerated electrons are converted into hexavalent molybdenum (Mo) 6+ ) Capture to generate pentavalent molybdenum (Mo) 5+ ) Thus pentavalent molybdenum (Mo) 5+ ) And protons (H) in the surrounding environment + ) And the reduced oxide are combined to form the molybdenum bronze, and the discoloration effect is generated. The photochromic properties of molybdenum-based compounds depend to a large extent on the method of preparation of the powder. For example by sol-gel methods, sonochemical methods, hydrothermal methods, chemical precipitation methods, solid phasesThe reaction method can synthesize molybdenum trioxide and the compound thereof with various shapes and phases. However, the molybdenum-based compound prepared by the above preparation method still has the problems of insufficient sensitivity of photochromic performance, high cost, high requirements on application conditions and the like.
Disclosure of Invention
The embodiment of the invention aims to provide a preparation method of a one-way color-changing nano material, and aims to solve the problems that the photochromic performance of a molybdenum-based compound prepared by the prior art is not sensitive enough, the cost is high, the requirement on application conditions is high and the like.
The embodiment of the invention is realized in such a way that the preparation method of the unidirectional color-changing nano material specifically comprises the following steps:
adding an inducer into the prepared acid solution, and obtaining a first mixed solution after the inducer is completely dissolved; the inducer is one or more of tyrosine, tryptophan, valine, serine, glycine and glutamic acid at any ratio;
adding the first mixed solution into the prepared molybdenum salt solution, and uniformly stirring to obtain a second mixed solution;
and transferring the second mixed solution to a hydrothermal reaction kettle for hydrothermal reaction, and washing and drying after the reaction is finished to obtain the unidirectional color-changing nano material.
Another object of the embodiments of the present invention is to provide a unidirectional color-changing nanomaterial, wherein the unidirectional color-changing nanomaterial is prepared by the preparation method of the unidirectional color-changing nanomaterial as described above.
Another object of an embodiment of the present invention is to claim the application of the unidirectional color-changing nanomaterial as described in the foregoing in the field of information security, wherein the unidirectional color-changing nanomaterial simultaneously generates irreversible color change and photoresponsive current under the action of light.
The preparation method of the one-way color-changing nano material provided by the invention has the advantages that amino groups in molecules of tyrosine, tryptophan, valine, serine, glycine and glutamic acid are protonated and positively charged under the strong acid atmosphere, and are easy to react with MoO 4 2- The combination induces the formation of a nano material crystal nucleus, a metastable phase nano rod is formed due to the kinetic factors in the hydrothermal process, and the structure of the final product becomes more uniform under the Oswald curing effect. The final product prepared by the preparation method of the one-way color-changing nano material provided by the invention has quick response to light, can generate macroscopic color change after being irradiated for 10 seconds under ultraviolet light, can generate macroscopic obvious color change after being irradiated for 30 seconds, can generate macroscopic color change after being irradiated for 30 seconds under sunlight, has strong light sensitivity and high sunlight utilization rate, is not easy to fade and reverse, and in the whole preparation process, the raw materials are simple and easy to obtain, are safe and nontoxic, do not need large-scale equipment, have simple synthesis conditions, and effectively reduce the preparation cost.
Drawings
Fig. 1 is an XRD standard spectrum of the molybdenum-based nano powder material prepared in example 1 of the present invention and molybdenum trioxide and glycine;
FIG. 2 is an SEM image and an EDS energy spectrum of the molybdenum-based nanopowder material prepared in example 1 of the invention;
fig. 3 is a UV-VIS diffuse reflection absorption spectrum of the molybdenum-based nano powder material prepared in example 1 of the present invention before and after excitation by 254nm ultraviolet light for 30 seconds;
fig. 4 is a UV-VIS diffuse reflection absorption spectrum of the molybdenum-based nano powder material prepared in example 2 of the present invention before and after excitation by 254nm ultraviolet light for 30 seconds;
fig. 5 is a UV-VIS diffuse reflection absorption spectrum of the molybdenum-based nano powder material prepared in example 3 of the present invention before and after excitation by 254nm ultraviolet light for 30 seconds;
fig. 6 shows a UV-VIS diffuse reflection absorption spectrum of the molybdenum-based nano powder material prepared in example 4 of the present invention before and after excitation by 254nm ultraviolet light for 30 seconds.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The instruments, reagents, materials and the like used in the following examples are conventional instruments, reagents, materials and the like in the prior art and are commercially available in a normal manner unless otherwise specified. Unless otherwise specified, the experimental methods, detection methods, and the like described in the following examples are conventional experimental methods, detection methods, and the like in the prior art.
The invention provides a preparation method of a novel one-way color-changing nano material, aiming at solving the problems of insufficient photochromic performance, high cost, high application condition requirement and the like of a molybdenum-based compound prepared by the existing preparation method, the method takes environment-friendly biological micromolecules (tyrosine, tryptophan, valine, serine, glycine and glutamic acid) as an inducer, takes sodium molybdate as a molybdenum source, has the advantages of simple and easily obtained raw materials, safety, no toxicity, no need of large-scale equipment, simple and easy synthesis conditions and reduced preparation cost, and the prepared molybdenum-based compound powder material has quick response to light, can generate macroscopic color change after being irradiated for 10 seconds under ultraviolet light, can generate macroscopic obvious color change after being irradiated for 30 seconds, can generate macroscopic color change after being irradiated for 30 seconds under sunlight, has strong photosensitivity and high sunlight utilization rate, is not easy to fade, in addition, the prepared product can be used for the safety warning of the encapsulation and the confidentiality conditions of confidential information, materials and substances and can also realize irreversible color change and alarm function and realize the alarm function under the action of photochromism.
The embodiment of the invention provides a preparation method of a one-way color-changing nano material, which comprises the following steps:
adding an inducer into the prepared acid solution, and obtaining a first mixed solution after the inducer is completely dissolved;
adding the first mixed solution into the prepared molybdenum salt solution, and uniformly stirring to obtain a second mixed solution;
and transferring the second mixed solution to a hydrothermal reaction kettle for hydrothermal reaction, and washing and drying after the reaction is finished to obtain the one-way color-changing nano material.
In the embodiment of the invention, the inducer is one or more of tyrosine, tryptophan, valine, serine, glycine and glutamic acid at any ratio.
In the embodiment of the invention, the acid solution is preferably a hydrochloric acid solution, and the molar concentration of the acid solution is 2-3 mol/L.
In the embodiment of the present invention, preferably, the molybdenum salt solution is a sodium molybdate dihydrate solution, and the molar concentration of the molybdenum salt solution is 0.1 to 0.3mol/L.
In the embodiment of the present invention, preferably, the molar ratio of the inducing agent to the molybdenum source in the molybdenum salt solution is (1 to 6): 1.
in the embodiment of the present invention, preferably, the inducing agent is glycine.
In the embodiment of the present invention, preferably, the molar ratio of the acid solution to the molybdenum salt solution is (4 to 10): 1.
in the embodiment of the present invention, it should be noted that the precursor solutions of different molybdenum-based materials can be obtained by adjusting the molar ratio of the acid solution to the molybdenum salt solution, adjusting the PH of the solution, and adjusting the molar ratio of the inducer to the molybdenum source in the molybdenum salt solution, so as to adjust the morphology of the prepared molybdenum-based compound powder material, and implement controllable preparation of the molybdenum-based nano powder material.
In the embodiment of the invention, the hydrothermal reaction is preferably carried out for 3 to 12 hours at 110 to 170 ℃. In particular, the reaction is generally carried out in a polytetrafluoroethylene-lined high-pressure hydrothermal reaction kettle.
In the embodiment of the invention, after the reaction is finished and the reaction kettle is naturally cooled to room temperature, the reaction kettle is washed and precipitated for a plurality of times by using deionized water and absolute ethyl alcohol alternately, and then the reaction kettle is dried for 3-5 hours at the temperature of 60-80 ℃ to obtain the unidirectional color-changing nano material.
The invention provides a preparation method of a one-way color-changing nano material, wherein tyrosine, tryptophan, valine, serine and glycine are adoptedThe amino group in glutamic acid molecule is protonated and positively charged in strong acid atmosphere, and is easy to react with MoO 4 2- The combination induces the formation of a nano material crystal nucleus, a metastable phase nano rod is formed due to the kinetic factors in the hydrothermal process, and the structure of the final product becomes more uniform under the Oswald curing effect. The final product prepared by the preparation method of the one-way color-changing nano material provided by the invention has quick response to light, can generate macroscopic color change after being irradiated for 10 seconds under ultraviolet light, can generate macroscopic obvious color change after being irradiated for 30 seconds, can generate macroscopic color change after being irradiated for 30 seconds under sunlight, has strong light sensitivity and high sunlight utilization rate, is not easy to fade and reverse, and in the whole preparation process, the raw materials are simple and easy to obtain, are safe and nontoxic, do not need large-scale equipment, have simple synthesis conditions, and effectively reduce the preparation cost.
The embodiment of the invention also provides a unidirectional color-changing nano material, which is prepared by the following preparation method:
adding an inducer into the prepared acid solution, and obtaining a first mixed solution after the inducer is completely dissolved;
adding the first mixed solution into the prepared molybdenum salt solution, and uniformly stirring to obtain a second mixed solution;
and transferring the second mixed solution to a hydrothermal reaction kettle for hydrothermal reaction, and washing and drying after the reaction is finished to obtain the one-way color-changing nano material.
The embodiment of the invention also provides the application of the unidirectional color-changing nano material in the field of information confidentiality, compared with the conventional color-changing nano material, the unidirectional color-changing nano material provided by the invention can generate light response current for warning and reminding besides irreversible color change under the action of illumination.
In order to facilitate understanding of the advantages of the product prepared by the above preparation process provided by the present invention over the prior art, the specific implementation processes of various embodiments and XRD standard patterns, SEM patterns and EDS energy spectrum patterns and UV-VIS diffuse reflection absorption spectra of the prepared product will be shown in the following.
Example 1:
1.4517g of sodium molybdate dihydrate (Na) was weighed 2 MoO 4 ·2H 2 O) dissolving the sodium molybdate solution in 20mL of deionized water in a beaker to obtain a sodium molybdate solution for later use;
measuring 16.67mL of concentrated hydrochloric acid (HCL) in a beaker, diluting with deionized water, transferring to a 100mL volumetric flask, and carrying out constant volume to obtain 2mol/L hydrochloric acid solution for later use;
weighing 7.5mL of hydrochloric acid solution from 2mol/L of hydrochloric acid solution for later use, dissolving 1.3513g of glycine in the hydrochloric acid solution, diluting to 20mL with 12.5mL of deionized water, slowly adding the hydrochloric acid solution into the sodium molybdate solution for later use, mixing the hydrochloric acid solution and the sodium molybdate solution, stirring for 30min, transferring to a 50mL high-pressure hydrothermal reaction kettle, heating at 110 ℃ for 12h, naturally cooling to room temperature, and adding deionized water and absolute ethyl alcohol (C) 2 H 5 OH) are alternately washed for 4 times and dried for 5 hours in a drying box at 60 ℃ to obtain the final product.
Example 2:
weighing 0.9678g of sodium molybdate dihydrate in a beaker, and dissolving with 20mL of deionized water to obtain a sodium molybdate solution for later use;
measuring 25mL of concentrated hydrochloric acid in a beaker, diluting the concentrated hydrochloric acid with deionized water, transferring the diluted concentrated hydrochloric acid to a 100mL volumetric flask, and carrying out constant volume to obtain a hydrochloric acid solution of 3mol/L for later use;
measuring 4mL of hydrochloric acid solution from 3mol/L of hydrochloric acid solution for later use, dissolving 1.8017g of glycine in the hydrochloric acid solution, diluting the hydrochloric acid solution to 20mL by 16.0mL of deionized water, slowly adding the hydrochloric acid solution into the sodium molybdate solution for later use, mixing the hydrochloric acid solution and the sodium molybdate solution, stirring the solution for 30min, transferring the solution to a 50mL high-pressure hydrothermal reaction kettle, heating the solution at 130 ℃ for 6h, washing the precipitate for 4 times by using deionized water and absolute ethyl alcohol alternately after the reaction kettle is naturally cooled to room temperature, and drying the precipitate for 3h at 80 ℃ in a drying box to obtain a final product.
Example 3:
weighing 0.9678g of sodium molybdate dihydrate in a beaker, and dissolving with 20mL of deionized water to obtain a sodium molybdate solution for later use;
measuring 20.83mL of concentrated hydrochloric acid in a beaker, diluting the concentrated hydrochloric acid with deionized water, transferring the diluted concentrated hydrochloric acid to a 100mL volumetric flask, and carrying out constant volume to obtain a 2.5mol/L hydrochloric acid solution for later use;
measuring 6mL of hydrochloric acid solution from 2.5mol/L of hydrochloric acid solution for later use, dissolving 0.9008g of glycine in the hydrochloric acid solution, diluting the hydrochloric acid solution to 20mL by 14.0mL of deionized water, then slowly adding the hydrochloric acid solution into sodium molybdate solution to mix the hydrochloric acid solution and the sodium molybdate solution, stirring the solution for 30min, transferring the solution to a 50mL high-pressure hydrothermal reaction kettle, heating the solution for 6h at 150 ℃, alternately washing and precipitating the solution for 3 times by using deionized water and absolute ethyl alcohol after the reaction kettle is naturally cooled to room temperature, and drying the solution for 4h at 70 ℃ in a drying box to obtain a final product.
Example 4:
0.7259g of sodium molybdate dihydrate is weighed and placed in a beaker, and 20mL of deionized water is used for dissolving to obtain a sodium molybdate solution for later use;
measuring 16.67mL of concentrated hydrochloric acid in a beaker, diluting with deionized water, transferring to a 100mL volumetric flask, and carrying out constant volume to obtain a 2mol/L hydrochloric acid solution for later use;
measuring 3mL of hydrochloric acid solution from 2mol/L of hydrochloric acid solution for later use, dissolving 0.6756g of glycine in the hydrochloric acid solution, diluting the hydrochloric acid solution to 20mL by 17.0mL of deionized water, then slowly adding the hydrochloric acid solution into sodium molybdate solution to mix the hydrochloric acid solution and the sodium molybdate solution, stirring the solution for 30min, transferring the solution to a 50mL high-pressure hydrothermal reaction kettle, heating the solution for 3h at 170 ℃, alternately washing and precipitating the solution for 3 times by using deionized water and absolute ethyl alcohol after the reaction kettle is naturally cooled to room temperature, and drying the solution for 4h at 60 ℃ in a drying box to obtain a final product.
The final products obtained in examples 1 to 4 were characterized by XRD, SEM, EDS and UV-VIS, respectively, as follows:
in the invention, a German Bruker D8 advanced X-ray diffractometer is used for detecting the crystal structure and phase information of the prepared molybdenum-based nano powder material. As shown in FIG. 1, the nanometer material and the MoO obtained in example 1 were sequentially arranged from bottom to top 3 (JCPDS No. 05-0508) and C 2 H 5 NO 2 (JCPDS No. 32-1702) XRD standard spectrum, from which MoO can be seen 3 The main diffraction peaks of (A) appear at 2 theta values of 23.32 DEG, 25.72 DEG and 27.24 DEG, glycine (C) 2 H 5 NO 2 ) Characteristic peaks appear at 2 theta values of 29.84 degrees, 14.78 degrees and 23.88 degrees, but the diffraction angle and the diffraction intensity of the obtained nano material are different from those of molybdenum trioxide and glycine, and are not the addition of the molybdenum trioxide and the glycine, but new peaks appear, so that the compound is a new substance completely different from the raw material, and the diffraction peak of the nano material is sharp, so that the crystallinity of the nano material is good, and the improvement of the cycle stability of the photochromic material is facilitated.
FIG. 2 is a SEM and EDS spectra of the product prepared in example 1 of the present invention, and the data corresponding to FIG. 2 are shown in the following table:
| Element | Wt％ | At％ |
| CK | 07.04 | 18.80 |
| NK | 04.43 | 10.14 |
| OK | 24.80 | 49.74 |
| MoL | 63.73 | 21.32 |
| Matrix | Correction | ZAF |
the nano materials are consistent in appearance, are all in a nano rod shape, have the length of 0.1-0.6 mu m and the width of about 100nm, and show that the nano materials can grow towards a certain direction in a specific way due to the existence of an inducer after nucleation under the dynamic condition, and the nano size effect causes the rapid response of the materials to light; the EDS energy spectrum shows that Mo, C, N, O and other elements possibly exist in the compound, and the molybdenum element is a main element, further, the photochromic nano material is a molybdenum base.
As shown in FIGS. 3 to 6, the UV-VIS diffuse reflection absorption spectra of the products obtained in examples 1 to 4 provided by the present invention before and after the excitation of ultraviolet light at 254nm for 30 seconds are respectively shown, wherein the light source used for the test is an ultraviolet mercury lamp with a power of 25W and a wavelength of 254nm, and the illumination intensity irradiated on the surface of the powder is 0.1mW/cm 2 The method comprises the following specific operations: the molybdenum-based powder material has good light absorption performance, after the molybdenum-based powder material is excited by light, the absorption of the powder material to the light is changed, the absorption intensity is increased, and meanwhile, the light can be absorbed before 700 nm.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. The preparation method of the one-way color-changing nano material is characterized by comprising the following steps of:
adding an inducer into the prepared acid solution, and obtaining a first mixed solution after the inducer is completely dissolved; the inducing agent is glycine;
adding the first mixed solution into the prepared molybdenum salt solution, and uniformly stirring to obtain a second mixed solution;
transferring the second mixed solution to a hydrothermal reaction kettle for hydrothermal reaction, and washing and drying after the reaction is finished to obtain the one-way color-changing nano material; the unidirectional color-changing nano material can generate irreversible color change and photoresponse current simultaneously under the action of illumination;
the acid solution is hydrochloric acid solution, and the molar concentration of the acid solution is 2-3 mol/L;
the hydrothermal reaction is carried out for 3 to 12 hours at the temperature of between 110 and 170 ℃.
2. The method for preparing a one-way color-changing nano material according to claim 1, wherein the molybdenum salt solution is a sodium molybdate dihydrate solution, and the molar concentration of the molybdenum salt solution is 0.1-0.3 mol/L.
3. The preparation method of the one-way color-changing nano material as claimed in claim 1, wherein the molar ratio of the inducer to the molybdenum source in the molybdenum salt solution is (1-6): 1.
4. the method for preparing the one-way color-changing nano material according to claim 1, wherein the molar ratio of the acid solution to the molybdenum salt solution is (4-10): 1.
5. the preparation method of the one-way color-changing nano material according to claim 1, wherein after the reaction is finished, the one-way color-changing nano material is obtained by alternately washing and precipitating with deionized water and absolute ethyl alcohol for a plurality of times and drying at 60-80 ℃ for 3-5 h.
6. A unidirectional color-changing nanomaterial, characterized in that the unidirectional color-changing nanomaterial is prepared by the preparation method of the unidirectional color-changing nanomaterial as claimed in any of claims 1~5.
7. The use of the unidirectional color-changing nanomaterial of claim 6 in the field of information security, wherein the unidirectional color-changing nanomaterial can generate irreversible color change and photoresponse current simultaneously under the action of light.
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