CN113523267A - Novel antibacterial composite powder, stainless steel, preparation method and application thereof - Google Patents
Novel antibacterial composite powder, stainless steel, preparation method and application thereof Download PDFInfo
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Abstract
The invention provides novel antibacterial composite powder, stainless steel, a preparation method and application thereof, wherein the antibacterial composite powder comprises stainless steel particles with the particle size of 0.5-15 mu m and silver-containing nano particles attached to the surfaces of the stainless steel particles, and the preparation method comprises the following steps: dispersing silver-containing nano particles in a dispersing agent, adding stainless steel particles with the particle size of 0.5-15 mu m, and adsorbing the silver-containing nano particles on the surfaces of the stainless steel particles to prepare the antibacterial composite powder. The antibacterial composite powder is prepared into silver-containing antibacterial stainless steel by adopting a powder metallurgy method. The silver-containing antibacterial stainless steel provided by the invention is simple in preparation process, has a series of advantages of a powder metallurgy method, and can be used as a functional and structural material. Since the whole stainless steel matrix contains fine silver phases which are uniformly distributed, the silver-containing stainless steel still has excellent antibacterial performance even after the surface is abraded.
Description
Technical Field
The invention belongs to the technical field of stainless steel, and particularly relates to novel antibacterial composite powder, antibacterial stainless steel prepared from the antibacterial composite powder, and preparation methods and applications of the antibacterial composite powder and the antibacterial stainless steel.
Background
Bacteria as pathogens have been a problem in the food industry and public health sector. Especially, with the development of social economy, people have more and more chances to contact in public places, and the safety and health problems are paid more and more attention. However, stainless steel, which is one of the most widely used materials in the field of public health, does not have an antibacterial function, so that people are at a higher risk of infecting various germs. Therefore, the development of stainless steel appliances with excellent and stable antibacterial performance has great significance and value.
The existing antibacterial stainless steel is mainly divided into two categories: copper-containing antimicrobial stainless steel and silver-containing antimicrobial stainless steel. The copper-containing antibacterial stainless steel has higher solid solubility in an austenite region, so that the copper-containing antibacterial stainless steel with copper phases or copper-rich phases uniformly distributed in a matrix can be easily obtained through the traditional casting and heat treatment process, and the excellent antibacterial performance of copper elements is exerted. The copper-containing antibacterial stainless steel prepared by the method has been successful in stainless steel with multiple grades, and typically comprises high-strength martensite antibacterial stainless steel added with 3-4% of copper and copper-containing austenite antibacterial stainless steel with wide application and excellent processing performance. At present, Chinese patent CN02144683.0 and Chinese patent CN02144568.0 are available. However, copper-containing antibacterial stainless steel requires a high copper addition amount and is limited by the fact that the bactericidal effect of copper itself is not perfect. Higher copper addition reduces the corrosion resistance and the processability of the original grade stainless steel. Copper and silver are used as alloy addition elements with antibacterial function, the antibacterial property of silver is about 100 times of that of copper, and the silver can generate obvious antibacterial effect only by adding a small amount of silver without subsequent complex heat treatment, so that the antibacterial property of the product is superior to that of copper-containing antibacterial steel, but the cost is not greatly different. In addition, silver has been shown to have a broader antibacterial spectrum and to have a better inhibitory or bactericidal effect on a wider variety of bacteria.
However, since silver and iron are typical immiscible element systems, they have very low solid solubility (0.0002% for silver in α -iron) in both solid and liquid states, and silver with a lower melting point is very volatile in the high temperature environment of steel making, and silver has a density about twice that of iron and is very easy to segregate during casting, so that it is difficult to uniformly add silver to stainless steel in the conventional casting process. Although research on improvement of silver phase distribution in cast silver-containing stainless steel through technical means such as aging heat treatment, solution heat treatment and the like is available, the research is limited by the extremely low solid solubility of silver in stainless steel, and it is still difficult to ensure that silver is uniformly distributed in a stainless steel matrix, so that the range of a local silver-poor area is large, and it is difficult to ensure that all bacteria can interact with a silver-containing precipitated phase, and thus, the antibacterial performance is unstable. In addition, the traditional method for preparing the antibacterial stainless steel by casting the metal material has the defects of high energy and raw material consumption, high production cost, environmental friendliness and the like.
Compared with the traditional casting process, the powder metallurgy technology has the following advantages: high shape freedom, no or little cutting, high material utilization up to 95%, and easy mass production. Therefore, the antibacterial stainless steel prepared by the powder metallurgy technology has wide prospect.
Disclosure of Invention
Therefore, the invention aims to provide silver-containing antibacterial stainless steel with excellent antibacterial performance prepared by adopting a powder metallurgy technology, and a preparation method and application thereof.
The inventors of the present invention have creatively considered the problems of the size of bacteria and the average spacing between silver phases in a stainless steel matrix based on the powder metallurgy technology, and ensured the interaction of bacteria and silver elements by adjusting the average spacing of silver phases in a silver-containing antibacterial stainless steel to be equivalent to the size of bacteria using stainless steel metal powder equivalent to the size of typical bacteria. Meanwhile, by using the nano-scale silver particles or silver-containing particles, the invention ensures that the fine and uniform silver element distribution can be ensured by trace added silver by utilizing the characteristics of small size and good adsorbability of the nano powder. The selection of a suitably sized stainless steel powder and the addition of nano-sized silver particles or silver-containing particles are the most important parts of the present invention. The improved silver-containing stainless steel matrix provided by the invention has dispersed fine silver phases, and can ensure the interaction between bacteria and the silver phases, so that the permanent and excellent antibacterial performance is obtained.
The invention provides an antibacterial composite powder, which comprises stainless steel particles with the particle size of 0.5-15 mu m and silver-containing nano particles attached to the surfaces of the stainless steel particles.
According to the antibacterial composite powder provided by the present invention, the silver-containing nanoparticles may be nanoscale silver particles and/or silver-containing compound particles. The silver-containing nanoparticles may have an average particle diameter of several nanometers to several hundred nanometers, and for example, may be 1 to 500nm, preferably 10 to 300nm, more preferably 50 to 200nm, and most preferably 50 to 100 nm. For example, in a preferred embodiment, the silver-containing nanoparticles have an average particle size of 80 nanometers. Wherein the silver-containing compound may be silver oxide, silver protoxide, or the like.
According to the antibacterial composite powder provided by the invention, the stainless steel particles are stainless steel metal powder or element powder with the size equivalent to or smaller than that of bacteria; the average particle diameter thereof may be 0.5 to 15 μm, preferably 1 to 10 μm, more preferably 1 to 5 μm. For example, in a preferred embodiment, the stainless steel powder has an average particle size of 2.5 microns.
According to the antibacterial composite powder provided by the invention, the content of the silver element in the antibacterial composite powder can be 0.05-1 wt%, and preferably 0.1-0.5 wt%.
The stainless steel particles used in the antimicrobial composite powder of the present invention may be any grade of stainless steel prealloyed powder or elemental powder that meets the dimensional characteristics described. In some embodiments of the invention, the stainless steel particles consist essentially of: 12 to 30 weight percent of chromium element, 0 to 18 weight percent of nickel element, less than or equal to 1.2 weight percent of carbon element, less than or equal to 3 weight percent of silicon element, less than or equal to 10 weight percent of manganese element, and can further contain one or more alloy elements selected from Cu, Mo, Co, Ti, Nb, V, Al, Zr and B, wherein the content of Cu is less than or equal to 4 weight percent, the content of Mo is less than or equal to 3.5 weight percent, the content of Al is less than or equal to 1.2 weight percent, the content of other alloy elements is less than or equal to 3 weight percent, and the balance is iron element.
For example, in some embodiments of the invention, an austenitic stainless steel powder is used, having a chemical composition of: less than or equal to 0.1 wt% of C, less than or equal to 3 wt% of Si, less than or equal to 10 wt% of Mn, Cr: 13-30 wt%, Ni: 4-18 wt%, Mo is less than or equal to 3.5 wt%, and silver element: 0.05-1 wt%, and the balance of iron and inevitable impurities.
The austenitic stainless steel powder can further contain one or more alloy elements selected from Cu, Mo, Co, Ti, Nb, V, Al, Zr and B, wherein Cu is less than or equal to 4wt percent, and the content of other alloy elements is less than or equal to 3wt percent.
For example, in other embodiments of the present invention, a ferritic stainless steel powder is used having a chemical composition of: less than or equal to 0.2 wt% of C, less than or equal to 2 wt% of Si, less than or equal to 2.5 wt% of Mn, Cr: 10-30 wt%, Ni: less than or equal to 2 wt%, silver element: 0.05-1 wt%, and the balance of iron and inevitable impurities.
The ferritic stainless steel powder may further contain one or more alloying elements selected from Cu, Mo, Co, Ti, Nb, V, Al, Zr and B, wherein Cu is 2.5 wt% or less and the content of other alloying elements is 3 wt% or less.
For example, in still other embodiments of the present invention, a martensitic stainless steel powder is used having a chemical composition of: c is less than or equal to 2 wt%, Si is less than or equal to 3 wt%, Mn is less than or equal to 3 wt%, Cr: 10-20 wt%, Ni: less than or equal to 5 wt%, silver element: 0.05-1 wt%, and the balance of iron and inevitable impurities.
The martensitic stainless steel powder may further contain one or more alloying elements selected from Cu, Mo, Co, Ti, Nb, V, Al, Zr and B, wherein Cu is less than or equal to 4 wt%, and the content of other alloying elements is less than or equal to 3 wt%.
The invention also provides a preparation method of the antibacterial composite powder, which comprises the following steps:
(1) dispersing silver-containing nano particles in liquid with a dispersing effect to obtain a suspension;
(2) and (2) adding stainless steel particles with the particle size of 0.5-15 mu m into the suspension obtained in the step (1), stirring and/or vibrating to enable the silver-containing nanoparticles to be adsorbed on the surfaces of the stainless steel particles, then pouring out the supernatant, and evaporating the remainder to dryness to obtain the stainless steel particles with the silver-containing nanoparticles adsorbed on the surfaces, namely the antibacterial composite powder.
According to the method for preparing the antibacterial composite powder provided by the invention, the liquid having a dispersing effect (or called as a dispersing agent) in the step (1) can be alcohol, an aqueous solution of alcohol or an aqueous solution containing a surfactant, as long as the nanoparticles can be well dispersed. Wherein the surfactant-containing aqueous solution is preferably: an aqueous solution of polyvinyl alcohol (PVA) or an aqueous solution of polyvinylpyrrolidone (PVP).
The amount of the liquid having a dispersing action in the step (1) used in the present invention is not particularly limited as long as the dispersing action is performed to form a suspension. In some preferred embodiments, in the step (1), 500ml of alcohol or 500ml of an aqueous solution in which 0.5g of PVP is dissolved can be used for dispersion with respect to 1g of nano-silver oxide.
According to the preparation method of the antibacterial composite powder provided by the invention, in the step (2), the addition amount of the stainless steel particles is such that the content of silver element in the antibacterial composite powder is 0.05-1 wt%, preferably 0.1-0.5 wt%.
The invention also provides silver-containing antibacterial stainless steel which is prepared from the antibacterial composite powder by adopting a powder metallurgy method.
The invention also provides a preparation method of the silver-containing antibacterial stainless steel, which comprises the step of preparing the silver-containing antibacterial stainless steel by using the antibacterial composite powder provided by the invention or the antibacterial composite powder prepared by the preparation method as a raw material and adopting a powder metallurgy method.
Specifically, the preparation method of the silver-containing antibacterial stainless steel can comprise the following steps:
(1) dispersing silver-containing nano particles in liquid with a dispersing effect to obtain a suspension;
(2) adding stainless steel particles with the particle size of 0.5-15 mu m into the suspension obtained in the step (1), stirring and/or vibrating to enable the silver-containing nanoparticles to be adsorbed on the surfaces of the stainless steel particles, then pouring out the supernatant, and evaporating the remainder to dryness to obtain the stainless steel particles with the silver-containing nanoparticles adsorbed on the surfaces;
(3) and (3) taking the stainless steel particles with silver-containing nano particles adsorbed on the surfaces obtained in the step (2) as raw materials, and preparing the silver-containing antibacterial stainless steel by adopting a powder metallurgy method.
According to the preparation method of the silver-containing antibacterial stainless steel provided by the invention, the definitions and characteristics of the silver-containing nano particles and the stainless steel particles are as described in the foregoing, and are not repeated herein.
According to the preparation method of the silver-containing antibacterial stainless steel provided by the invention, the definitions and characteristics of the step (1) and the step (2) are the same as those of the preparation method of the antibacterial composite powder, and the details are not repeated here.
According to the preparation method of the silver-containing antibacterial stainless steel provided by the invention, the powder metallurgy method in the step (3) is such as cold press molding sintering, hot press sintering, spark plasma sintering, metal injection molding and the like, so that antibacterial stainless steel products with various shapes and sizes can be obtained.
In one embodiment of the invention, for example, a powder metallurgy process using conventional press sintering: adopting cold press molding or hot press molding technology to press and mold the mixed powder (namely, the stainless steel powder with silver-containing nano particles adsorbed on the surface) to prepare green bodies with various shapes; and sintering the obtained green body in the atmosphere of protective gas or reducing gas to obtain the silver-containing antibacterial stainless steel appliance.
In another aspect, the invention also provides a stainless steel appliance, wherein the stainless steel appliance comprises the silver-containing antibacterial stainless steel provided by the invention. The stainless steel appliances include various medical appliances, living goods and the like, such as a whole body including a door handle, tweezers, a watch and the like or components thereof.
The principle of the invention is as follows: stainless steel pre-alloyed powder or element powder (namely, stainless steel particles) with the size equivalent to that of bacteria is adopted, meanwhile, the characteristics of small size and good adsorbability of the nano silver-containing powder are utilized, a layer of silver-containing nano particles is uniformly adsorbed on the surface of the stainless steel metal powder, and the obtained mixed powder is sintered by using a powder metallurgy process to obtain the novel silver-containing antibacterial stainless steel. The resulting stainless steel material has fine silver particles throughout the matrix and the average spacing of the silver phases is comparable to or even smaller than the size of typical bacteria to ensure that each bacteria can interact with elemental silver. Therefore, the silver-containing antibacterial stainless steel prepared by the powder metallurgy method improved by adding the silver-containing nano particles has the characteristics of lasting antibacterial property and wide antibacterial range.
The core content of the invention lies in the selection of stainless steel powder with proper size and the use of nano silver-containing particles. Namely, stainless steel metal powder with the size equal to or smaller than that of typical bacteria is adopted, and the characteristics of nano silver-containing particles, small size and easy adsorption are utilized, so that the obtained silver-containing stainless steel has more uniform and fine silver distribution under the same silver content, and thus excellent and stable antibacterial performance is obtained. In addition, the method for obtaining the composite powder by dispersing the nano silver-containing particles on the surface of the stainless steel powder recited in the present invention is only a typical process, and any minor modification based on the innovative points of the present invention, such as using different dispersants, adopting different dispersing processes, or adding and dispersing nano-scale (or micro-nano-scale) silver-containing particles on the surface of the stainless steel powder in different stages of a specific powder metallurgy process, should be within the protection scope of the present invention.
The novel silver-containing antibacterial stainless steel provided by the invention is simple in manufacturing process, has a series of advantages of a powder metallurgy process, can be used as a functional and structural material, can be conveniently manufactured into various stainless steel appliances with complex shapes, and has wide application fields. In addition, the whole stainless steel matrix contains fine silver phases which are uniformly distributed, so the novel silver-containing stainless steel has excellent antibacterial performance even after the surface is abraded.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a scanning electron microscope image of the silver-containing antibacterial stainless steel prepared in example 1;
FIG. 2 is a scanning electron microscope image of the silver-containing antibacterial stainless steel prepared in example 1 under a low-magnification, back-scattered electron signal;
FIG. 3 is a scanning electron microscope image of the silver-containing antibacterial stainless steel prepared in example 1 under high power and secondary electron signals;
FIG. 4 is a scanning electron microscope image of different regions of a typical cast silver-containing stainless steel;
FIG. 5 is a photograph of an antibacterial test of the silver-containing antibacterial stainless steel prepared in example 1;
FIG. 6 is a photograph of an antibacterial test of the silver-containing antibacterial stainless steel prepared in example 2;
FIG. 7 is a photograph of an antibacterial test of a common 316L stainless steel as a control;
fig. 8 is a photograph of an antimicrobial test of a typical cast 316L silver-containing antimicrobial stainless steel as a control.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments, which are given for the purpose of illustration only and are not intended to limit the scope of the invention.
Example 1
Taking 99.7g of 316L stainless steel prealloyed powder with the purity of more than 99.5 percent and D90 being 5 mu m and 0.3g of nano silver oxide powder with the average grain diameter of 80nm and the purity of more than 99.5 percent, preparing the silver-containing antibacterial stainless steel according to the following steps:
(1) adding nano silver oxide powder into 300ml of alcohol, and dispersing uniformly under ultrasonic oscillation to form stable suspension;
(2) adding the 316L stainless steel metal powder into the suspension liquid obtained in the step (1), continuously stirring to enable the nano silver oxide to be adsorbed on the surfaces of stainless steel powder particles, pouring out the supernatant, and evaporating the residual alcohol to dryness to obtain 316L stainless steel powder with the surface uniformly adsorbing the nano silver oxide;
(3) and (3) putting the 316L stainless steel powder with the surface adsorbed with the nano silver oxide obtained in the step (2) into a cylindrical graphite mold, setting the sintering parameters of the discharge plasma as 50Mpa, keeping the temperature at 950 ℃ for 15min, starting a sintering program under a vacuum condition, and obtaining an initial workpiece after the heat preservation is finished.
Example 2
Taking 99.7 parts of 316L stainless steel prealloyed powder with the purity of more than 99.5 percent and the purity of D90 being 5 mu m and 0.3 part of nano silver powder with the average grain diameter of 80nm and the purity of more than 99.5 percent, preparing the silver-containing antibacterial stainless steel according to the following steps:
(1) adding nano-silver powder into 500ml of aqueous solution containing a surfactant (the surfactant is PVP (molecular weight: 58000), and the concentration is 1g/L), and dispersing uniformly under ultrasonic oscillation to form stable suspension;
(2) adding the 316L stainless steel powder into the suspension liquid obtained in the step (1), continuously stirring to enable the nano silver to be adsorbed on the surface of the stainless steel powder particles, pouring out the supernatant, and evaporating the residual solution to dryness to obtain 316L stainless steel powder with the surface uniformly adsorbing the nano silver;
(3) and (3) preparing 316L stainless steel powder with the surface adsorbed with nano silver obtained in the step (2) into a disc green body by utilizing cold press molding, putting the disc green body into a sintering furnace, heating to 1350 ℃ under the protection of argon, preserving heat for 2 hours, sintering, and cooling along with the furnace to obtain an initial workpiece.
Performance testing
(1) In examples 1 and 2, the stainless steel powder was comparable in size to the bacteria. FIG. 1 is a scanning electron microscope image of the silver-containing antibacterial stainless steel prepared in example 1. FIG. 2 is a scanning electron microscope image of the silver-containing antibacterial stainless steel prepared in example 1 under low-magnification, back-scattered electron signals, in which white particles are silver phase and black is stainless steel matrix. FIG. 3 is a scanning electron microscope image of the silver-containing antibacterial stainless steel prepared in example 1 under high power and secondary electron signals, wherein the white particles are silver.
FIG. 4 is a scanning electron microscope image of different areas of a typical cast silver-containing stainless steel under the same magnification. In the figure, the bright white particles are silver, and it can be seen that the silver particles are coarse and are concentrated and distributed only in a part of the region.
(2) The stainless steel wafers obtained in examples 1 and 2 were subjected to an antibacterial property test, and the antibacterial rate was higher than 99% according to JISZ2801-2010 "antibacterial processed article-antibacterial property test method and antibacterial effect". The results of comparing the antibacterial stainless steel of the present invention with the common stainless steel and the existing silver-containing antibacterial stainless steel are shown in fig. 4 to 7, in which:
FIG. 5 is a photograph of an antibacterial test of the silver-containing antibacterial stainless steel prepared in example 1;
FIG. 6 is a photograph of an antibacterial test of the silver-containing antibacterial stainless steel prepared in example 2;
FIG. 7 is a photograph of an antibacterial test of a general 316L stainless steel (Standard Industrial 316L stainless steel) as a control;
fig. 8 is a photograph of an antimicrobial test of a typical cast 316L silver-containing antimicrobial stainless steel as a control.
In the antibacterial experiment, the bacterial residue on the surface of the sample and Escherichia coli after 24 hours of co-culture was compared. As can be seen from comparing fig. 5 to 8, the antibacterial stainless steels prepared in examples 1 and 2 of the present invention have a more significant antibacterial effect against surface bacteria than the common stainless steels and the typical cast 316L silver-containing antibacterial stainless steels: the ordinary 316L is full of bacteria, the number of bacteria in the cast silver-containing 316L stainless steel is reduced, but a large amount of bacteria still exist, and the colony number of the silver-containing 316L stainless steel is very small. The residual bacteria on the surface of the stainless steel after 24 hours of culture are few, and the antibacterial rate of the silver-containing 316L stainless steel reaches 99 percent or more by calculation. Under the same test conditions, the antibacterial rate of a typical cast 316L silver-containing antibacterial stainless steel is about 87%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. An antibacterial composite powder comprising stainless steel particles having a particle size of 0.5-15 μm and silver-containing nanoparticles attached to the surface of the stainless steel particles.
2. The antimicrobial composite powder according to claim 1, wherein the silver-containing nanoparticles have an average particle size of 1-500nm, preferably 10-300nm, more preferably 50-200nm, most preferably 50-100nm, preferably the stainless steel powder has an average particle size of 1-10 μ ι η, preferably 2-6 μ ι η.
3. The antimicrobial composite powder according to claim 1 or 2, wherein the content of elemental silver in the antimicrobial composite powder is 0.05-1 wt%, preferably 0.1-0.5 wt%.
4. A method for preparing the antibacterial composite powder of any one of claims 1 to 3, comprising the steps of:
(1) dispersing silver-containing nano particles in liquid with a dispersing effect to obtain a suspension;
(2) and (2) adding stainless steel particles with the particle size of 0.5-15 mu m into the suspension obtained in the step (1), stirring and/or vibrating to enable the silver-containing nanoparticles to be adsorbed on the surfaces of the stainless steel particles, then pouring out the supernatant, and evaporating the remainder to dryness to obtain the stainless steel particles with the silver-containing nanoparticles adsorbed on the surfaces, namely the antibacterial composite powder.
5. The method for preparing an antibacterial composite powder according to claim 4, wherein the liquid having a dispersing action in step (1) is alcohol, an aqueous solution of alcohol or an aqueous solution containing a surfactant, preferably, the aqueous solution containing a surfactant is an aqueous solution of polyvinyl alcohol or an aqueous solution of polyvinyl pyrrolidone.
6. The method of preparing antibacterial composite powder according to claim 4, wherein in step (2), the stainless steel particles are added in an amount such that the silver element content in the silver-containing antibacterial stainless steel is 0.05 to 1 wt%, preferably 0.1 to 0.5 wt%.
7. An antibacterial stainless steel containing silver, which is prepared from the antibacterial composite powder according to any one of claims 1 to 3 by a powder metallurgy method.
8. A method for preparing silver-containing antibacterial stainless steel, which comprises the step of preparing the silver-containing antibacterial stainless steel by a powder metallurgy method by using the antibacterial composite powder as claimed in any one of claims 1 to 3 or the antibacterial composite powder prepared by the preparation method as claimed in any one of claims 4 to 6 as a raw material.
9. The method of claim 8, wherein the powder metallurgy method is cold press molding sintering, hot press sintering, spark plasma sintering or metal injection molding.
10. A stainless steel appliance comprising the silver-containing antimicrobial stainless steel of claim 7, preferably a medical appliance or a living goods, such as a door handle, tweezers, and watch, as a whole or a component thereof.
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