CN115029664A - Preparation method of photo-thermal film material with broad-spectrum antibacterial property - Google Patents

Preparation method of photo-thermal film material with broad-spectrum antibacterial property Download PDF

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CN115029664A
CN115029664A CN202210827952.5A CN202210827952A CN115029664A CN 115029664 A CN115029664 A CN 115029664A CN 202210827952 A CN202210827952 A CN 202210827952A CN 115029664 A CN115029664 A CN 115029664A
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sputtering
film material
copper
power supply
photothermal
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邓乔元
林新凯
李世洋
文峰
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Hainan University
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Hainan University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/354—Introduction of auxiliary energy into the plasma
    • G—PHYSICS
    • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
    • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
    • G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/40—Solar thermal energy, e.g. solar towers

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Abstract

The invention discloses a preparation method of a photo-thermal film material with broad-spectrum antibacterial property on a screen of electronic display equipment, which forms a titanium nitride/copper composite film material on the surface of a base material to ensure that TiN-Cu X The film has good photo-thermal antibacterial performance on electronic screens of mobile phones and the like, and the obtained TiN-Cu X The film has good photo-thermal sterilization performance under the condition of visible light, good abrasion resistance and excellent blue light filtering effect. Under normal natural light conditions, the TiN has good photo-thermal property, the addition of the Cu element enhances the photo-thermal effect of the TiN, and the TiN-Cu enhances the photo-thermal effect X The photothermal effect of the film can effectively improve the antibacterial property of the material, so that the surface of the electronic screen is kept clean, the process is simple and stable, environment-friendly and energy-saving, and the plated film layer conforms to the EUThe ROHS standard.

Description

Preparation method of photo-thermal film material with broad-spectrum antibacterial property
Technical Field
The invention relates to the technical field of material surface treatment, in particular to a preparation method of a photothermal thin film material with broad-spectrum antibacterial property.
Background
With the advent of touch screen technology and the increasing availability and use of touch screen technology, the antimicrobial properties of screens have also drawn considerable attention and researchers are beginning to consider the potential of these touch screen surfaces as nosocomial pathogen repositories. Recent studies have investigated patients and staff in hospital environments and recovered microorganisms from Mobile devices [ R.R. Brady, et al, Mobile phone technology and related substrates: a cross-sectional cultural study of bacterial microbial contamination, and substrate options and bearings, Clin.Microbiol. Infect.17(6) (2011) 830-835 ]. A review shows that during 2005 to 2009 all studies in this field reported microbial contamination of the devices, with up to 40% of the study devices presenting staphylococcus aureus, a clinically significant microbe in nosocomial infections [ u. Clearly, there is increasing evidence that the mobile device screen may be a reservoir for nosocomial pathogens. Although the healthcare professional under investigation is aware of this, 78% recognize the problem, only 8% acknowledge that the device was cleaned. Cleaning protocols such as 70% isopropyl alcohol wipes, bleach, and even simple wet microfiber cloths have proven effective in reducing the microbial load on the device display, and in some cases, below the detection limit, but have little use if the health care provider's cleaning compliance is poor. In the general public's mobile device users, cleaning compliance may be even lower than that of medical professionals. It would be advantageous to help reduce microbial contamination of the device screen, thereby reducing its usefulness as a pathogenic microbe, a self-disinfecting screen that requires little or no user compliance. Researchers have employed a layer of Light-activated antimicrobial protectant to coat the surface of mobile devices to reduce the contamination of electronic device screens by microorganisms [ Kristacher Page, Annapula Correia, Michael Wilson b, Elaine Allan, Ivan P. Parkin, Light-activated antimicrobial screens for mobile telephone and tablet computers, Journal of Photochemistry and Photobiology A: Chemistry 296(2015) 19-24 ].
In addition, electronic devices such as computers and mobile phones are ubiquitous in modern society, and are an essential part of daily life. Up to 69% of computer users report eye strain, termed "Computer Vision Syndrome (CVS)". CVS refers to a set of eye and vision related problems due to long term use of electronic devices. The most common symptoms of CVS are blurred vision, dry eyes, redness and headaches [ LeBlanc AG, Guinell KE, Prince SA, Saunders TJ, Barnes JD, Chaput JP. the below of the screen: an overview of the scales and bones of the screen time in outer model of the clinical Journal of the American College of Sports medicine.9.2017; (17) 104-. Recently, more and more patients with symptoms of CVS have appeared in ophthalmology. It is estimated that CVS will affect 6000 million people worldwide, finding 100 million new cases per year [ Heus P, verbek JH, Tikka c. optical correction of removable error for predicting and treating eye systems in computers users. cobalt Database system rev.2018; 4(4).
CVS is most likely caused by blue light emitted from electronic screens such as computers and mobile phones, and various professional ophthalmic lenses for reducing transmission of blue light to eyes are also sold in the market to reduce eye fatigue in computer use [ Singh S, Anderson AJ, down le. instruments international optometers' knowledge and attude towards describing blue light-blocking ophthalmic device. opthalmic physical op.2019; 39(3) 194-204).
Therefore, a technical problem to be solved by those skilled in the art is how to provide a method for preparing a photo-thermal film material having broad-spectrum antibacterial property on the screen of electronic equipment such as mobile phones.
Disclosure of Invention
In view of this, the present invention provides a method for preparing a photothermal thin film material with broad-spectrum antibacterial properties. The photo-thermal film material which can be firmly combined with the surface of a substrate such as an electronic screen and the like, has broad-spectrum antibacterial property and good blue light prevention performance and wear resistance is prepared by magnetron sputtering, so that the microbial pollution of the screen of equipment and the visual fatigue caused by blue light are obviously reduced, the wear resistance is improved, and the service life is prolonged.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a photo-thermal film material with broad-spectrum antibacterial property forms a titanium nitride/copper composite film material on the surface of a substrate material, so that a TiN-Cux film has good photo-thermal antibacterial property on an electronic screen of a mobile phone and the like, and specifically comprises the following preparation steps:
A. ultrasonic cleaning the base material, vacuum pumping in a magnetron sputtering apparatus until the vacuum degree reaches 3 × 10 -3 Introducing argon below Pa, adjusting the partial pressure of the argon to 3.0-5.0 Pa, starting a substrate bias source to adjust the substrate bias voltage to generate glow discharge to form plasma, cleaning the surface of the metal substrate for 20min by the plasma, closing a bias power supply, adjusting the vacuum pressure to 0.5Pa, starting a sputtering power supply, carrying out sputtering cleaning and sputtering on the copper target and the titanium target for 5min, and closing the sputtering power supply;
B. and (3) after the sputtering power supply is closed, introducing nitrogen, adjusting the proportion of the nitrogen and the argon in the A to ensure that the vacuum pressure is stabilized at 0.5Pa, applying a bias voltage of-50V on the base material treated by the A, starting the sputtering power supply, sputtering the copper target by using a high-power pulse magnetron sputtering power supply, then sputtering the titanium target by using a constant current of a direct current power supply, and preparing a target product on the surface of the base material, wherein the TiN film material is doped with metallic copper.
The photo-thermal film material with broad-spectrum antibacterial property is prepared, certain blue light resistance and wear resistance are added, and a certain content of metal copper element is doped in the film. The copper element also has good photo-thermal property, and the addition of the copper can improve the photo-thermal effect of the TiN film, thereby improving the broad-spectrum antibacterial property of the photo-thermal film material. In addition, in the service process of the titanium nitride film material (TiN-Cux) on electronic equipment such as a mobile phone, a tablet personal computer and the like, metal copper ions are released, and the surfaces of the copper ions can also directly interact with the outer bacterial membrane to break the outer bacterial membrane; the TiN-Cux composite film has higher absorption rate to blue light (between the wavelength of 435-. Titanium nitride can be used as a ceramic material with good wear resistance due to the characteristics of high hardness, good chemical stability and the like, and the film surface can be golden yellow and can be widely subjected to surface modification so as to improve the long-term stability and service life of the material.
Preferably, the ultrasonic cleaning in step a is ultrasonic cleaning in acetone and ethanol for 10min respectively.
The preferable beneficial effects are that a layer of colloid is attached to the surface of the 304 stainless steel substrate material, the colloid is dissolved and removed by washing with acetone for 10min, the acetone and stains (such as residual colloid, dust, grease and the like) on the surface of the 304 stainless steel are washed away by washing with ethanol for 10min, and the ethanol is easy to clean, can be volatilized quickly and is not easy to leave stains.
Preferably, the vacuum pumping in step a is performed by using a mechanical pump or a molecular pump.
The preferred advantage of the above is that the main function of the mechanical pump is to provide the necessary forevacuum for the start-up of the (turbo) molecular pump. The main function of the molecular pump is to provide and maintain the vacuum degree of the experiment. The combined use of mechanical and molecular pumps greatly facilitates the maintenance and operating specifications of mechanical equipment.
Preferably, the substrate bias voltage is adjusted in step A to apply a negative DC bias voltage of-600V to the surface of the substrate material.
The preferable beneficial effect is that the substrate is given a certain negative bias voltage so that the argon ions can thoroughly carry out sputtering cleaning on the substrate, and under certain conditions, the higher the negative bias voltage is, the more thorough the sputtering cleaning is.
Preferably, the sputtering power supply current in the step A is 0.3A.
The preferable beneficial effects are that in the step A, a (constant current) direct current magnetron sputtering power supply of 0.3A is adopted when the titanium target material is cleaned, and the magnetron sputtering power cannot exceed 7W/cm 2 Too high sputtering power can break down the melting target material, and too low sputtering power can cause the problems of incomplete sputtering cleaning, low deposition efficiency, incompact film combination and the like. Selecting proper target material according to the size of the target material in the laboratoryThe current of (2) was 0.3A.
Preferably, in the step B, when the high-power pulse magnetron sputtering power supply is used for sputtering the copper target, the power supply voltage is-500-600V, and the average power is 1-2W/cm 2 The operation can regulate and control the copper doping amount and the size of copper crystal grains in the film, and realize good photo-thermal property
The optimized high-power pulse power supply has the beneficial effects that the copper doping amount and the grain size of copper in the film are regulated and controlled by controlling the voltage change (500V/550V/600V) of the high-power pulse power supply, and the grain size of the copper is 1-2W/cm 2 The average power of the high-power pulse power supply can enable copper elements to be uniformly doped, 500-600V is the most stable current/voltage ratio interval of the high-power pulse power supply, the stable current/voltage ratio can well control the grain size of copper, and uniform grains can be obtained.
Preferably, in the step B, during the sputtering of the titanium target by using the constant current of the direct current power supply, the constant current is kept at 0.3A, and the average sputtering power is 3W/cm 2 The operation can regulate and control the internal thickness of the film to improve the photo-thermal effect of the TiN.
The preferable beneficial effects are that in the process of depositing the TiCuN film, the constant current of 0.3A is adopted, so that on one hand, the normal work of the target can be ensured, on the other hand, the stable sputtering power can be provided, and the average sputtering power is 3W/cm 2 The thickness of the lower film is uniform and moderate, and the contribution to the photothermal effect is the largest.
Preferably, the doping amount of the metallic copper in the metallic copper doped TiN thin film material in the step B is 20-50%.
The copper doping amount of 20-50% is determined by the voltage and deposition time of a high-power pulse magnetron sputtering power supply, and the photo-thermal property of TiN can be well improved by doping 20-50% of copper.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
firstly, in the preparation process of the photo-thermal film, the photo-thermal film is prepared by adopting a composite high-power pulse magnetron sputtering technology of high-power magnetron sputtering and direct-current magnetron sputtering in parallel, wherein the deposition of a copper element adopts a high-power pulse magnetron sputtering method, and the release deposition of a titanium element adopts a conventional direct-current (constant-current) magnetron sputtering method. Compared with the traditional direct current magnetron sputtering technology, the composite high-power pulse magnetron sputtering method can control the grain size of the deposited copper element, so that the film is more compact, and the photothermal effect of the film is improved.
And secondly, compared with the traditional direct-current magnetron sputtering technology, the film prepared by adopting the composite high-power pulse magnetron sputtering technology has the advantages that the surface of the film is smoother, the average roughness is reduced by 1.32nm, the adhesive force of the deposited film is improved, the mechanical property is more excellent, and the hardness is improved by 2.68GPa under the condition of the same target average power.
And compared with the traditional silver/copper ion doped antibacterial film, the photothermal antibacterial film has better timeliness and permanence, the main mechanism of silver/copper ion doped antibacterial film is that the cell membrane of bacteria is damaged through ion release to cause cell deterioration, the timeliness of the silver/copper ion doped film depends on the amount and release speed of silver/copper ions, the silver/copper ion doped film can be invalid after a certain time, but the photothermal effect of the photothermal film has permanence, and the antibacterial rate can reach 99.9%.
And fourthly, the titanium nitride film material (TiN-Cux) doped with the metal copper improves the photo-thermal property of the titanium nitride through the photo-thermal effect (converting light energy into heat energy) of the nano titanium nitride and the addition of the metal copper, so that the local temperature of the film is increased, the bacterial cell membrane can be damaged, and the protein denaturation is caused, thereby achieving the effects of resisting bacteria and inhibiting microbial pollution.
And fifthly, the titanium nitride film in the film material can also be used as a ceramic material, and has the advantages of high hardness, good chemical stability, good wear resistance, golden color of the film and the like, so that the titanium nitride film can be widely used for surface modification and modification to enhance the wear resistance of the surface of the material and prolong the service life of the material.
Sixthly, the absorption rate of the film material to blue light is excellent, the effect of preventing the blue light and reducing eye visual fatigue can be effectively achieved, wherein the absorption rate of titanium nitride to the blue light can reach more than 90%, and human eyes can be well protected from being damaged by the blue light.
And seventh, the novel titanium nitride thin film material (TiN-Cux) can deposit the surfaces of different materials, such as quartz glass, silicon wafers, 304 stainless steel, ceramics and the like.
Eighthly, the atomic concentration of the doped metal copper element of the film material can be controlled between 20% and 50% according to the service condition.
The plasma surface modification method belongs to low-temperature plasma treatment, and has the advantages of simple preparation process, environmental protection, low cost, rich applicable material types and difficult deformation of a matrix.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic diagram of a magnetron sputtering apparatus;
FIG. 2 is a schematic diagram of limiting temperature rise of a photothermal film;
FIG. 3 is a schematic view of a cyclic heating of a photothermal film;
FIG. 4 shows the antibacterial effect of the photothermal film against Staphylococcus aureus (a-c are diluted 10-3, 10-6, 10-9 times, respectively, and d-f are bacterial colonies on the surface of the photothermal film under an electron microscope);
FIG. 5 is a graph showing the absorbance of a photothermal film;
FIG. 6 is a graph of coefficient of friction for different photothermal films.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
A. Cleaning the surfaces of the substrate and the target material:respectively ultrasonically cleaning the workpiece in acetone and ethanol for 10 minutes, and then drying the workpiece in the air for later use; fixing the substrate on a metal substrate, placing in a vacuum chamber of a magnetron sputtering device, and pumping vacuum to 3 × 10 by a mechanical pump and a molecular pump -3 Introducing argon into the vacuum chamber to make the air pressure of the vacuum chamber be 3.0Pa, applying-600V direct current negative bias on the surface of the substrate to make the argon generate glow discharge, forming plasma and carrying out sputtering cleaning on the surface of the substrate for 20 minutes, then closing the bias power supply, adjusting the gate valve to further adjust the air pressure of the vacuum chamber to be 0.5Pa, applying 0.3A current on the target material, cleaning the copper target and the titanium target for 5 minutes, and then closing the bias power supply.
B. Introducing nitrogen into a vacuum chamber, adjusting the flow ratio of the nitrogen to the argon, adjusting the air pressure of the vacuum chamber to 0.5Pa, then starting a sputtering power supply, respectively applying voltage on the surfaces of a copper target and a metal target material, wherein the sputtering bias voltage of the copper target is-500V, the titanium target adopts direct current sputtering, the constant current is set to 0.3A, and the sputtering average power of the copper target is 1-2W/cm 2 The average power of sputtering on the titanium target was 3W/cm 2 The titanium nitride film material (TiN-Cux) doped with metallic copper is prepared, and the atomic percentage of the metallic copper element is 20 percent.
Example 2
A. Cleaning the surfaces of the substrate and the target material: respectively ultrasonically cleaning the workpiece in acetone and ethanol for 10 minutes, and then drying the workpiece in the air for later use; fixing the substrate on a metal substrate, placing in a vacuum chamber of a magnetron sputtering device, and pumping vacuum to 3 × 10 by a mechanical pump and a molecular pump -3 Introducing argon into a vacuum chamber with the pressure of 3.0Pa, applying a direct current negative bias of-600V on the surface of the substrate to generate glow discharge for the argon, forming plasma, performing sputtering cleaning on the surface of the substrate for 20 minutes, then closing a bias power supply, and closing the argon: argon gas was introduced into the vacuum chamber to make the pressure in the vacuum chamber 0.5Pa, 0.3A current was applied to the target material, and sputtering cleaning was performed for 5 minutes for the copper target and the titanium target, after which the bias power supply was turned off.
B. Closing argon, introducing nitrogen into the vacuum chamber to make the pressure of the vacuum chamber be 0.5Pa, and then opening the sputtering deviceThe power supply applies voltage to the surfaces of the copper target and the metal target respectively, the sputtering bias voltage of the copper target is-550V, the titanium target adopts direct current sputtering, the constant current is set to be 0.3A, and the sputtering average power of the copper target is 1-2W/cm 2 The average power of sputtering on the titanium target was 3W/cm 2 And preparing the titanium nitride film material (TiN-Cux) doped with the metallic copper, wherein the atomic percent of the metallic copper element is 30 percent.
Example 3
A. Cleaning the surfaces of the substrate and the target material: respectively ultrasonically cleaning the workpiece in acetone and ethanol for 10 minutes, and then drying in the air for later use; fixing the substrate on a metal substrate, placing in a vacuum chamber of a magnetron sputtering device, and pumping vacuum to 3 × 10 by a mechanical pump and a molecular pump -3 Introducing argon into a vacuum chamber with the pressure of 3.0Pa, applying a direct current negative bias of-600V on the surface of the substrate to generate glow discharge for the argon, forming plasma, performing sputtering cleaning on the surface of the substrate for 20 minutes, then closing a bias power supply, and closing the argon: argon gas was introduced into the vacuum chamber to make the pressure in the vacuum chamber 0.5Pa, a current of 0.3A was applied to the target material, and sputtering cleaning was performed for 5 minutes for the copper target and the titanium target, after which the bias power supply was turned off. B. Closing argon, introducing nitrogen into the vacuum chamber to enable the air pressure of the vacuum chamber to be 0.5Pa, then starting a sputtering power supply, respectively applying voltage on the surfaces of the copper target and the metal target material, wherein the sputtering bias voltage of the copper target is-600V, the titanium target adopts direct current sputtering, the constant current is set to be 0.3A, and the sputtering average power of the copper target is 1-2W/cm 2 The average power of sputtering on the titanium target was 3W/cm 2 And preparing the titanium nitride film material (TiN-Cux) doped with the metallic copper, wherein the atomic percent of the metallic copper element is 50 percent.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (8)

1. A preparation method of a photothermal thin film material with broad-spectrum antibacterial property is characterized in that a titanium nitride/copper composite thin film material is formed on the surface of a base material, and specifically comprises the following preparation steps:
A. ultrasonic cleaning the base material, vacuum pumping in magnetically controlled sputtering apparatus to vacuum degree of 3 x 10 -3 Introducing argon below Pa, adjusting the partial pressure of the argon to 3.0-5.0 Pa, starting a substrate bias source to adjust the substrate bias voltage to generate glow discharge to form plasma, cleaning the surface of the metal substrate for 20min by the plasma, closing a bias power supply, adjusting the vacuum pressure to 0.5Pa, starting a sputtering power supply, carrying out sputtering cleaning and sputtering on the copper target and the titanium target for 5min, and closing the sputtering power supply;
B. and (3) after the sputtering power supply is closed, introducing nitrogen, adjusting the proportion of the nitrogen and the argon in the A to ensure that the vacuum pressure is stabilized at 0.5Pa, applying a bias voltage of-50V on the base material treated by the A, starting the sputtering power supply, sputtering the copper target by using a high-power pulse magnetron sputtering power supply, then sputtering the titanium target by using a constant current of a direct current power supply, and preparing a target product on the surface of the base material, wherein the TiN film material is doped with metallic copper.
2. The method for preparing the photothermal thin film material with broad-spectrum antibacterial activity according to claim 1, wherein the ultrasonic cleaning in step a is ultrasonic cleaning in acetone and ethanol for 10min respectively.
3. The method for preparing the photothermal thin film material with a broad spectrum antibacterial property of claim 1, wherein the step a is performed by a mechanical pump or a molecular pump.
4. The method for preparing a photothermal thin film material having a broad spectrum antibacterial activity according to claim 1, wherein the substrate bias voltage is adjusted in step a to apply a negative dc bias voltage of-600V to the surface of the substrate material.
5. The method for preparing the photothermal thin film material with broad spectrum antibacterial activity of claim 1 wherein the sputtering power current of the titanium target in step A is 0.3A.
6. The method for preparing the photothermal thin film material with broad-spectrum antibacterial activity according to claim 1, wherein in the step B, the high-power pulse magnetron sputtering power source is used for sputtering the copper target, the power voltage is-500-600V, and the average power is 1-2W/cm 2 。
7. The method for preparing the photothermal thin film material with the broad spectrum antibacterial property of claim 1, wherein in the step B, the titanium target is sputtered by the constant current of the direct current power supply, the constant current is maintained at 0.3A, and the average sputtering power is 3W/cm 2 。
8. The method for preparing the photothermal thin film material with broad spectrum antibacterial activity as claimed in claim 1, wherein the amount of copper doped in the copper-doped TiN thin film material in step B is 20-50%.
CN202210827952.5A 2022-07-13 2022-07-13 Preparation method of photo-thermal film material with broad-spectrum antibacterial property Pending CN115029664A (en)

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