CN114231966A - Cold spraying copper-containing stainless steel coating with antibacterial and antiviral functions - Google Patents
Cold spraying copper-containing stainless steel coating with antibacterial and antiviral functions Download PDFInfo
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Abstract
The invention aims to provide a cold spraying copper-containing stainless steel coating with antibacterial and antiviral functions and a preparation process thereof, which endow public facilities such as doorknobs, handrails or handrails in a public environment with effective inhibition effect on bacteria and viruses with higher concentration in the environment within 2 hours, and enable the antibacterial rate to reach 99.9% and the virus inhibition rate to reach more than 90% within 4 hours. The copper-containing stainless steel coating is prepared by mixing 304L stainless steel and pure Cu powder, and the cold spraying coating with long-acting antibacterial and antiviral functions is obtained by controlling the speed and time of powder mixing, the carrier gas temperature, the spraying distance, the spraying pressure and the powder feeding temperature of cold spraying. The cold spraying preparation process is simple and feasible, and is suitable for large-scale popularization of production lines. The corrosion resistance of the base material is greatly improved, and simultaneously, the attachment and the propagation of bacteria and viruses in a living environment can be fundamentally inhibited, and the propagation chain of microorganisms in a public area is fundamentally cut off.
Description
Technical Field
The invention belongs to the technical field of cold spraying coatings and preparation methods thereof, and particularly relates to a cold spraying copper (Cu) -containing stainless steel coating with antibacterial and antiviral functions and a preparation method thereof.
Background
In modern buildings and decoration, door handles or handrails are mostly made of zinc alloy and aluminum alloy, and the materials have the advantages of elegant appearance, firmness and durability. However, after the conventional door handle is used for a long time, various microorganisms (including bacteria and viruses) remain on the surface of the door handle, and even if the door handle is simply wiped, part of the bacteria and viruses cannot be removed, so that the problem of cross infection of subsequent users is caused. Contact of the hand with the mucosal tissue of the body, through surface to hand contact, forms an integral pathway for the transmission of bacteria and viruses. In addition, traditional door handle can produce the corrosion phenomenon after breeding the bacterium in humid air, and originally less pitting can stretch into the corrosion of large scale along with the continuous increase of degree of corrosion, has seriously influenced aluminum alloy, zinc alloy's use and decorative effect. Thus, improving or imparting anti-corrosion, anti-bacterial, and anti-viral functionality to a door handle would effectively reduce the health risks posed by touching the door handle or armrest and increase its durability in use.
Suitable surface treatment methods can impart biological functions not possessed by the base material, while maintaining the original physical properties of the base material. Since the 20 th century, Champagne and hellreitch prepared pure Cu coatings by cold spraying, so that the coatings have high-efficiency and excellent antibacterial performance, and discuss the difference of antibacterial performance of pure Cu coatings prepared by thermal spraying (plasma spraying and electric arc spraying) and cold spraying Cu coatings. Subsequently, Sundberg et al extended the original microbial range from bacteria to viruses, and found that both nano-scale and conventional cold-sprayed Cu coatings inhibited Influenza A virus (Influenza A) activity by 99.3%. However, while providing antibacterial and antiviral functions, the pure Cu cold spray coating cannot improve the corrosion resistance of the conventional door handle and ensure the aesthetic property of metallic silvery luster. Therefore, further improvements in the composition and preparation process of cold spray coatings are needed.
As is known, the stainless steel containing Cu is a novel stainless steel material with high corrosion resistance and broad-spectrum antibacterial performance, can inhibit the formation of bacterial biofilms and has good biocompatibility. The mode of action of the pure Cu cold spraying coating on microorganisms is the same, and the released Cu ions interact with the microorganisms, so that the activity of the coating is finally inhibited or killed. Therefore, the stainless steel containing Cu has excellent antibacterial function and potential antiviral function while ensuring the corrosion resistance of the base material. The ability of a Cu-containing stainless steel substrate to readily release Cu ions and to readily diffuse to microorganisms in contact with the surface determines the basis on which inhibition of microbial activity can be achieved.
Based on the background, the mature cold spraying technology is adopted to prepare the copper-containing stainless steel coating on the surface of the traditional door handle or handrail, so that the solubility limit of alloy elements in the smelting process can be broken, the expected components can be obtained by adjusting the element proportion in the powder, and the processing and forming process does not need to be considered. The corrosion resistance of the base material can be greatly improved, and simultaneously, the attachment and propagation of bacteria and viruses in the living environment can be fundamentally inhibited, and the propagation chain of microorganisms in a public area is fundamentally cut off.
Disclosure of Invention
In order to solve the technical problems, the invention provides a copper-containing stainless steel coating with antibacterial and antiviral functions and a cold spraying preparation method. The Cu-containing stainless steel cold spray coating can effectively and quickly inhibit high-concentration bacteria (1 x 10) in the environment5～2×105CFU/mL), high concentration of pathogenic virus (6X 10)6～7×106TCID50/mL), cutting the possibility of transmission of pathogenic microorganisms, significantly reducing the risk of bacterial and viral transmission during use of the door handle or armrest.
The invention prepares the copper-containing stainless steel coating on the surface of the door handle or the handrail prepared from the aluminum alloy and the zinc alloy by the cold spraying technology, so that the door handle or the handrail has quick and long-acting antibacterial and antiviral functions, and can be widely applied to public facilities containing pathogenic microorganism propagation.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the powder used for cold spraying the copper-containing stainless steel coating with the antibacterial and antiviral functions is composite powder formed by mixing 304L stainless steel and pure Cu spherical powder. Due to the density of pure Cu powder (8.96 g/cm)3) Density less than 304L stainless steel (7.93 g/cm)3) The difference of the kinetic energy obtained by the two powders is inevitably caused in the spraying process. Therefore, it is necessary to select the particle size distribution of each powder in the composite powder, which is an important factor for ensuring lower porosity and uniform distribution of Cu in the cold spray coating. The powder material selected by the invention has the particle size distribution D50 value of Cu spherical powder smaller than the D50 value of 304L stainless steel spherical powder, and the corresponding ratio of the sizes of the two is 0.50-0.90. The D50 value of the particle size distribution of 304L stainless steel spherical powder is 18.0-30.0 μm, the D50 value of the preferred spherical powder is 23.0-25.0 μm, the D50 value of the particle size distribution of Cu spherical powder is 10.0-22.0 μm, and the D50 value of the preferred spherical powder is 12.0-20.0 μm. In the mixed powder, the addition amount of pure Cu is 4.0-25.0% and the balance is 304L stainless steel powder; the preferable addition amount of pure Cu is 5.0-20.0%, and the balance is 304L stainless steel powder.
The invention adopts a cold spraying method to prepare the cold spraying copper-containing stainless steel coating with antibacterial and antiviral functions, which comprises the following specific steps:
1) powder mixing: weighing 304L stainless steel powder and pure Cu powder according to a proportion by adopting a mechanical mixing process, mixing the weighed powder and steel balls, putting the mixture into a mixing barrel, and uniformly mixing the mixture at a set speed and time parameter;
2) preparing a base material: before cold spraying treatment is carried out on a base material, the base material is subjected to surface oil removal by adopting a mixed solution of ethanol and acetone, the mixing ratio of the ethanol to the acetone is 1:1, and after oil removal is finished, sand blasting roughening treatment is carried out by adopting white corundum;
3) preparing a cold spraying coating: and putting the uniformly mixed powder into a powder feeder, setting appropriate process parameters, vertically fixing a spray gun on a support, and moving a sample on an X-Y two-dimensional motion platform relative to the spray gun to finish the preparation of the Cu-containing stainless steel cold spraying coating.
The composite powder is uniformly mixed by a mechanical mixer, the powder mixed according to the proportion is placed into a mixing barrel, steel balls with the diameter of 5mm are added into the barrel, a mixing bottle containing the powder and the steel balls is placed into the mixer to be uniformly mixed, the mixing speed is 25-50 r/min, the preferred mixing speed is 30-40 r/min, the mixing time is 3.0-6.0 hours, and the preferred mixing time is 4.0-5.0 hours.
A cold spray coating device for preparing copper-containing stainless steel coating comprises a control system, a powder feeder, a gas heater, a Laval nozzle and a powder heater. The cold spraying method for preparing the copper-containing stainless steel coating by using the cold spraying device has the technical parameters that: the heating temperature of the carrier gas is 200-. The preferred cold spraying process parameters are as follows: the heating temperature of the carrier gas is 300-700 ℃, the spraying distance is 15.0-25.0mm, the spraying pressure is 2.0-3.0MPa, and the powder feeding heating temperature is 300-500 ℃.
For preparing the cold spraying coating, the powder components and the cold spraying process are the key factors influencing the performance of the coating. In the invention, Cu is an important alloy element in the copper-containing stainless steel coating, and is a necessary condition for ensuring that the cold spray coating has quick and long-acting antibacterial and antiviral functions, the release of Cu ions can damage ribonucleic acid, nucleoprotein and membrane protein of microorganisms, and ROS generated in the release process of Cu ions can generate interaction with pathogenic microorganisms, so that the continuous growth of cells is inhibited, and the apoptosis of the cells is finally caused. According to the weight percentage, the addition amount of the Cu powder is 4.0-25.0%; preferably 5.0-20.0%, to ensure that the Cu ions are released continuously during the service process.
On the other hand, the coating prepared by the invention needs to ensure less defects and high quality, and needs a proper cold spraying device and a set of reasonable cold spraying process parameters. The cold spraying equipment adopted by the invention utilizes compressed air to send powder and accelerate the powder. The cold spray apparatus includes two heaters, the first of which is a carrier gas that heats the particles to increase their velocity, thereby increasing the kinetic energy of the particles to facilitate bonding to the substrate. The second is a powder feeding heater which is positioned between the powder feeder and the Laval nozzle, can directly heat the powder fed by the powder feeder, plays the roles of softening the powder and improving the plastic deformation capability of the powder, effectively reduces the defects of holes and the like in the coating and obviously improves the quality of the coating. The quality of the coating can regulate and control the corrosion resistance of the coating, and further can regulate and control the Cu ion release process of the cold spraying copper-containing stainless steel coating. In the present invention, the cold spray process parameters and preferred process parameters are as described above.
Therefore, the beneficial effects of the invention are as follows:
1. according to the invention, the composite powder containing Cu stainless steel is obtained by uniformly mixing 304L stainless steel powder and pure Cu powder, and the copper-containing stainless steel coating is prepared on the surface of the substrate by adopting a cold spraying process, so that the copper-containing stainless steel coating has quick and long-acting antibacterial and antiviral functions, and can cut off the propagation chain of pathogenic microorganisms in a short time.
2. The cold spraying device is simultaneously provided with the carrier gas heater and the powder feeding heater, and the carrier gas heater and the powder feeding heater can preheat powder and increase the kinetic energy of the powder; the copper-containing stainless steel coating can soften the powder sent out by the powder feeder, increase the plastic deformation capacity of the powder, obtain the copper-containing stainless steel coating with the powder compact and tightly combined with the matrix, regulate and control the corrosion resistance of the coating, play a role in controlling the release process of Cu ions in the copper-containing stainless steel coating and enable the copper-containing stainless steel coating to have quick and long-acting antibacterial and antiviral functions. In addition, the cold spraying process has high efficiency and low cost, and is beneficial to large-scale popularization.
3. The copper-containing stainless steel coating can be prepared on the surfaces of aluminum alloy and zinc alloy, and particularly applied to door handles, stair handrails or handrails frequently contacted with pathogenic microorganisms.
Drawings
FIG. 1 is an SEM photograph of the interface of a cold sprayed copper-containing stainless steel coating and a substrate in example 5 of the present invention.
Detailed Description
The technical solution of the present invention is further explained by concrete implementation according to the present invention. The examples are only for the purpose of facilitating understanding of the present invention and are not to be construed as specifically limiting the present invention. The powder compositions and the cold spray process parameters used in the examples and comparative examples are shown in table 1.
The specific implementation process is as follows:
(1) powder mixing: weighing 304L stainless steel powder and pure Cu powder according to a proportion, mixing the weighed powder with a steel ball with the diameter and the size of 5mm, putting the powder into a special mixing barrel, and uniformly mixing the powder at a set speed and time parameter.
(2) Preparing a base material: before cold spraying treatment is carried out on the base material, mixed liquid of ethanol and acetone is adopted to carry out surface oil removal on the base material, the mixing ratio of the ethanol to the acetone is 1:1, and after oil removal is finished, white corundum is adopted to carry out sand blasting roughening treatment.
(3) Preparing a cold spraying coating: and putting the uniformly mixed powder into a powder feeder, setting appropriate process parameters, vertically fixing a spray gun on a support, and moving a sample on an X-Y two-dimensional motion platform relative to the spray gun to finish the preparation of the Cu-containing stainless steel cold spraying coating.
TABLE 1 Cold spray powder compositions and Cold spray Process parameters for the examples and comparative examples
1. Detection of antibacterial Properties
According to the relevant standard regulations of JIS Z2801 & 2000 & lt & gt antibacterial processing product-antibacterial property test method and antibacterial effect & gt, GB/T2591 & lt & gt 2003 & lt & gt antibacterial property test method and antibacterial effect & gt for antibacterial plastics & gt, the antibacterial rate of the cold-sprayed copper-containing stainless steel coating shown in Table 1 after acting on common bacteria (Escherichia coli E. Wherein the co-culture time is set to 2 hours and 4 hours, and the concentration of co-cultured bacteria is set to (1-2). times.105CFU/mL. The results of the antibacterial performance test are shown in table 2, wherein the calculation formula of the antibacterial rate is as follows: the antibacterial rate (%) - (number of viable bacteria on the surface of the uncoated base material-number of viable bacteria on the surface of the copper-containing stainless steel coating)/number of viable bacteria on the surface of the uncoated base material]×100％。
2. Antiviral Performance test
The viruses selected for the test of antiviral properties in examples and comparative examples were influenza A virus (H1N1) and coronavirus (SARS-CoV), and Vero-E6 cells were inoculated into 96-well cell culture plates and cultured at 37 ℃ for 24 hours, and then stored. Dripping 10 mu L of the mixture with the concentration of (6-7) multiplied by 106TCID50/mL of motor canine kidney cell (MDCK) cell supernatant was applied to the surface of the cold spray copper-containing stainless steel coated samples and allowed to air dry rapidly. After culturing in a cell culture chamber at 37 ℃ for 4 hours, cytopathic effect (CPE) was observed under a microscope: and taking the culture supernatant to carry out neuraminidase activity detection. Blank control wells (normal cells) and virus control wells (untreated virus wells) were set for the experiments, and the sample wells were cold spray copper-containing stainless steel coated samples. The calculation formula of the virus inhibition rate is as follows: inhibition (%) 100- [ (sample well-blank)/(virus control-blank)]×100％。
3. Porosity detection
The porosity of the cold-sprayed copper-containing stainless steel coating is represented by an image method, an interface picture of the coating and a substrate is shot at 200x by using a metallographic microscope, and the area ratio of pores in the coating is obtained by performing contrast analysis on the coating by using ImagePro software.
4. Corrosion resistance
The corrosion resistance test is analyzed through a salt spray corrosion test, and whether the corrosion resistance test passes the salt spray test is judged according to the change of the surface macroscopic morphology after the test according to the test of the national standard GB/T10125-.
Table 2 relevant performance test experimental results of Cu-containing stainless steel cold spray coatings of examples and comparative examples
From the results in table 2, it can be seen that the copper-containing stainless steel coatings cold sprayed in the embodiments 1 to 7 of the present invention exhibit rapid and effective antibacterial and antiviral functions, and within 4 hours, the antibacterial rate can reach 99.9%, and the virus inhibition rate can reach more than 90%. Compared with the comparative example, the coating has lower porosity and meets the use requirement. Therefore, the setting of proper powder parameters, powder mixing process and cold spraying process parameters is the key point for obtaining the copper-containing stainless steel cold spraying coating with the antibacterial and antiviral functions.
Cold spray imposes size requirements on the particle size distribution of the selected powder, which can affect the porosity of the cold spray coating. First, within the range satisfying the requirement of the ratio of the two powder particle size distributions D50, the particle size distributions D50 of the pure Cu powder and the 304L stainless steel powder are too large, the gravity of the large particle powder exceeds the aerodynamic force and the electrostatic force, and the powder falls down before reaching the surface of the workpiece due to the action of gravity during the flight, resulting in a decrease in the powdering rate, thereby increasing the porosity of the coating and decreasing the corrosion resistance (comparative examples 1 and 3). When the particle size distribution D50 of the pure Cu powder and the 304L stainless steel powder is too small, the too fine powder is agglomerated into powder clusters, and smooth small packets are formed when the powder clusters are sprayed on the surface of the substrate, so that the appearance is influenced. Furthermore, the ultrafine powder is easy to absorb moisture and agglomerate, the stability is reduced, and the phenomena of spray gun blockage, poor powder spraying and the like are generated when the ultrafine powder is used (comparative example 2 and comparative example 4). In addition, the selection of the particle size distribution D50 of both powders is within the range of application, and the D50 ratio is not within the claimed range, the D50 ratio is too low, which causes the uniformity of Cu content to be poor, resulting in the decrease of corrosion resistance (comparative example 5), and the D50 ratio is too high, which causes the increase of porosity and the decrease of corrosion resistance (comparative example 6).
The Cu element is an important alloy element in the copper-containing stainless steel coating and is a necessary condition for ensuring that the cold spraying coating has quick and long-acting antibacterial and antiviral functions. The cold spray coating prepared by the method cannot exert effective antibacterial and antiviral functions in a short time due to the excessively low Cu content (comparative example 7), and the corrosion resistance of the coating is reduced due to the excessively high Cu content (comparative example 8) although the coating can be ensured to exert the effective antibacterial and antiviral functions due to the excessively high Cu content.
Before cold spraying of the powder, the composite powder needs to be mechanically mixed, in order to further improve the uniformity of the powder mixed by the traditional machine, a steel ball with the diameter of 5mm is added, and the mixing speed and the mixing time can influence the uniformity of the powder. If the mixing speed is too low or too high, powder with good uniformity cannot be obtained within a limited time, and the porosity of the coating of the cold spray Cu-containing stainless steel is too high, the corrosion resistance is lowered (comparative examples 9 and 10). Too short a mixing time results in failure to obtain powder with good uniformity and increase in coating porosity, while too long a mixing time wastes resources and does not contribute to further improvement in coating functionality and porosity (comparative examples 11 and 12).
The parameters of the cold spraying process mainly include carrier gas temperature, spraying distance, spraying pressure and powder feeding temperature. Too low carrier gas temperature and too low powder feeding temperature give too small kinetic energy to the powder particles, resulting in poor deposition during powder spraying, resulting in increased porosity and decreased corrosion resistance (comparative examples 13 and 19). The carrier gas temperature is too high, the powder feeding temperature is too high, the deposition efficiency of the composite coating is facilitated, the porosity is reduced, but Cu in the composite coating is burnt, and the antibacterial and antiviral effects are reduced (comparative example 14 and comparative example 20).
The spray distance of the cold spray is too close and the pressure is too high, so that the powder particles are scattered, and the porosity of the coating is improved and the corrosion resistance is reduced (comparative example 15 and comparative example 18). Too far spraying distance and too small pressure lead to unstable powder velocity reduction, thus leading to increased porosity of the coating and reduced corrosion resistance (comparative example 16 and comparative example 17).
From the above examples and comparative examples, it can be seen that the antibacterial and antiviral properties of the cold spray copper-containing stainless steel coating and the porosity of the coating can be influenced by the basic powder parameters, the powder mixing process and the cold spray process parameters, and the cold spray copper-containing stainless steel coating with high antibacterial and antiviral properties and high porosity can be obtained only by setting the process parameters within the scope of the present invention.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. The cold spraying copper-containing stainless steel coating with antibacterial and antiviral functions is characterized by comprising the following components in percentage by weight: the addition amount of the pure Cu spherical powder is 4.0-25.0 percent, and the balance is 304L stainless steel spherical powder;
wherein the D50 value of the particle size distribution of the 304L stainless steel spherical powder is 18.0-30.0 μm, and the D50 value of the particle size distribution of the pure Cu spherical powder is 10.0-22.0 μm.
2. The cold spray copper-containing stainless steel coating having antibacterial and antiviral effects according to claim 1, wherein the ratio of the particle size distribution D50 of the pure Cu spherical powder to the 304L stainless steel spherical powder is 0.50 to 0.90.
3. The cold spray copper-containing stainless steel coating with antibacterial and antiviral functions of claim 1, wherein the copper-containing stainless steel coating comprises the following components in percentage by weight: the addition amount of the pure Cu spherical powder is 5.0-20.0, and the balance is 304L stainless steel spherical powder;
wherein the D50 value of the particle size distribution of the 304L stainless steel spherical powder is 23.0-25.0 μm, and the D50 value of the particle size distribution of the pure Cu spherical powder is 12.0-20.0 μm; the ratio of the particle size distribution D50 of the pure Cu spherical powder and the 304L stainless steel spherical powder is 0.50-0.90.
4. A preparation method of the cold spraying copper-containing stainless steel coating with antibacterial and antiviral functions as claimed in any one of claims 1 to 3, characterized in that the stainless steel coating is prepared by a cold spraying method, and the preparation method comprises the following specific steps:
1) powder mixing: weighing 304L stainless steel powder and pure Cu powder according to a proportion by adopting a mechanical mixing process, mixing the weighed powder and steel balls, putting the mixture into a mixing barrel, and uniformly mixing the mixture at a set speed and time parameter;
2) preparing a base material: before cold spraying treatment is carried out on the base material, mixed liquid of ethanol and acetone is adopted to carry out surface oil removal on the base material, the mixing ratio of the ethanol and the acetone mixed liquid is 1:1, and after oil removal is finished, white corundum is adopted to carry out sand blasting roughening treatment;
3) preparing a cold spraying coating: and putting the uniformly mixed powder into a powder feeder, setting appropriate process parameters, vertically fixing a spray gun on a support, and moving a sample on an X-Y two-dimensional motion platform relative to the spray gun to finish the preparation of the Cu-containing stainless steel cold spraying coating.
5. The method for preparing the copper-containing stainless steel coating with antibacterial and antiviral functions as claimed in claim 4, wherein the method comprises the following steps: in the step 1), steel balls with the diameter of 5mm are added into a mixing barrel, the mixing barrel containing the powder and the steel balls is put into a mixer to be uniformly mixed, the mixing speed is 25-50 r/min, and the mixing time is 3.0-6.0 hours.
6. The method for preparing the copper-containing stainless steel coating with antibacterial and antiviral functions as claimed in claim 4, wherein the method comprises the following steps: in the step 3), a cold spraying device is adopted for coating preparation, and the cold spraying device comprises a control system, a powder feeder, a gas heater, a Laval nozzle and a powder heater; the cold spraying process parameters for preparing the stainless steel coating by using the cold spraying device are as follows: the heating temperature of the carrier gas is 200-.
7. The method for preparing the copper-containing stainless steel coating with antibacterial and antiviral functions as claimed in claim 4, wherein the method comprises the following steps: in the step 3), the cold spraying process parameters are as follows: the heating temperature of the carrier gas is 300-700 ℃, the spraying distance is 15.0-25.0mm, the spraying pressure is 2.0-3.0MPa, and the powder feeding heating temperature is 300-500 ℃.
8. A cold spray copper-containing stainless steel coating prepared by the method of any one of claims 4 to 6, wherein: the coating shows rapid and effective antibacterial and antiviral functions, and the concentration is 1 multiplied by 10 within 4 hours5-2×105The antibacterial rate of the bacteria of CFU/mL reaches 99.9 percent, and the concentration is 6 multiplied by 106～7×106The virus inhibition rate of TCID50/mL reaches more than 90%.
9. The cold spray copper-containing stainless steel coating of claim 8, wherein: the spraying base material is aluminum alloy or zinc alloy.
10. Use of the cold sprayed copper-containing stainless steel coating of claim 8 as a door handle, stair railing or railing in a public environment.
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