CN110359043B - Preparation method of titanium-based lanthanum oxide nanoflower film with dielectric wetting low-voltage response - Google Patents

Preparation method of titanium-based lanthanum oxide nanoflower film with dielectric wetting low-voltage response Download PDF

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CN110359043B
CN110359043B CN201910685394.1A CN201910685394A CN110359043B CN 110359043 B CN110359043 B CN 110359043B CN 201910685394 A CN201910685394 A CN 201910685394A CN 110359043 B CN110359043 B CN 110359043B
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titanium substrate
lanthanum oxide
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王建
章建文
李燕
陈建彪
王成伟
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Northwest Normal University
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Abstract

The invention discloses a preparation method of a titanium-based lanthanum oxide nanoflower film with dielectric wetting low-voltage response, which comprises the following steps: s1, cleaning and degreasing the titanium substrate; s2, electrochemically polishing the titanium substrate; s3, preparation of precursor solution: dissolving 1 part by weight of lanthanum nitrate hexahydrate in 35-45 parts by weight of isopropanol, and fully stirring to obtain a lanthanum oxide precursor solution; s4, carrying out hydrothermal growth of lanthanum oxide; s5, post-processing: and taking out the high-pressure reaction kettle, naturally cooling, taking out the titanium substrate and drying by blowing so as to obtain the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode. The preparation method is simple, low in cost and controllable at low temperature, and the prepared lanthanum oxide nanoflower film is novel in structure, low in dielectric wetting response voltage and high in application value in the aspects of liquid lenses, dielectric wetting display, liquid conveying systems and the like.

Description

Preparation method of titanium-based lanthanum oxide nanoflower film with dielectric wetting low-voltage response
Technical Field
The invention belongs to the technical field of nano materials, and relates to a preparation method of a titanium-based lanthanum oxide nanoflower film.
Background
Dielectric wetting is the behavior of a liquid drop on the surface of a solid dielectric medium to spread on the surface of the medium under the action of an applied electric field. The method is mainly characterized by utilizing the change rule of the contact angle of the liquid drop along with the applied voltage. Due to the advantages of intelligent controllability, quick response and the like of dielectric wetting, the method has great application value in the aspects of biochips, liquid lenses, dielectric wetting display, liquid conveying systems and the like. However, many theoretical and technical problems still exist in the development and utilization of the dielectric wetting device, such as large power consumption caused by large response voltage, difficulty in spontaneous reversibility of dielectric wetting, dielectric wetting hysteresis, contact angle saturation and the like. At present, people mainly try to break through the technical problems restricting the development and application of dielectric wetting devices by preparing high dielectric materials and surface micro-nano structures.
Lanthanum oxide (La)2O3) The rare earth oxide is one of important rare earth oxide rare earth oxides, has a unique electronic structure, can inhibit the formation of hydrogen bonds and surface water molecules, has good hydrophobicity, and is a green and efficient corrosion-resistant coating material. More importantly, La2O3Is a high dielectric material with a dielectric constant of up to 15 and a large initial contact angle, and is clearly an ideal dielectric wetting substrate. Nevertheless, lanthanum oxide (La)2O3) Are very rare in dielectric wetting device development applications. The main reason is nano lanthanum oxide (La)2O3) The problem of the preparation method. Currently, the current practice is. The preparation method of the nano lanthanum oxide mainly comprises a solid phase method, a precipitation method, a hydrothermal method, a sol-gel method and the like. However, the prepared lanthanum oxide is mainly powder composed of nano-rods, nano-spheres, nano-sheets and other particles, and needs to be subjected to a heat treatment process at a temperature of over 700K, which limits the application of the lanthanum oxide in dielectric wetting. Therefore, for the research and development of dielectric wetting devices, the lanthanum oxide (La) which is simple in development, low in temperature and low in cost and has a micro-nano structure surface is developed2O3) The preparation method of the nanoflower film is very necessary. Hydrothermal growth has many unique advantages: 1) because the growth of the lanthanum oxide is carried out on the solid substrate, the problem of an electrode of a dielectric wetting device can be directly solved by selecting a metal substrate titanium sheet; 2) the temperature of the hydrothermal growth is much lower than that of the heat treatment process of other methods; 3) by selecting proper conditions, lanthanum oxide grown by hydrothermal reaction can be directly crystallized, and nanocrystalline nanoflower films with various nanostructures can be spontaneously formed on a substrate under the action of growth stress. Therefore, the preparation of the titanium-based lanthanum oxide nanoflower film with dielectric wetting low voltage response should be paid attention.
Disclosure of Invention
The invention aims at the problems and provides a preparation method of a titanium-based lanthanum oxide nanoflower film with dielectric wetting and low voltage response, which comprises the following steps:
s1, cleaning the titanium substrate: ultrasonically cleaning a titanium sheet for 20 minutes by using acetone and absolute ethyl alcohol, cleaning by using deionized water, and blow-drying to obtain a cleaned titanium substrate;
s2, electrochemical polishing of the titanium substrate: polishing the cleaned titanium substrate by utilizing an electrochemical reaction to obtain a polished titanium substrate;
s3, preparation of precursor solution: dissolving 1 part by weight of lanthanum nitrate hexahydrate in 35-45 parts by weight of isopropanol, and fully stirring to obtain a lanthanum oxide precursor solution;
s4, hydrothermal growth of lanthanum oxide: placing the polished titanium substrate in a high-pressure reaction kettle, measuring the lanthanum oxide precursor solution in the high-pressure reaction kettle, placing the high-pressure reaction kettle in an oven with the temperature of 180-200 ℃, and standing for 19-22 hours;
s5, post-processing: and taking out the high-pressure reaction kettle, naturally cooling, taking out the titanium substrate, and drying by blowing to obtain the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Further, before S1, the titanium sheet is cut.
Further, in S2, the electrochemical polishing is performed in a mixed solution of HCl and HF.
Further, the HCl and HF are in a volume ratio of 8: 1.
Further, in S2, in the electrochemical reaction, the cleaned titanium substrate was used as an anode, the graphite plate was used as a cathode, the distance between the two was maintained at 3cm, and a voltage of 10V was applied for 3 minutes.
Further, in S3, the isopropyl alcohol was used in an amount of 39.3 parts by weight.
Further, in S4, the polished titanium substrate is placed in an autoclave while being tilted.
Further, in S4, the amount of the precursor solution is less than 4/5 of the volume of the reaction tank.
Further, in S4, the temperature of the oven is 190 ℃, and the standing time is 20 h.
Further, in S5, after the titanium substrate is taken out, the method further includes the steps of washing the taken out titanium substrate with water and drying the substrate with nitrogen.
The invention has the advantages that:
the preparation method is simple, low in cost and controllable at low temperature, and the prepared lanthanum oxide nanoflower film is novel in structure, low in dielectric wetting response voltage which is only 4-7V, large in contact angle modulation range and as high as 130oThe liquid lens has great application value in the aspects of liquid lenses, dielectric wetting display, liquid conveying systems and the like.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below with reference to the drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention.
FIG. 1 is an X-ray photoelectron spectrum of a lanthanum oxide nanoflower film prepared in example 1;
FIG. 2 is a narrow scanning spectrum of La3d of the lanthanum oxide nanoflower film prepared in example 1;
FIG. 3 is a narrow scan spectrum of O1s of the lanthanum oxide nanoflower film prepared in example 1;
FIG. 4 is an SEM image of the surface morphology of the lanthanum oxide nanoflower film prepared in example 1;
fig. 5 is a contact angle versus applied voltage curve of the lanthanum oxide nanoflower film prepared in example 1.
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.
According to the present invention, there is provided a method for preparing a dielectric wetting low voltage response titanium based lanthanum oxide nanoflower film, comprising the steps of:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: adding 35-45 parts by weight of isopropanol serving as a solvent into a beaker, then adding 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) and fully stirring to obtain a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: the polished titanium substrate was placed in an inclined position in a 25ml autoclave, and 20ml of the precursor solution was taken and added to the autoclave. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to be 180-200 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the standing growth time is 19-22 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Wherein, before S1, the method also comprises the step of cutting the titanium substrate, and cutting a titanium sheet with the purity of 99.999% into 0.3mm multiplied by 30mm multiplied by 12mm, which is beneficial to putting the titanium sheet into a reaction kettle, and can also indirectly improve the growth rate of lanthanum oxide to a certain extent, thereby better obtaining the lanthanum oxide nano flower film which grows on the titanium substrate in a hydrothermal way. Of course, in a large reaction kettle, the cutting size of the titanium substrate can be adjusted properly.
In S1, the absolute ethyl alcohol and the acetone are washed without the limitation of sequence, and only the final step of washing with deionized water and drying by blowing is needed.
In S2, the electrochemical polishing is carried out in a mixed electrolyte with the volume ratio of HCl to HF being 8:1, so that the polishing operation can be better carried out on the titanium substrate, and better growth conditions are provided for the subsequent hydrothermal growth of lanthanum oxide.
In S3, the solvent may be water, but the lanthanum oxide product is not very efficient, the resulting lanthanum hydroxide and lanthanum carbonate products are very high, and the hydrothermally grown nanostructures are not. In addition, the solvent can also be polyethylene glycol, but the product is mostly lanthanum hydroxide, and the subsequent high-temperature annealing process of more than 750 ℃ is needed to generate lanthanum oxide.
S4, selecting a high-pressure reaction kettle with the volume of 25ml, wherein the dosage of the precursor solution is not more than 20ml, so that the reaction kettle can achieve good utilization rate under the premise of better obtaining the lanthanum oxide nanoflower film grown on the titanium substrate in a hydrothermal mode, and the volume of the reaction kettle is not limited by the reaction.
And (S5) opening the reaction kettle, washing the taken titanium substrate with water, and then drying the titanium substrate under the condition of nitrogen, thereby obtaining the lanthanum oxide nanoflower film with higher purity.
The prepared titanium-based lanthanum oxide nanoflower film is placed on a sample loading platform of a dielectric wetting test system, 5ul of water is dripped on the surface of a sample to form water drops, and the contact angle reaches 150o. Then, the titanium base of the sample surface is connected with a power supply anode, a needle-shaped platinum electrode is connected with a cathode and is inserted into a liquid drop, the voltage is gradually increased, and the contact angle of the liquid drop is recorded. The threshold voltage was found to be only 4V and a saturated contact angle of 20 was reached at 7VoContact angle modulation range as high as 130o。
Example 1:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: 39.3 parts by weight of isopropanol which is an organic solvent is added into a beaker, and then 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) is added and fully stirred, thereby obtaining a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to 190 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 20 hours.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 2:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: adding 35 parts by weight of isopropanol serving as an organic solvent into a beaker, then adding 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) and fully stirring to obtain a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to 190 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 20 hours.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 3:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: adding 45 parts by weight of isopropanol serving as an organic solvent into a beaker, then adding 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) and fully stirring to obtain a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to 190 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 20 hours.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 4:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: 39.3 parts by weight of isopropanol which is an organic solvent is added into a beaker, and then 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) is added and fully stirred, thereby obtaining a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to 180 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 22 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 5:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: 39.3 parts by weight of isopropanol which is an organic solvent is added into a beaker, and then 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) is added and fully stirred, thereby obtaining a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to 180 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 22 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 6:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: adding 35 parts by weight of isopropanol serving as an organic solvent into a beaker, then adding 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) and fully stirring to obtain a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to 180 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 22 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 7:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: 39.3 parts by weight of isopropanol which is an organic solvent is added into a beaker, and then 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) is added and fully stirred, thereby obtaining a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to be 200 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 19 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 8:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: adding 35 parts by weight of isopropanol serving as an organic solvent into a beaker, then adding 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) and fully stirring to obtain a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to be 200 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 19 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 9:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: adding 45 parts by weight of isopropanol serving as an organic solvent into a beaker, then adding 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) and fully stirring to obtain a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to be 200 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 19 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 10:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: 39.3 parts by weight of isopropanol which is an organic solvent is added into a beaker, and then 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) is added and fully stirred, thereby obtaining a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to be 200 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 22 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 11:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: adding 35 parts by weight of isopropanol serving as an organic solvent into a beaker, then adding 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) and fully stirring to obtain a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to be 200 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 22 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 12:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: adding 45 parts by weight of isopropanol serving as an organic solvent into a beaker, then adding 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) and fully stirring to obtain a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to be 200 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 22 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 13:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: 39.3 parts by weight of isopropanol which is an organic solvent is added into a beaker, and then 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) is added and fully stirred, thereby obtaining a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to 180 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 19 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 14:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: adding 35 parts by weight of isopropanol serving as an organic solvent into a beaker, then adding 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) and fully stirring to obtain a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to 180 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 19 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Example 15:
s1, cleaning and degreasing the titanium substrate: firstly, placing the cut titanium sheet into a beaker filled with absolute ethyl alcohol, then placing the beaker into an ultrasonic pool for ultrasonic treatment for 20 minutes, then replacing the absolute ethyl alcohol in the beaker with acetone solution to continue the ultrasonic treatment for 20 minutes, then washing the beaker twice by using deionized water and drying the beaker.
S2, electrochemical polishing of the titanium substrate: the cleaned and degreased titanium substrate is clamped at an anode, a graphite plate is used as a cathode, the distance between the two electrodes is kept at 3cm, then the titanium substrate is placed in a mixed electrolyte of HCl and HF (the volume ratio is 8: 1), and a voltage of 10V is applied for 3 minutes, so that the electrochemical polishing of the titanium substrate is realized.
S3, preparing a hydrothermal growth precursor solution: adding 45 parts by weight of isopropanol serving as an organic solvent into a beaker, then adding 1 part by weight of lanthanum nitrate hexahydrate (La (NO3) 3.6H 2O) and fully stirring to obtain a lanthanum oxide hydrothermal growth precursor solution.
S4, hydrothermal growth of lanthanum oxide: and (3) obliquely and vertically placing the cleaned and degreased titanium substrate in a 25ml high-pressure reaction kettle, and adding 20ml of the precursor liquid into the high-pressure reaction kettle. And then sealing the high-pressure reaction kettle and standing in an oven, wherein the temperature of the oven can be set to 180 ℃, so that the hydrothermal growth of the lanthanum oxide is started, and the growth time is 19 h.
S5, post-processing: and then taking the high-pressure reaction kettle out of the oven, naturally cooling, opening the high-pressure reaction kettle, taking out the placed titanium substrate, washing twice by using water, and drying by using nitrogen, thereby obtaining the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
Experimental example 1:
the lanthanum oxide nanoflower film prepared in example 1 was subjected to an X-ray photoelectron spectroscopy (XPS) test.
Fig. 1 is an X-ray photoelectron spectroscopy (XPS) of the lanthanum oxide nanoflower film prepared in example 1, and fig. 2 is a narrow scan La3d of the lanthanum oxide nanoflower film prepared in example 1; fig. 3 is a narrow scan spectrum of O1s of the lanthanum oxide nanoflower film prepared in example 1.
When the XPS full spectrum and the La3d and O1s narrow scan spectra of the lanthanum oxide nanoflower film were combined for analysis, it can be concluded that: the prepared sample contains lanthanum oxide as a component and also contains part of lanthanum hydroxide impurities.
Experimental example 2:
the lanthanum oxide nanoflower film prepared in example 1 was subjected to surface topography Scanning Electron Microscope (SEM) testing.
FIG. 4 is a Scanning Electron Microscope (SEM) photograph of the surface morphology of the lanthanum oxide nanoflower film prepared in example 1, wherein the compact La is observed2O3Thereon a large amount of La is grown2O3A structured surface is formed.
Experimental example 3:
placing the lanthanum oxide nanoflower film prepared in example 1 on a sample loading platform of a dielectric wetting test system, dripping 5ul of water on the surface of a sample to form a water drop, wherein the contact angle reaches 150o. Then, the titanium base of the sample surface is connected with a power supply anode, a needle-shaped platinum electrode is connected with a cathode and is inserted into a liquid drop, the voltage is gradually increased, and the contact angle of the liquid drop is recorded.
Fig. 5 is a graph showing a relationship between a contact angle of a water droplet on the surface of the lanthanum oxide nanoflower film prepared in example 1 and an applied voltage. It is apparent that the initial contact angle is 150oThe threshold voltage is only 4V, and the contact angle reaches the saturated contact angle when the voltage is increased to 7V, which is only 20oLeft and right, the modulation range of the contact angle is as high as 130o。
Because of the high dielectricity of the lanthanum oxide, the lanthanum oxide nano flower film is arranged on the lanthanum oxide nano flower film under the action of an external electric fieldA large amount of charges are polarized on the surface, and meanwhile, the double-charge-layer capacitor is formed by the charges and the heterogeneous charges induced on the lower surface of the liquid drop, so that the liquid drop is driven to spread on the surface of the medium, and the contact angle is reduced; meanwhile, due to the surface structure, under the action of an external electric field, liquid can also generate electric adsorption to enter the gaps of the nano structure, and the contact angle can also be reduced. The response voltage of the prepared lanthanum oxide nanoflower film dielectric wetting is greatly reduced, the threshold voltage is only 4V, and the modulation range of the contact angle is greatly improved to 130o. And the lanthanum oxide nanoflower film is prepared hydrothermally and has a low dielectric wetting response voltage of 4V and a dielectric wetting response voltage as high as 130oContact angle modulation range of (1).
The technology of the invention is a simple, low-cost and low-temperature controllable method for preparing lanthanum oxide, and the prepared lanthanum oxide nanoflower film has novel structure, low dielectric wetting response voltage which is only 4-7V, large contact angle modulation range which is as high as 130oThe liquid lens has great application value in the aspects of liquid lenses, dielectric wetting display, liquid conveying systems and the like.
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, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. The preparation method of the dielectric wetting low-voltage response titanium-based lanthanum oxide nanoflower film is characterized by comprising the following steps of:
s1, cleaning the titanium substrate: ultrasonically cleaning a titanium sheet for 20 minutes by using acetone and absolute ethyl alcohol, cleaning by using deionized water, and blow-drying to obtain a cleaned titanium substrate;
s2, electrochemical polishing of the titanium substrate: polishing the cleaned titanium substrate by utilizing an electrochemical reaction to obtain a polished titanium substrate;
s3, preparation of precursor solution: dissolving 1 part by weight of lanthanum nitrate hexahydrate in 35-45 parts by weight of isopropanol, and fully stirring to obtain a lanthanum oxide precursor solution;
s4, hydrothermal growth of lanthanum oxide: placing the polished titanium substrate in a high-pressure reaction kettle, measuring the lanthanum oxide precursor solution in the high-pressure reaction kettle, placing the high-pressure reaction kettle in an oven with the temperature of 180-200 ℃, and standing for 19-22 hours;
s5, post-processing: and taking out the high-pressure reaction kettle, naturally cooling, taking out the titanium substrate, and drying by blowing to obtain the lanthanum oxide nanoflower film which grows on the titanium substrate in a hydrothermal mode.
2. The method for preparing a titanium-based lanthanum oxide nanoflower film according to claim 1, further comprising: and cutting the titanium sheet before S1.
3. The method of claim 1, wherein the electrochemical polishing is performed in a mixed solution of HCl and HF in S2.
4. The method of claim 3, wherein the volume ratio of HCl to HF is 8: 1.
5. The method of claim 1, wherein in step S2, the cleaned titanium substrate is used as an anode, the graphite plate is used as a cathode, the distance between the two electrodes is maintained at 3cm, and a voltage of 10V is applied for 3 minutes.
6. The method of claim 1, wherein the isopropyl alcohol is used in an amount of 39.3 parts by weight in S3.
7. The method of claim 1, wherein the polished titanium substrate is placed in an autoclave while being tilted at S4.
8. The method of claim 1, wherein the amount of the precursor solution used in S4 is less than 4/5 of the volume of the reaction tank.
9. The method for preparing titanium-based lanthanum oxide nanoflower film according to claim 1, wherein in S4, the temperature of the oven is 190 ℃ and the standing time is 20 h.
10. The method of claim 1, wherein in step S5, after the titanium substrate is taken out, the method further comprises the steps of washing the taken out titanium substrate with water and drying the substrate with nitrogen.
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