CN115350295B - Deep ultraviolet LED photocatalyst module and preparation method thereof - Google Patents
Deep ultraviolet LED photocatalyst module and preparation method thereof Download PDFInfo
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- 229910010413 TiO 2 Inorganic materials 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 2
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
- A61L2/08—Radiation
- A61L2/10—Ultraviolet radiation
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/26—Accessories or devices or components used for biocidal treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B82Y40/00—Manufacture or treatment of nanostructures
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2101/00—Chemical composition of materials used in disinfecting, sterilising or deodorising
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Abstract
The invention provides a deep ultraviolet LED photocatalyst module and a preparation method thereof, which belong to the technical field of ultraviolet LEDs and comprise a sapphire substrate, wherein the sapphire substrate comprises a group of opposite etching surfaces, and a plurality of pyramids are arranged on the etching surfaces; the etching surface is also provided with a photocatalyst nanowire array film. According to the invention, the sapphire substrate with good light transmittance on the front surface and the side surface is selected as the photocatalyst carrier; the specific surface area of the photocatalyst is increased through the photocatalyst nano arrays on the two sides of the sapphire substrate; light is reflected and refracted through the double-sided pyramid, light enters the sapphire substrate from the side surface, the light passes through the refraction and reflection process and achieves the photocatalysis effect of the bottom, active points are added on the contact surface of the sapphire substrate, so that the light energy extraction rate is effectively increased, the sterilization effect is improved, the binding force of the photocatalyst and the sapphire substrate is improved, and the service life is prolonged.
Description
Technical Field
The invention relates to the technical field of ultraviolet LEDs, in particular to a deep ultraviolet LED photocatalyst module and a preparation method thereof.
Background
In recent years, the ultraviolet LED has become a research and development focus due to the advantages of low heat productivity, no heat radiation, higher safety and the like, and is widely applied to the fields of resin curing, anti-counterfeiting identification, printing ink, sterilization, medical health and the like.
When the luminous wavelength of the LED is less than 300nm, the LED is called a deep ultraviolet LED, and the deep ultraviolet light belongs to short-wave light, so that the sterilization effect is good, the light source of the deep ultraviolet LED is stable, instant starting, no stimulation and the like, and the environmental or human injury caused by modes such as mercury lamp sterilization, chemical sterilization, radiation sterilization and the like is overcome.
However, the shorter wavelength leads to faster attenuation of deep ultraviolet light energy, so that the sterilization distance of the deep ultraviolet LED is limited, generally, sterilization can only be performed in a range within a range of ten centimeters from the surface of the LED, and the high polymer has weaker deep ultraviolet oxidation resistance, and easily leads to falling of photocatalytic particles, so that the photocatalytic effect is reduced.
In the prior art, a photocatalyst carrier is added, a photocatalyst material is introduced, and the photocatalytic effect is improved through photocatalyst, but the traditional photocatalyst carrier usually adopts ceramic, asbestos and metal mesh as the photocatalyst carrier, the inside of the material does not have light transmittance, and a light source irradiates the surface of the carrier to be absorbed, so that light reflection and refraction cannot be generated; if the conventional glass is used as the substrate, the glass has higher blocking degree to deep ultraviolet rays.
Besides the defects of the existing photocatalyst carrier, the photocatalyst and the carrier have the problem of insufficient binding force, the photocatalyst is easy to fall off and layer on the surface of the base material, the final sterilization effect of the ultraviolet LED is not ideal, and breakthrough is difficult to obtain.
For example:
CN105987443B adopts TiO 2 The particles are covered on the porous ceramic substrate for use, and the porous ceramic substrate is coated with TiO 2 The relation between the calcination temperature and the performance is compared. But in view of the particulate TiO 2 Has low specific surface area, and does not consider photocatalyst TiO 2 The morphology of the carrier and the influence of the carrier on the catalytic effect, so the ultraviolet light utilization efficiency of the invention is to be improved, and the filled TiO is 2 The particles are easy to fall off in the using process.
CN110280274A is CdS-WS2-TiO 2 ArrayThe optical fiber bundle composite material realizes the promotion of the photocatalytic active point and widens the utilization rate of spectrum. But the optical fiber has small and brittle cross-sectional area, lacks certain laying tension, is easy to break and is inconvenient for later maintenance. In addition, the light source is arranged in the air, the inside of the optical fiber and the TiO by means of refraction 2 The transfer of energy, either limited energy into the fiber, or some of the energy transferred into the fiber, does not promote the photocatalytic process (since the fiber carrier itself is not a photocatalytic material) when the fiber is internally reflective to the light being consumed.
Disclosure of Invention
The invention provides a deep ultraviolet LED photocatalyst module and a preparation method thereof, which can improve the sterilization effect of a deep ultraviolet LED.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the deep ultraviolet LED photocatalyst module comprises a sapphire substrate, wherein the sapphire substrate comprises a group of opposite etching surfaces, and a plurality of pyramids are arranged on the etching surfaces; the etching surface is also provided with a photocatalyst nanowire array film. The sapphire substrate with good light transmittance on the front surface and the side surface is selected as a photocatalyst carrier; the specific surface area of the photocatalyst is increased through the photocatalyst nano arrays on the two sides of the sapphire substrate; light is refracted and refracted through the double-sided pyramid, and active points are added on the contact surface of the sapphire substrate, so that the light energy extraction rate is effectively increased, and the sterilization effect is improved.
Further, the pyramids are regularly arranged.
Further, the diameter of the photocatalyst nanowire in the photocatalyst nanowire array film is 5 nm-20 nm, and the length is 1-10 um; number of photocatalyst nanowires per square centimeter of area: 10 3 ～10 7 。
The preparation method of the deep ultraviolet LED photocatalyst module comprises the following steps: providing a sapphire substrate; etching a plurality of pyramids which are regularly arranged on a group of opposite surfaces of the sapphire substrate to form etching surfaces; and growing a photocatalyst nanowire array film on the etching surface.
Further, a photocatalyst nanowire array film is grown on the etching surface in situ through a liquid phase method.
Drawings
The invention and its features, aspects and advantages will become more apparent from the detailed description of non-limiting embodiments with reference to the following drawings. Like numbers refer to like parts throughout. The drawings are not intended to be drawn to scale, emphasis instead being placed upon illustrating the principles of the invention.
FIG. 1 is a schematic cross-sectional view of an etched pyramid on a sapphire substrate provided by the present invention;
FIG. 2 is a schematic perspective view of an etched pyramid on a sapphire substrate provided by the present invention;
FIG. 3 is a schematic diagram of refraction and active point generation of deep ultraviolet light irradiated on a deep ultraviolet LED photocatalyst module;
FIG. 4 is a schematic structural diagram of a deep ultraviolet LED photocatalyst module with deep ultraviolet LED irradiation according to the present invention;
fig. 5 is a schematic structural diagram of a deep ultraviolet LED photocatalyst module irradiated by a deep ultraviolet LED according to the present invention.
Detailed Description
The invention will now be further described with reference to the accompanying drawings and specific examples, which are not intended to limit the invention.
The low optical power density of the deep ultraviolet LED is caused by the characteristics of short wavelength, short transmission distance, rapid energy attenuation and the like of the deep ultraviolet light, so that the sterilization function of the deep ultraviolet is limited.
Therefore, the embodiment of the invention provides a deep ultraviolet LED photocatalyst module, as shown in fig. 1 to 5, which comprises a sapphire substrate 1, wherein the sapphire substrate 1 comprises a group of opposite etching surfaces, and a plurality of pyramids 2 are arranged on the etching surfaces; and the etching surface is also provided with a photocatalyst nanowire array film 3. The sapphire single crystal is used as an excellent wave-transmitting material and has good transmittance in ultraviolet, visible light, infrared wave bands and microwave wave bands, so that the sapphire substrate 1 is used as a photocatalyst carrier, and a certain part of photons totally reflected originally from the front surface can penetrate to the back surface of the device, so that the light extraction efficiency is improved to a certain extent; the etching surface of the sapphire substrate 1 is etched with a plurality of micro-scale or nano-scale pyramids 2, so that the combination capability of a photocatalyst and a photocatalyst carrier is increased, light refraction or refraction can be caused, photons emitted into the sapphire substrate 1 from the side surface become photocatalytic active sites on the contact surface of the photocatalyst nanowire array film 3 and the sapphire substrate 1, the active sites in unit area are obviously increased by the structure of the double-sided micro-nano pyramids 2 and the middle light-transmitting part of the sapphire substrate 1, as shown in fig. 3, the combination of photo-generated electrons and holes is obviously reduced, and the utilization rate of photo-generated electrons is further improved; the photocatalyst nanowire array film 3 is used for realizing the immobilization of the catalytic material, so that the aggregation of the photocatalyst is avoided, the specific surface area of the photocatalytic reaction is increased, and more active surfaces are provided for the photocatalytic reaction. Therefore, the deep ultraviolet LED photocatalyst structure effectively improves the sterilization function of the deep ultraviolet LED.
The pyramids 2 are regularly arranged, and the double-sided etched sapphire surface with a regular three-dimensional structure is beneficial to increasing the binding force of the photocatalyst and the sapphire substrate 1 and prolonging the service life of the photocatalytic material.
The diameter of the photocatalyst nanowire in the photocatalyst nanowire array film 3 is 5 nm-20 nm, and the length is 1-10 um; number of photocatalyst nanowires per square centimeter of area: 10 3 ～10 7 Of these, 10 is preferred 5 This arrangement mainly ensures that the density of the photocatalyst nanowire array film 3 is sufficient, but not too dense, so as to prevent too dense shielding light from irradiating the sapphire substrate 1.
Specifically, the material of the photocatalyst nanowire array film 3 can be TiO 2 ，TiO 2 The material of B, co, ni and the like can be doped simultaneously, and WO can be deposited alternatively 3 、Fe 2 O 3 Or SnO 2 And different photocatalyst materials. In this embodiment, tiO is specifically used 2 As a photocatalyst.
The invention also provides a preparation method of the deep ultraviolet LED photocatalyst module, which comprises the following steps: providing a sapphire substrate 1 as a photocatalyst carrier; double-sided etching is carried out on a group of opposite surfaces of the sapphire substrate 1, a plurality of pyramids 2 which are regularly arranged are etched, and etching surfaces are formed; the specific etching method comprises the following steps: selecting a mask with a conventional shape on the group of opposite surfaces for ICP etching, and establishing an ICP mask pattern process adjustment rule; calculating compensation parameters between the mask with the conventional shape and the mask with the target pyramid shape according to the established ICP mask pattern process adjustment rule and the parameter requirements of the mask with the target pyramid shape, wherein the compensation parameters comprise compensation quantity, compensation time and compensation shape; and designing and generating a mask conforming to the shape of the target prism based on the mask of the selected conventional shape according to the calculated compensation parameters.
Then in-situ growing a photocatalyst nanowire array film 3 on the etched surface by a liquid phase method, and using TiO 2 For example, the sapphire substrate is vertically placed in a tetrafluoro tank, hydrochloric acid and absolute ethyl alcohol are respectively added into the tetrafluoro tank for stirring, the hydrochloric acid is mainly used for inhibiting precipitation, then a certain amount of tetrabutyl titanate is gradually dripped in the stirring process, then the reaction kettle is transferred into an oven for reaction for 1-24 hours at 150-350 ℃, in this embodiment, the reaction is carried out for 6 hours at 120 ℃, and the reaction is taken out after cooling. Compared with the existing liquid phase method, the method is more favorable for growing a uniform photocatalyst nanowire array at a slow speed by utilizing the reaction condition of low temperature for a long time.
In practical application, the deep ultraviolet LED photocatalyst module is vertically arranged below two deep ultraviolet LEDs with 280nm wavelength, the wavelength of the deep ultraviolet LEDs is not limited to 280nm, and the number of the deep ultraviolet LEDs and the number of the photocatalyst modules can be adjusted according to practical requirements.
The module is placed in an experiment cabinet with the same closed space, the same strain concentration, the same temperature and the same humidity to test the photocatalysis effect, and the sample is sampled and tested after sterilization for 5 minutes. The invention adopts the deep ultraviolet LEDs with the same power as experiments, and the sterilization effects of the deep ultraviolet LEDs with different powers are greatly different under the influence of the power of the LEDs.
Experiment group 1 Using the sapphire substrate with the double-sided etching regular pyramid provided by the invention, tiO was deposited on the surface of the sapphire substrate 2 The nanowire film is irradiated by using a deep ultraviolet LED;
the control group 1 is directly irradiated by using a deep ultraviolet LED without adding a photocatalyst;
etching the sapphire surface of the control group 2 by using hydrofluoric acid, and depositing TiO on the surface of the sapphire substrate 2 The nanowire film is irradiated by using a deep ultraviolet LED;
control group 3 silica glass was surface etched with hydrofluoric acid to deposit TiO 2 The nanowire film was irradiated with deep ultraviolet LEDs.
The experimental results are as follows:
| sequence number | Pre-kill concentration (cfu/m) 3 ) | Post-consumer concentration (cfu/m) 3 ) | Killing rate% |
| Experiment group 1 | 4.3*10 6 | 3.5*10 5 | 91.86 |
| Control group 1 | 4.5*10 6 | 7.2*10 5 | 84.0 |
| Control group 2 | 4.3*10 6 | 4.6*10 5 | 89.3 |
| Control group 3 | 4.2*10 6 | 5.1*10 5 | 87.86 |
Therefore, the photocatalyst on the sapphire substrate of the double-sided etching regular pyramid provided by the invention can generate free radical active substances with extremely strong oxidation capability through photocatalytic oxidation reaction, and can effectively increase the decomposition speed of bacteria in unit time. Using a sapphire substrate and TiO 2 The composite catalyst formed at the interface does help to promote the photocatalytic effect.
The method for evaluating the binding capacity between the photocatalyst and the carrier comprises the following steps: the photocatalyst of the experiment group 1, the control group 2 and the control group 3 is placed in an ultrasonic machine to be subjected to ultrasonic treatment at a certain frequency for 30 seconds, and then the color change of the solution and the TiO on the surface of the carrier are compared 2 And (3) falling off. As a result, it was found that the solutions of control group 2 and control group 3 both exhibited slight milky white, and that control group 2 and control group 3 were not greatly different. Experiments prove that the TiO of the experimental group 2 The load is more firm.
In summary, in view of the fact that the irradiation area of deep ultraviolet rays is wired and the external quantum efficiency is low, the sapphire substrate with good light transmittance on the front surface and the side surface is selected as the photocatalyst carrier; the specific surface area of the photocatalyst is increased through the photocatalyst nano arrays on the two sides of the sapphire substrate; through double-sided pyramid photocatalyst and refraction of light, active points are added on the contact surface of the sapphire substrate, so that the light energy extraction rate is effectively increased, and the sterilization effect is improved.
The foregoing describes preferred embodiments of the present invention; it is to be understood that the invention is not limited to the specific embodiments described above, wherein devices and structures not described in detail are to be understood as being implemented in a manner common in the art; any person skilled in the art will make many possible variations and modifications, or adaptations to equivalent embodiments without departing from the technical solution of the present invention, which do not affect the essential content of the present invention; therefore, any simple modification, equivalent variation and modification of the above embodiments according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (3)
1. The deep ultraviolet LED photocatalyst module is characterized by comprising a sapphire substrate, wherein the sapphire substrate comprises a group of opposite etching surfaces, and a plurality of pyramids are arranged on the etching surfaces; the etching surface is also provided with photocatalyst nanowire array films which are uniformly distributed; a plurality of pyramids are regularly arranged;
the diameter of the photocatalyst nanowire in the photocatalyst nanowire array film is 5 nm-20 nm, and the length is 1-10 um; the number of the photocatalyst nanowires per square centimeter of area: 10 3 ～10 7 ；
Photons entering the sapphire substrate from the side face are refracted and refracted through the double-sided pyramid, and the contact surface of the photocatalyst nanowire array film and the sapphire substrate becomes an active point of photocatalysis.
2. The preparation method of the deep ultraviolet LED photocatalyst module is based on the deep ultraviolet LED photocatalyst module as claimed in claim 1, and is characterized by comprising the following steps:
providing a sapphire substrate;
etching a plurality of pyramids which are regularly arranged on a group of opposite surfaces of the sapphire substrate to form etched surfaces, wherein the method comprises the following steps of:
etching a group of opposite surfaces of the sapphire substrate through an ICP etching process based on a mask conforming to the target prismatic shape to form regularly arranged pyramids;
growing a photocatalyst nanowire array film on the etching surface; when the photocatalyst nanowire array film is made of TiO 2 The process is as follows:
and vertically placing the sapphire substrate in a tetrafluoro tank, respectively adding hydrochloric acid and absolute ethyl alcohol into the tetrafluoro tank for stirring, wherein the hydrochloric acid is mainly used for inhibiting precipitation, gradually dripping tetrabutyl titanate in the stirring process, transferring the reaction kettle into an oven for reaction for 1-24 hours at 150-350 ℃, and cooling and taking out.
3. The method for preparing the deep ultraviolet LED photocatalyst module according to claim 2, wherein the photocatalyst nanowire array film is grown on the etched surface in situ by a liquid phase method.
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| CN102597863A (en) * | 2009-08-31 | 2012-07-18 | 高丽大学校产学协力团 | Transparent structures |
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