CN111355131A - Composite material negative ion release head, preparation method thereof and negative ion generating electrode - Google Patents
Composite material negative ion release head, preparation method thereof and negative ion generating electrode Download PDFInfo
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- CN111355131A CN111355131A CN201811573508.5A CN201811573508A CN111355131A CN 111355131 A CN111355131 A CN 111355131A CN 201811573508 A CN201811573508 A CN 201811573508A CN 111355131 A CN111355131 A CN 111355131A
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Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01T—SPARK GAPS; OVERVOLTAGE ARRESTERS USING SPARK GAPS; SPARKING PLUGS; CORONA DEVICES; GENERATING IONS TO BE INTRODUCED INTO NON-ENCLOSED GASES
- H01T23/00—Apparatus for generating ions to be introduced into non-enclosed gases, e.g. into the atmosphere
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01T—SPARK GAPS; OVERVOLTAGE ARRESTERS USING SPARK GAPS; SPARKING PLUGS; CORONA DEVICES; GENERATING IONS TO BE INTRODUCED INTO NON-ENCLOSED GASES
- H01T19/00—Devices providing for corona discharge
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01T—SPARK GAPS; OVERVOLTAGE ARRESTERS USING SPARK GAPS; SPARKING PLUGS; CORONA DEVICES; GENERATING IONS TO BE INTRODUCED INTO NON-ENCLOSED GASES
- H01T19/00—Devices providing for corona discharge
- H01T19/04—Devices providing for corona discharge having pointed electrodes
Abstract
The invention discloses a composite material anion release head, which comprises: the titanium dioxide nanotube array comprises a plurality of titanium dioxide nanotubes, the plurality of titanium dioxide nanotubes are formed on the conductive metal wire, and the fullerene layer is formed on the part of the conductive metal wire, which is not covered by the titanium dioxide nanotube array, and the titanium dioxide nanotube array. The invention also discloses a method for preparing the composite material negative ion release head and a negative ion generating electrode. The composite material anion releasing head can release more anions, almost no by-products such as ozone, nitric oxide and the like are generated, and the service life is long.
Description
Technical Field
The invention relates to a negative ion generating technology, in particular to a composite material negative ion release head, a preparation method thereof and a negative ion generating electrode.
Background
At present, the most advanced anion generation technology at home and abroad basically adopts a negative high voltage source to make carbon fibers into a discharge electrode, namely an anion release head. The negative ion releasing head is fixed on the metal rod to form a negative ion generating electrode. When the negative ion generating electrode is applied, the negative ion generating electrode is connected with a high-voltage power supply, the carbon fiber negative ion releasing head sprays electrons to the surrounding space at a high speed, the electrons are quickly captured by air ions to form air negative ions, and meanwhile, the positive ions are neutralized and reduced by utilizing the potential induction of a negative electric field to obtain a relatively purified negative ion field. The carbon fiber material adopted by the relatively advanced anion release head on the market at present is mainly fullerene (C60). The fullerene is a superconducting material with the resistance close to zero, is beneficial to the free precipitation of electric ions, can generate ecological-grade small-particle-size negative oxygen ions with small particle size, high activity and long migration distance, has high negative ion purity, and hardly generates byproducts such as ozone, nitrogen oxides, positive ions and the like.
The fullerene anion release head on the market generally works under the negative pressure of more than 8000V at present, and the release concentration of anions can be guaranteed, however, the strength of the carbon fiber is low, the external environment is easy to influence the performance of the release head, and the surface of the cellulose is easy to adsorb dust and needs to be frequently cleaned, so that the maintenance period is short, and the service life is also influenced.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a composite material negative ion release head, a preparation method thereof and a negative ion generating electrode. The composite material anion release head provided by the invention can release more doses of anions, almost no product is generated, and the service life is longer.
In order to achieve the above object, in a first aspect, the present invention provides a composite negative ion discharge head comprising: the titanium dioxide nanotube array comprises a plurality of titanium dioxide nanotubes, the plurality of titanium dioxide nanotubes are formed on the conductive metal wire, and the fullerene layer is formed on the part of the conductive metal wire, which is not covered by the titanium dioxide nanotube array, and the titanium dioxide nanotube array.
In an embodiment of the invention, a mass ratio of the titanium dioxide nanotube array to the fullerene layer may be 0.1 to 1:1, and optionally, may be 0.1 to 0.5: 1.
In an embodiment of the invention, the thickness of the fullerene layer may be 2 to 10nm, and optionally, may be 5 to 10 nm.
In an embodiment of the present invention, the conductive metal wire may be a titanium wire, a molybdenum wire, a tungsten wire, or an iron wire.
In a second aspect, the present invention provides a method of making a composite negative ion-releasing head, the method comprising:
forming a titanium dioxide nanotube array on the conductive metal wire; and
and forming a fullerene layer on the part of the conductive metal wire which is not covered by the titanium dioxide nanotube array and the titanium dioxide nanotube array.
In an embodiment of the present invention, the forming the titanium dioxide nanotube array on the conductive wire may include:
forming a titanium film on the conductive wire; and
and annealing the titanium film to form a titanium dioxide nanotube array.
In an embodiment of the present invention, the method for forming the titanium film on the conductive metal wire may be an electron beam evaporation coating method.
In the embodiment of the invention, the conditions of the electron beam evaporation coating method can comprise that the vacuum degree of a chamber is 1 × 10 when the titanium film is deposited-8～5×10-8And Torr, and controlling the thickness of the titanium film to be 100-300 nm.
In an embodiment of the present invention, the annealing treatment conditions may include: the annealing temperature is 350-600 ℃, and optionally, the annealing temperature is 450-500 ℃; the annealing time is 1 to 5 hours, optionally 2 to 3 hours.
In an embodiment of the present invention, the method may further include: prior to forming the array of titanium dioxide nanotubes on the conductive wire,
cleaning and drying the conductive wire; and
and (4) removing impurities from the surface of the dried conductive metal wire by using acid liquor.
In an embodiment of the present invention, the washing and drying the conductive wire may include: and sequentially carrying out ultrasonic cleaning in acetone, absolute ethyl alcohol and deionized water, and then blowing the ultrasonically cleaned conductive metal wire by using nitrogen.
In an embodiment of the present invention, the acid solution may be an HF solution.
In an embodiment of the present invention, the method may further include: after the cleaning and drying of the conductive wire, before the impurity removing process,
and plating a transition metal layer on the dried conductive metal wire.
In an embodiment of the present invention, the transition metal layer may be an aluminum layer or a molybdenum layer.
In an embodiment of the invention, the thickness of the transition metal layer may be 0.5 to 2.5 μm.
In an embodiment of the present invention, the forming a fullerene layer on the portion of the conductive wire not covered by the titanium dioxide nanotube array and the titanium dioxide nanotube array may include:
dispersing fullerene in water to form a stable suspension;
putting the conductive metal wire with the titanium dioxide nanotube array into the suspension, and forming a fullerene layer on the part of the conductive metal wire which is not covered by the titanium dioxide nanotube array and the titanium dioxide nanotube array by adopting a vertical deposition method to obtain a negative ion release head; and
and taking the negative ion release head out of the suspension and drying.
In an embodiment of the invention, a method of forming a stable suspension may comprise:
crushing fullerene;
mixing the pulverized fullerene with water in a container, and ultrasonically dispersing until no fullerene is attached to the surface of the container and the solution in the container is not layered.
In the embodiment of the invention, the concentration of the fullerene in the suspension can be 0.1-1 g/L.
In an embodiment of the present invention, the conditions of the vertical deposition method may include: the temperature is 50-120 ℃, and optionally, the temperature is 60-100 ℃; the time is 15 to 31 hours, optionally 16 to 30 hours.
In a third aspect, the invention provides the composite material negative ion release head prepared by the method.
In a fourth aspect, the present invention provides an anion generating electrode, which comprises a metal rod, a conductive fixing device and an anion releasing head, wherein the anion releasing head is fixed on the metal rod through the conductive fixing device, and is electrically connected with the metal rod, and the anion releasing head is the composite material anion releasing head as described above or the composite material anion releasing head prepared by the method as described above.
The negative ion release head of the composite material is formed by loading the composite material of the titanium dioxide nanotube array and the fullerene on a conductive metal wire. The conductive metal wire can conduct electricity and improve the hardness of the negative ion release head, so that the service life of the composite material negative ion release head is prolonged. The titanium dioxide nanotube array endows the anion release head with the functions of decontamination and sterilization.
Meanwhile, the titanium dioxide nanotube array and the conductive metal wire do not bring adverse effects on the performance of the negative ion release head, so that the negative ion release head made of the composite material can generate ecological-grade small-particle-size negative oxygen ions with small particle size, high activity and long migration distance, the purity of the negative ions is high, and almost no byproducts such as ozone, nitrogen oxide and the like are generated.
Drawings
Fig. 1 is an enlarged schematic view of a partial structure of a composite material negative ion release head according to an embodiment of the present invention.
Fig. 2 is a schematic structural view of a negative ion generating electrode according to an embodiment of the present invention.
Reference numerals in the drawings denote:
1-conductive metal wire 2-titanium dioxide nanotube array 3-fullerene layer
4-metal rod 5-conductive fixing device 6-negative ion release head
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. 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.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
An embodiment of the present invention provides a composite material negative ion release head, as shown in fig. 1, the composite material negative ion release head includes: the conductive metal wire comprises a conductive metal wire 1, a titanium dioxide nanotube array 2 and a fullerene layer 3, wherein the titanium dioxide nanotube array 2 comprises a plurality of titanium dioxide nanotubes, the plurality of titanium dioxide nanotubes are formed on the conductive metal wire 1, and the fullerene layer 3 is formed on the part of the conductive metal wire 1 which is not covered by the titanium dioxide nanotube array 2 and the titanium dioxide nanotube array 2.
The negative ion release head of the embodiment of the invention is formed by loading a composite material of a titanium dioxide nanotube array 2 and fullerene on a conductive metal wire 1. The conductive metal wire 1 has conductivity, is convenient for transmission and release of electrons, and can improve the hardness of the negative ion release head, thereby prolonging the service life of the negative ion release head. The titanium dioxide nanotube array 2 can generate negative ions, and the release amount of the negative ions can be improved to a certain extent; moreover, the introduction of the titanium dioxide nanotube array 2 also enables the anion air generated by the anion release head under the illumination condition to increase the functions of decontamination and sterilization. The principle that the titanium dioxide nanotube array 2 generates negative ions and enables the negative ion air to have the functions of decontamination and sterilization is as follows:
under irradiation of light or ultraviolet rays, TiO2Electrons on the surface absorb enough energy to be separated, and positively charged holes are formed at the positions where the electrons are separated, and the holes are attached to the TiO2The water molecules on the surface are oxidized to be converted into hydroxyl radicals with great activity, and the hydroxyl radicals can take electrons once meeting organic matters, so that the organic matter molecules are decomposed due to the breakage of bonds. The general pollutants or pathogens are mostly carbohydrates and are decomposed into water and carbon dioxide, so that the effects of decontamination and sterilization can be achieved. Detachment of TiO2The electrons on the surface reduce oxygen in the air, so that the oxygen becomes negative oxygen ions (i.e., air negative ions). The negative oxygen ion can also react with TiO2The organic compounds on the surface are oxidatively decomposed.
It should be understood by those skilled in the art that the plurality of titanium dioxide nanotubes of the titanium dioxide nanotube array 2 may be vertically grown on the conductive metal wire 1, or may be obliquely grown on the conductive metal wire 1, for example, the included angle between the titanium dioxide nanotubes and the conductive metal wire 1 may be 30 ° or 60 ° or other angles.
In an embodiment of the invention, a mass ratio of the titanium dioxide nanotube array to the fullerene layer may be 0.1 to 1:1, for example, 0.1 to 0.5: 1. The corresponding mass can be obtained by weighing.
In an embodiment of the invention, the thickness of the fullerene layer may be 2 to 10nm, for example, 5 to 10 nm.
In the embodiment of the present invention, the conductive metal wire 1 may be a titanium wire, a molybdenum wire, a tungsten wire, or an iron wire. Alternatively, stainless steel wire may be used instead of the conductive wire.
In the embodiment of the invention, 20-40 conductive metal wires can be arranged on 1 negative ion release head.
The embodiment of the invention also provides a method for preparing the composite material negative ion release head, which comprises the following steps:
forming a titanium dioxide nanotube array 2 on the conductive metal wire 1; and
and forming a fullerene layer 3 on the part of the conductive metal wire 1 which is not covered by the titanium dioxide nanotube array 2 and the titanium dioxide nanotube array 2.
In an embodiment of the present invention, the forming the titanium dioxide nanotube array 2 on the conductive wire 1 may include:
forming a titanium film on the conductive wire 1; and
and annealing the titanium film to form the titanium dioxide nanotube array 2.
In the embodiment of the present invention, the method for forming the titanium film on the conductive metal wire 1 may be an electron beam evaporation coating method. Compared with other coating methods, the electron beam evaporation coating method can generate a film with higher purity and precision.
In the embodiment of the invention, the vacuum degree of the chamber when the titanium film is deposited by adopting the electron beam evaporation coating method can be 1 × 10-8～5×10-8Torr may be, for example, 3 × 10-8～5×10-8Torr，1×10-8～5×10-8The vacuum degree of Torr can ensure that a titanium film with expected thickness is formed, and the titanium film has better uniformity and moderate compactness; the thickness of the titanium film can be 100-300 nm, for example, 200-300 nm, the titanium film with the thickness of 100-300 nm has good adhesiveness, is not easy to fall off from the conductive metal wire, and can ensure the length of the titanium dioxide nanotube which grows subsequently. The target material for depositing the titanium film by adopting the electron beam evaporation coating method can be titanium, and the sample stage can be static or rotate at the speed of 10rpm during deposition.
In an embodiment of the present invention, an annealing temperature of the annealing treatment may be 350 to 600 ℃, for example, 450 to 500 ℃. When the annealing temperature is 350-600 ℃, the titanium film can grow into more titanium dioxide nanotube arrays 2 along the expected direction, and when the annealing temperature is 450-500 ℃, the titanium film can be ensured to completely grow into the titanium dioxide nanotube arrays 2. The annealing time of the annealing treatment can be 1-5 hours, for example, 2-3 hours, and the annealing time is 1-5 hours, so that the titanium film can be fully oxidized into titanium dioxide. The annealing process may be performed in air or oxygen.
In an embodiment of the present invention, the method may further include: before the titanium dioxide nanotube array 2 is formed on the conductive metal wire 1,
cleaning and drying the conductive wire 1; and
and (3) removing impurities from the surface of the dried conductive metal wire 1 by using acid liquor.
In an embodiment of the present invention, the washing and drying the conductive wire 1 may include: and sequentially carrying out ultrasonic cleaning in acetone, absolute ethyl alcohol and deionized water, and then blowing the ultrasonically cleaned conductive metal wire 1 by using nitrogen. The purpose of cleaning is to remove organic matters on the surface of the conductive metal wire 1, and the cleaning can also be carried out by adopting separate acetone or absolute ethyl alcohol, but better cleaning effect can be obtained by sequentially adopting acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning. The power of ultrasonic cleaning can be 200-600W, and the time of ultrasonic cleaning can be 5-10 minutes, for example, 10 minutes. The conductive metal wire is dried by adopting a nitrogen blow-drying mode, so that the surface of the conductive metal wire can be prevented from being oxidized, and the purity of nitrogen is over 99 percent.
In an embodiment of the present invention, the acid solution may be an HF solution. Removing impurities from the surface of the dried conductive metal wire 1 by using acid liquor: and soaking the conductive metal wire 1 in an HF solution. The impurities on the surface of the conductive metal wire 1 are mainly organic matters, oxides, stains and the like, and can be removed by the HF solution.
The mass fraction of the HF solution can be 5-10%, the soaking time can be 2-5 minutes, the HF solution with the concentration and the soaking time can ensure that organic matters, natural oxidation layers and stains on the surface of the metal wire 1 can be thoroughly removed, and the metal wire 1 is not corroded. And (3) removing a natural oxide layer on the surface of the conductive metal wire 1 by soaking in an HF solution to form a free surface, so that the subsequent attached growth of a titanium film is facilitated.
In an embodiment of the present invention, the method may further include: after the conductive metal wire 1 is cleaned and dried, before the impurity removal treatment, a transition metal layer is plated on the dried conductive metal wire 1.
In the embodiment of the present invention, the method for plating the transition metal layer on the conductive metal wire 1 may be a magnetron sputtering method or an evaporation method.
The purpose of plating the transition metal layer on the conductive wire 1 is to improve the decomposition corrosion resistance of the conductive wire 1. In an embodiment of the present invention, the transition metal layer may be an aluminum layer or a molybdenum layer. The thickness of the transition metal layer may be 0.5 to 2.5 μm, for example, 1 to 2 μm. The transition metal layer with the thickness of 0.5-2.5 microns has better adhesiveness and is not easy to fall off, the formation of a subsequent titanium film is not influenced, and the subsequent titanium film can be completely formed on the transition metal layer and cannot be formed on the metal wire 1. When the conductive metal wire 1 is a molybdenum wire, the step of plating the transition metal layer can be omitted because the molybdenum wire itself has a sufficient decomposition corrosion resistance.
In an embodiment of the present invention, the forming of the fullerene layer 3 on the portion of the conductive metal wire 1 not covered by the titanium dioxide nanotube array 2 and the titanium dioxide nanotube array 2 may include:
dispersing fullerene in water to form a stable suspension; and
putting the conductive metal wire 1 with the titanium dioxide nanotube array 2 into the suspension, and forming a fullerene layer 3 on the part of the conductive metal wire 1 which is not covered by the titanium dioxide nanotube array 2 and the titanium dioxide nanotube array 2 by adopting a vertical deposition method to obtain a negative ion release head; and
and taking the negative ion release head out of the suspension and drying.
The method for depositing the fullerene layer 3 by adopting the vertical deposition method is simple, the growth temperature is low, the viscosity of the growth solution is low, the integrity of the grown fullerene layer 3 is good, and the surface is more uniform.
In the embodiment of the present invention, the temperature when the fullerene layer 3 is formed by the vertical deposition method may be 50 to 120 ℃, for example, the deposition temperature may be 60 to 100 ℃, and the deposition temperature is 50 to 120 ℃, which is favorable for forming the fullerene layer 3 with good compactness, and the speed of forming the fullerene layer 3 is fast. The deposition time may be 15 to 31 hours, for example, 16 to 30 hours, and the deposition time of 15 to 31 hours is favorable for forming the fullerene layer 3 with a desired thickness. The thickness of the fullerene layer 3 may be 2 to 10 nm.
In an embodiment of the present invention, the dispersing fullerenes in water to form a stable suspension may include:
crushing fullerene;
mixing the pulverized fullerene with water in a container, and ultrasonically dispersing until no fullerene is attached to the surface of the container and the solution in the container is not layered.
In the embodiment of the invention, the fullerene can be pulverized by grinding, ball milling and the like, but the ball milling process is simple, and the effect of improving the dispersibility is good. The particle size of the fullerene after pulverization is less than 1 μm, and may be, for example, 100 to 500 nm.
In the embodiment of the invention, the concentration of the fullerene in the suspension can be 0.1-1 g/L, and the suspension with the concentration can ensure that a composite material layer with proper thickness (for example, 2-10 nm) and good uniformity is obtained in the subsequent deposition growth process, and is beneficial to the negative ion release head to release electrons and release negative ions with higher concentration.
In an embodiment of the present invention, drying the negative ion releasing head may include: and drying the negative ion release head at a constant temperature. The drying temperature can be 60-80 ℃, and the drying time can be 30-60 minutes.
The embodiment of the invention also provides an anion generating electrode, which comprises a metal rod 4, a conductive fixing device 5 and an anion releasing head 6, wherein the anion releasing head 6 is fixed on the metal rod 4 through the conductive fixing device 5, the anion releasing head 6 is electrically connected with the metal rod 4, and the anion releasing head 6 is the composite material anion releasing head or the composite material anion releasing head prepared by the method.
Examples
The present invention will be described in detail below by way of examples, but the present invention is not limited thereto. In the following examples, unless otherwise specified, all methods used are conventional in the art, and all reagents used are commercially available.
In each embodiment, the conductive fixing device is a copper wire, and the conductive metal wire is fixed on the metal rod in a bundling mode.
Example 1
The method for preparing the composite material anion release head of the embodiment comprises the following steps:
s1: carrying out ultrasonic cleaning on a titanium wire in acetone, absolute ethyl alcohol and deionized water in sequence, wherein the ultrasonic cleaning power is 200W, the ultrasonic cleaning time is 10 minutes, and then blowing the titanium wire by using high-purity nitrogen with the purity of 99.9 percent;
s2: plating an aluminum layer with the thickness of 2.5 mu m on the surface of the titanium wire by adopting an evaporation method;
s3: soaking the titanium wire plated with the aluminum layer in 5 mass percent of HF solution for 5 minutes, and then drying the titanium wire in a nitrogen atmosphere;
s4, fixing the titanium wire obtained in the step S3 on a sample table of an electron beam evaporation coating machine, taking titanium as a target material, and pumping a chamber of the electron beam evaporation coating machine to 5 × 10-8High vacuum of Torr, and making the sample stage still, growing a titanium film with the thickness of 100nm on the titanium wire;
s5: annealing the product obtained in the step S4 in air at 450 ℃ for 3 hours, and growing a titanium film into a titanium dioxide nanotube array;
s6: grinding fullerene balls to the particle size of 100-500 nm, putting into a container, adding deionized water into the container, and ultrasonically dispersing until no fullerene is attached to the surface of the container and the solution in the container is not layered to obtain a stable suspension, wherein the concentration of the fullerene in the suspension is 0.1 g/L;
s7: binding 25 titanium wires with the titanium dioxide nanotube array obtained in the step S5 on a titanium rod through a conductive fixing device, placing the titanium wires into the suspension obtained in the step S6, then placing the titanium wires into a thermostat for growth, setting the temperature of the thermostat to be 60 ℃, and growing a fullerene layer with the thickness of 5nm on the part, which is not covered by the titanium dioxide nanotube array, of the titanium wires and the titanium dioxide nanotube array by adopting a vertical deposition method for 30 hours to obtain a composite material negative ion release head, wherein the mass ratio of the titanium dioxide nanotube array to the fullerene layer is 0.1: 1;
s8: and taking the negative ion release head out of the suspension, and drying at the constant temperature of 60 ℃ for 60 minutes.
Example 2
The method for preparing the composite material anion release head of the embodiment comprises the following steps:
s1: carrying out ultrasonic cleaning on the molybdenum wire in acetone, absolute ethyl alcohol and deionized water in sequence, wherein the ultrasonic cleaning power is 400W, the ultrasonic cleaning time is 8 minutes, and then blowing and drying the molybdenum wire by using high-purity nitrogen with the purity of 99.9%;
s2: soaking the blow-dried molybdenum wire in an HF solution with the mass fraction of 7% for 3 minutes, and then drying the molybdenum wire in a helium atmosphere;
s3, fixing the molybdenum wire obtained in the step S2 on a sample table of an electron beam evaporation coating machine, taking titanium as a target material, and pumping a chamber of the electron beam evaporation coating machine to 3 × 10-8A high vacuum of Torr is carried out, and a sample stage is rotated at a speed of 10rpm, and a titanium film with the thickness of 200nm is grown on the molybdenum wire;
s4: annealing the product obtained in the step S3 in oxygen at 475 ℃ for 2.5 hours, and growing a titanium film into a titanium dioxide nanotube array;
s5: grinding fullerene balls to the particle size of 100-500 nm, putting into a container, adding deionized water into the container, and ultrasonically dispersing until no fullerene is attached to the surface of the container and the solution in the container is not layered to obtain a stable suspension, wherein the concentration of the fullerene in the suspension is 0.5 g/L.
S6: binding 30 molybdenum wires with the titanium dioxide nanotube array obtained in the step S4 on a molybdenum rod through a conductive fixing device, placing the molybdenum wires into the suspension obtained in the step S5, then placing the molybdenum wires into a thermostat for growth, setting the temperature of the thermostat to be 80 ℃, and growing a fullerene layer with the thickness of 7nm on the part, which is not covered by the titanium dioxide nanotube array, of the molybdenum wires and the titanium dioxide nanotube array by adopting a vertical deposition method, so as to obtain the composite material negative ion release head, wherein the mass ratio of the titanium dioxide nanotube array to the fullerene layer is 0.3: 1;
s7: and taking the negative ion release head out of the suspension, and drying at the constant temperature of 70 ℃ for 50 minutes.
Example 3
The method for preparing the composite material anion release head of the embodiment comprises the following steps:
s1: carrying out ultrasonic cleaning on a tungsten filament in acetone, absolute ethyl alcohol and deionized water in sequence, wherein the ultrasonic cleaning power is 600W, the ultrasonic cleaning time is 5 minutes, and then blowing the tungsten filament by using high-purity nitrogen with the purity of 99.9 percent;
s2: plating a molybdenum layer with the thickness of 0.5 mu m on the surface of the tungsten wire by adopting a magnetron sputtering method;
s3: soaking the tungsten wire plated with the molybdenum layer in 10 mass percent of HF solution for 2 minutes, and then drying the tungsten wire in a neon gas atmosphere;
s4, fixing the tungsten filament obtained in the step S3 on a sample table of an electron beam evaporation coating machine, taking titanium as a target material, and pumping a chamber of the electron beam evaporation coating machine to 1 × 10-8A high vacuum of Torr and rotating a sample stage at a speed of 10rpm, and growing a titanium film with a thickness of 300nm on the tungsten wire;
s5: annealing the product obtained in the step S4 in oxygen at 500 ℃ for 2 hours, and growing a titanium film into a titanium dioxide nanotube array;
s6: grinding fullerene balls to the particle size of 100-500 nm, putting into a container, adding deionized water into the container, and ultrasonically dispersing until no fullerene is attached to the surface of the container and the solution in the container is not layered to obtain a stable suspension, wherein the concentration of the fullerene in the suspension is 1 g/L.
S7: binding 35 tungsten wires with the titanium dioxide nanotube array obtained in the step S5 on a tungsten rod through a conductive fixing device, placing the tungsten wires into the suspension obtained in the step S6, then placing the tungsten wires into a thermostat for growth, setting the temperature of the thermostat to be 100 ℃, and growing a fullerene layer with the thickness of 10nm on the part, which is not covered by the titanium dioxide nanotube array, of the tungsten wires and the titanium dioxide nanotube array by adopting a vertical deposition method for 15 hours to obtain a composite material negative ion release head, wherein the mass ratio of the titanium dioxide nanotube array to the fullerene layer is 0.5: 1;
s8: and taking the negative ion release head out of the suspension, and drying at the constant temperature of 80 ℃ for 30 minutes.
Example 4
This example differs from example 2 only in that: the annealing temperature in step S4 was 350 ℃, and the annealing time was 5 hours.
Example 5
This example differs from example 2 only in that: the annealing temperature in step S4 was 600 ℃ and the annealing time was 1 hour.
Example 6
This example differs from example 2 only in that: the temperature of the oven in step S6 was 120 ℃ for 15 hours.
Example 7
This example differs from example 2 only in that: in the composite material anion releasing head obtained in step S6, the mass ratio of the titanium dioxide nanotube array to the fullerene layer is 1: 1.
Comparative example 1
The negative ion emitting head of this comparative example comprises fullerene and the same molybdenum rod as in example 2 of the present invention, and fibers of the fullerene were bundled on the molybdenum rod using copper wires.
Performance testing
1. Anion release test
1) Testing instrument
Hand-held atmospheric negative ion tester-manufacturer: hua Si Tong; the instrument model is as follows: WST-3200 Pro.
2) Test conditions
Temperature: 18 deg.C
Relative humidity: 18 percent of
PM2.5：30μg/m2
Output voltage connected to one end of the metal rod: 40 kV.
3) Test procedure
A tester holds the atmosphere negative ion tester, respectively stands in the positive front, the left side of the negative ion release head to be tested in the direction of 22.5 degrees, and the right side of the negative ion release head to be tested in the direction of 22.5 degrees, and respectively stands at the positions 2 and 4m away from the negative ion release head to be tested, and the quantity of negative ions released by the negative ion release head to be tested is tested.
4) Test results
After the anion releasing heads of each example and comparative example were prepared, the use was continued for 10 hours, and then the test was performed. The test results of the negative ion emitting heads of examples and comparative examples are shown in Table 1 (note: the left, middle and right in Table 1 indicate the 22.5 degree left direction, the right direction and the front direction of the negative ion emitting head, respectively).
TABLE 1
As can be seen from table 1, the negative ion release amount of the composite negative ion release head according to the example of the present invention was not reduced or even more compared to the fullerene negative ion release head according to the comparative example. The introduction of the conductive metal wire does not bring adverse effects on the release amount of negative ions, and the composite negative ion release head provided by the embodiment of the invention can generate ecological-grade small-particle-size negative oxygen ions with small particle size, high activity and long migration distance. But the introduction of the conductive metal wire improves the service life of the anion releasing head.
2. Ozone and nitrogen oxides (NO and NO)2) Release amount test
1) Testing instrument
Nitrogen oxide tester-manufacturer: polyclone; the instrument model is as follows: WSQ-NOX;
ozone tester-manufacturer: polyclone; the instrument model is as follows: WSQ-O3.
2) Test conditions
Temperature: 18 deg.C
Relative humidity: 18 percent of
PM2.5：30μg/m2
Output voltage connected to one end of the metal rod: 40 kV.
3) Test procedure
A tester holds a nitrogen oxide tester or an ozone tester by hands, respectively stands in the positions which are respectively in the positive front, the left side and the right side of the negative ion release head to be tested and are respectively 2 m and 4m away from the negative ion release head in the direction of 22.5 degrees, and tests the concentration of ozone and nitrogen oxide released by the negative ion release head to be tested.
4) Test results
After the anion releasing heads of each example and comparative example were prepared, the use was continued for 10 hours, and then the test was performed. Ozone and nitrogen oxide release amounts (NO and NO) of anion releasing heads of examples and comparative examples2Total amount released) the test results are shown in table 2.
TABLE 2
As can be seen from table 2, the composite negative ion emitting head of the example of the present invention did not emit nitrogen oxide and the amount of ozone emitted was reduced relative to the negative ion emitting head of the comparative example, as compared to the fullerene negative ion emitting head of the comparative example.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (11)
1. A composite anion release head, comprising: the titanium dioxide nanotube array comprises a plurality of titanium dioxide nanotubes, the plurality of titanium dioxide nanotubes are formed on the conductive metal wire, and the fullerene layer is formed on the part of the conductive metal wire, which is not covered by the titanium dioxide nanotube array, and the titanium dioxide nanotube array.
2. The composite negative ion release head of claim 1, wherein the mass ratio of the titanium dioxide nanotube array to the fullerene layer is 0.1 to 1:1, optionally 0.1 to 0.5: 1; and/or
The thickness of the fullerene layer is 2-10 nm; and/or
The conductive metal wire is a titanium wire, a molybdenum wire, a tungsten wire or an iron wire.
3. A method of making a composite negative ion release head, the method comprising:
forming a titanium dioxide nanotube array on the conductive metal wire; and
and forming a fullerene layer on the part of the conductive metal wire which is not covered by the titanium dioxide nanotube array and the titanium dioxide nanotube array.
4. The method of claim 3, wherein the forming a titanium dioxide nanotube array on a conductive wire comprises:
forming a titanium film on the conductive wire; and
and annealing the titanium film to form a titanium dioxide nanotube array.
5. The method of claim 4, wherein the titanium film is formed on the conductive wire by electron beam evaporation, optionally wherein the electron beam evaporation comprises a chamber vacuum of 1 × 10-8～5×10-8Torr, controlling the thickness of the titanium film to be 100-300 nm; and/or
The conditions of the annealing treatment include: the annealing temperature is 350-600 ℃, and optionally, the annealing temperature is 450-500 ℃; the annealing time is 1 to 5 hours, optionally 2 to 3 hours.
6. The method of claim 3, further comprising: prior to forming the array of titanium dioxide nanotubes on the conductive wire,
cleaning and drying the conductive wire; and
and (4) removing impurities from the surface of the dried conductive metal wire by using acid liquor.
7. The method of claim 6, wherein the washing and drying the conductive wire comprises: sequentially carrying out ultrasonic cleaning in acetone, absolute ethyl alcohol and deionized water, and then blowing the ultrasonically cleaned conductive metal wire by using nitrogen;
optionally, the acid solution is an HF solution.
8. The method of claim 6, further comprising: after the cleaning and drying of the conductive wire, before the impurity removing process,
plating a transition metal layer on the dried conductive metal wire;
optionally, the transition metal layer is an aluminum layer or a molybdenum layer, and the thickness of the transition metal layer is 0.5-2.5 μm.
9. The method of any of claims 3-8, wherein the forming a fullerene layer on the portion of the conductive wire not covered by the array of titanium dioxide nanotubes and the array of titanium dioxide nanotubes comprises:
dispersing fullerene in water to form a stable suspension;
putting the conductive metal wire with the titanium dioxide nanotube array into the suspension, and forming a fullerene layer on the part of the conductive metal wire which is not covered by the titanium dioxide nanotube array and the titanium dioxide nanotube array by adopting a vertical deposition method to obtain a negative ion release head; and
and taking the negative ion release head out of the suspension and drying.
10. The method of claim 9, wherein forming a stable suspension comprises:
crushing fullerene;
mixing the pulverized fullerene with water in a container, and ultrasonically dispersing until no fullerene is attached to the surface of the container and the solution in the container is not layered; optionally, the concentration of the fullerene in the suspension is 0.1-1 g/L; and/or
The conditions of the vertical deposition method include: the temperature is 50-120 ℃, and optionally, the temperature is 60-100 ℃; the time is 15 to 31 hours, optionally 16 to 30 hours.
11. An anion generating electrode, characterized in that, the anion generating electrode comprises a metal rod, a conductive fixing device and an anion releasing head, the anion releasing head is fixed on the metal rod through the conductive fixing device, and the anion releasing head is electrically connected with the metal rod, the anion releasing head is the composite material anion releasing head of claim 1 or 2 or the composite material anion releasing head prepared by the method of any one of claims 3 to 10.
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| CN109494010A (en) * | 2018-12-14 | 2019-03-19 | 张桂林 | A kind of anion superconductor, reaction film and negative ion generating device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2524406Y (en) * | 2001-12-30 | 2002-12-04 | 西安交通大学 | Negative ion generator for growing nano carbon tube array on discharge terminal |
| CN203071402U (en) * | 2012-12-05 | 2013-07-17 | 马骧彬 | Multi-polar type oxygen anion combination electrode and oxygen anion generator thereof |
| CN205265040U (en) * | 2015-12-03 | 2016-05-25 | 刘延兵 | Positive and negative ions emitter |
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