CN113322412A - High-strength austenite antibacterial stainless steel and preparation method thereof - Google Patents
High-strength austenite antibacterial stainless steel and preparation method thereof Download PDFInfo
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Abstract
The invention relates to high-strength austenitic antibacterial stainless steel, and belongs to the field of stainless steel materials. The stainless steel comprises the following components in percentage by weight: c: less than or equal to 0.03 percent; si: less than or equal to 1.0 percent; mn: less than or equal to 1.0 percent; cu: 3.5-4.5%; ni: 11.0-13.0%; al: 1.0-1.5%; cr: 17.0-19.0%; n: less than or equal to 0.005 percent; s is less than or equal to 0.010 percent; p: 0.05-0.10%; the balance being Fe. The invention utilizes the strong solid solution strengthening effect of P and the precipitation strengthening mode of two nanometer precipitated phases of a Cu-rich phase and a NiAl phase to fully play the composite strengthening effect of the Cu-rich phase and the NiAl phase in steel. Through the regulation and control of the graded aging heat treatment, the NiAl phase is separated out firstly, and the Cu-rich phase is separated out later, so that the high-strength austenitic antibacterial stainless steel is obtained.
Description
Technical Field
The invention relates to the field of stainless steel, in particular to high-strength austenitic antibacterial stainless steel.
Background
The austenitic stainless steel is Fe-Cr-Ni or Fe-Cr-Mn-Ni- (N) type stainless steel which mainly takes an austenitic structure at high temperature and room temperature. The Fe-Cr-Ni austenitic stainless steel is the stainless steel with the best comprehensive performance, the most brands, the most complete variety and specification, the widest application range, the fastest development, the largest yield and the widest consumption field in the five types of the prior stainless steel. The stainless steel has excellent corrosion resistance in various corrosive mediums, good comprehensive mechanical property and excellent processing property and weldability, thereby being widely applied to various fields of food, chemical industry, light industry and the like. The non-ferromagnetic and good low temperature toughness of austenitic stainless steels further expand their range of applications.
The copper-containing austenitic antibacterial stainless steel is a new steel material developed on the basis of Fe-Cr-Ni austenitic stainless steel, and shows a strong, broad-spectrum and durable sterilization function by utilizing Cu alloying and continuously dissolved trace Cu ions, so that the new material integrating the structure and the function has a wide application prospect.
However, the Cu-containing Fe-Cr-Ni type austenitic antibacterial stainless steel has low strength and hardness, and is not suitable for use in equipment or parts which are subjected to heavy load and have requirements for hardness and wear resistance. Therefore, if the Cu-containing austenitic stainless steel can be endowed with higher strength and hardness, and the excellent comprehensive performance of the original Fe-Cr-Ni type austenitic stainless steel is not reduced, the application field of the austenitic stainless steel can be further widened.
Disclosure of Invention
The invention aims to provide high-strength austenitic antibacterial stainless steel and a preparation method thereof, which are used for realizing the precipitation of a Cu-rich phase and a NiAl phase through a P solid solution strengthening and nano precipitated phase synergistic strengthening technology and a graded heat treatment process, fully playing the composite strengthening role of solid solution strengthening and precipitation strengthening and realizing higher strength of the Cu-containing austenitic antibacterial stainless steel.
The technical scheme of the invention is as follows:
a high-strength austenite antibacterial stainless steel comprises the following chemical components in percentage by weight:
c: less than or equal to 0.03 percent; si: less than or equal to 1.0 percent; mn: less than or equal to 1.0 percent; cu: 3.5-4.5%; ni: 11.0-13.0%; al: 1.0-1.5%; cr: 17.0-19.0%; n: less than or equal to 0.005 percent; s is less than or equal to 0.010 percent; p: 0.05-0.10%; the balance being Fe.
As a preferred technical scheme, in the high-strength austenitic antibacterial stainless steel, the content relation of Ni and Al is limited, and the contents of Ni and Al in percentage by weight meet the following requirements: (Ni-8%)/Al is greater than or equal to 3.
The preparation method of the high-strength austenitic antibacterial stainless steel comprises the following steps:
(1) mixing raw materials according to the requirements of chemical components, and obtaining a steel ingot through vacuum induction smelting and pouring;
(2) and (3) carrying out heat preservation on the steel ingot at 1250-1300 ℃ for more than 4 hours, and then forging: the initial forging temperature is 1150-1200 ℃, the final forging temperature is 1000-1100 ℃, multi-direction (longitudinal-transverse-longitudinal three-direction) large reduction forging is carried out in the forging process, the initial reduction is not more than 10%, the other single reduction is more than 20%, the total forging ratio is more than 12, and the forging is carried out by air cooling to the room temperature;
(3) and carrying out solid solution treatment and graded aging heat treatment after forging.
The method for the graded solution treatment and the aging heat treatment comprises the following steps:
1) firstly, solid solution is carried out at 1050-1100 ℃ for 0.5-2 hours, and air cooling is carried out;
2) secondly, carrying out primary aging heat treatment at 760-860 ℃, wherein the aging time is 2-4 hours, and air cooling;
3) then, carrying out secondary aging heat treatment at 650-700 ℃, wherein the aging time is 4-6 hours, and air cooling;
4) and finally, carrying out third aging heat treatment at 450-550 ℃, wherein the aging time is 8-12 hours, and carrying out air cooling.
The microstructure of the stainless steel is austenite by preparing and carrying out a heat treatment method according to the components of the steel.
According to the preparation of the steel and the implementation of the heat treatment method, the yield strength of the stainless steel is more than or equal to 400MPa, the tensile strength is more than or equal to 1000MPa, and the elongation is more than or equal to 40.0%.
The stainless steel prepared according to the components of the steel and subjected to a heat treatment method has excellent antibacterial performance, and the antibacterial rate to escherichia coli is more than 99%, and the antibacterial rate to staphylococcus aureus is more than 99%.
The design idea of the invention is as follows:
the invention fully exerts the composite strengthening function of the P-rich phase and the NiAl-rich phase in steel by reasonable component design and utilizing the strong solid solution strengthening of the P and two nano precipitated phase precipitation strengthening modes. By means of the graded aging heat treatment process, the precipitation sequence of two precipitated phases is regulated and controlled, the NiAl phase is precipitated firstly, and the Cu-rich phase is precipitated later, so that the strength and the excellent antibacterial performance of the austenitic antibacterial stainless steel are improved simultaneously.
The invention has the beneficial effects that:
the austenite antibacterial stainless steel material obtained by the method can improve the strength and the antibacterial performance at the same time, and can widen the application field of the copper-containing austenite antibacterial stainless steel.
Drawings
FIG. 1 is a microstructure diagram of example 1.
FIG. 2 is a microstructure diagram of comparative example 5.
Detailed Description
In the specific implementation process, the preparation and heat treatment method of the high-strength austenitic antibacterial stainless steel are as follows:
(1) the raw materials are mixed according to the chemical components of the invention, and a steel ingot is obtained through vacuum induction smelting and pouring.
(2) Keeping the temperature of the steel ingot at 1250 ℃ for 5 hours, and then forging: the initial forging temperature is 1180 ℃, the final forging temperature is 1070 ℃, the forging process is carried out with the large reduction forging in a longitudinal-transverse-longitudinal three-way circulation mode, the first reduction is about 8 percent, the other single reductions are about 22 percent, 27 percent and 26 percent, the total forging ratio is 20, and the forging is carried out with air cooling to the room temperature;
(3) and cutting a heat treatment sample of the forged steel ingot, wherein the size of the sample is a plurality of squares of 11mm multiplied by 70mm, and then carrying out solution treatment and graded aging heat treatment.
And (4) processing the mechanical property sample of the steel sample after heat treatment, and testing the mechanical property. The sample specification is 5mm in diameter, 25mm in gauge length, and the test temperature is room temperature.
The antibacterial performance is detected according to standards such as JIS Z2801-2000 antibacterial processed product-antibacterial property test method and antibacterial effect, GB/T2591-2003 antibacterial plastic antibacterial property test method and antibacterial effect, and strains such as Escherichia coli and Staphylococcus aureus.
Hereinafter, the present invention will be described by comparing various examples and comparative examples, which are for illustrative purposes only and the present invention is not limited to these examples.
Example 1
The steel comprises the following chemical components in percentage by weight: c: 0.023%; si: 0.32 percent; mn: 0.25 percent; cu: 3.75 percent; ni: 12.3 percent; al: 1.35 percent; cr: 18.2 percent; n: 0.004%; s: 0.008 percent; p: 0.07 percent; the balance being Fe. The content relation of Ni and Al is as follows: (Ni-8%)/Al-3.2.
The heat treatment mode after forging is as follows:
(1) firstly, carrying out solid solution at 1070 ℃ for 1.0 hour, and cooling in air;
(2) secondly, carrying out primary aging heat treatment at 800 ℃, wherein the aging time is 3 hours, and air cooling;
(3) then, carrying out secondary aging heat treatment at 680 ℃ for 5 hours, and air-cooling;
(4) and finally, carrying out third aging heat treatment at 500 ℃ for 10 hours, and cooling in air.
The content relation of Ni and Al is as follows: (Ni-8%)/Al >3, and the microstructure is shown in FIG. 1 as an austenite structure. The sterilization rate and mechanical property tests are shown in table 1. The steel of example 1 has excellent antibacterial properties and high strength values.
Example 2
The steel comprises the following chemical components in percentage by weight: c: 0.018%; si: 0.53 percent; mn: 0.64 percent; cu: 3.55 percent; ni: 11.9 percent; al: 1.27 percent; cr: 18.5 percent; n: 0.004%; s: 0.008 percent; p: 0.10 percent; the balance being Fe. The content relation of Ni and Al is as follows: (Ni-8%)/Al 3.1.
The heat treatment mode after forging is as follows:
(1) firstly, solid solution is carried out at 1050 ℃, the solid solution time is 1.0 hour, and air cooling is carried out;
(2) secondly, carrying out primary aging heat treatment at 840 ℃ for 2.5 hours, and air cooling;
(3) then, carrying out secondary aging heat treatment at 660 ℃, wherein the aging time is 6 hours, and air cooling;
(4) and finally, carrying out third aging heat treatment at 480 ℃ for 12 hours, and cooling in air.
The content relation of Ni and Al is as follows: (Ni-8%)/Al 3.1>3, and the bactericidal rate and mechanical properties were measured as shown in Table 1.
The steel of example 2 has excellent antibacterial properties and high strength values.
Example 3
The chemical composition of the steel in weight percent is shown in table 2. Stainless steel having excellent antibacterial properties and high strength values was prepared according to the composition of steel described in table 2 and subjected to the heat treatment method as described in example 1.
Comparative example 1
The steel comprises the following chemical components in percentage by weight: c: 0.025 percent; si: 0.35 percent; mn: 0.30 percent; cu: 3.68 percent; ni: 12.2 percent; cr: 18.1 percent; n: 0.004%; s: 0.008 percent; p: 0.009%; the balance being Fe. The content relation of Ni and Al is as follows: (Ni-8%)/Al ∞.
The heat treatment mode after forging is as follows:
(1) firstly, carrying out solid solution at 1070 ℃ for 1.0 hour, and cooling in air;
(2) secondly, carrying out primary aging heat treatment at 800 ℃, wherein the aging time is 3 hours, and air cooling;
(3) then, carrying out secondary aging heat treatment at 680 ℃ for 5 hours, and air-cooling;
(4) and finally, carrying out third aging heat treatment at 500 ℃ for 10 hours, and cooling in air.
The content relation of Ni and Al is as follows: (Ni-8%)/Al ∞ >3, and the sterilization rate and mechanical property tests are shown in Table 1. Comparative example 1 the same heat treatment process as in example 1 was performed, but the composition did not contain Al and the P content in the steel was low, and the comparative example steel had excellent antibacterial property but low strength value.
Comparative example 2
The steel comprises the following chemical components in percentage by weight: c: 0.023%; si: 0.32 percent; mn: 0.25 percent; cu: 3.75 percent; ni: 12.3 percent; al: 1.35 percent; cr: 18.2 percent; n: 0.004%; s: 0.008 percent; p: 0.07 percent; the balance being Fe. The content relation of Ni and Al is as follows: (Ni-8%)/Al-3.2.
The heat treatment mode after forging is as follows:
(1) firstly, solid solution is carried out at 1070 ℃ for 0.5 hour, and air cooling is carried out;
(2) and finally, aging at 680 ℃ for 5 hours, and cooling in air.
The content relation of Ni and Al is as follows: (Ni-8%)/Al 3.2>3, and the bactericidal rate and mechanical properties were measured as shown in Table 1. Comparative example 2 and example 1 have the same chemical composition, but the heat treatment process is performed for only 1 aging, and the comparative example steel has only obtained good antibacterial property and the strength value is not maximized.
Comparative example 3
The steel comprises the following chemical components in percentage by weight: c: 0.023%; si: 0.32 percent; mn: 0.25 percent; cu: 3.75 percent; ni: 12.3 percent; al: 1.35 percent; cr: 18.2 percent; n: 0.004%; s: 0.008 percent; p: 0.07 percent; the balance being Fe. The content relation of Ni and Al is as follows: (Ni-8%)/Al-3.2.
The heat treatment mode after forging is as follows:
(1) firstly, solid solution is carried out at 1070 ℃ for 0.5 hour, and air cooling is carried out;
(2) secondly, carrying out primary aging heat treatment at 680 ℃, wherein the aging time is 5 hours, and air cooling;
(3) then, carrying out secondary aging heat treatment at 800 ℃, wherein the aging time is 3 hours, and air cooling;
(4) and finally, carrying out third aging heat treatment at 500 ℃ for 10 hours, and cooling in air.
The content relation of Ni and Al is as follows: (Ni-8%)/Al 3.2>3, and the bactericidal rate and mechanical properties were measured as shown in Table 1. Comparative example 3, which has the same chemical composition as example 1 but the order of the first and second aging heat treatment processes is opposite to example 1, has not been optimized for antibacterial performance although higher strength values are obtained.
Comparative example 4
The steel comprises the following chemical components in percentage by weight: c: 0.023%; si: 0.32 percent; mn: 0.25 percent; cu: 3.75 percent; ni: 12.3 percent; al: 1.35 percent; cr: 18.2 percent; n: 0.004%; s: 0.008 percent; p: 0.07 percent; the balance being Fe. The content relation of Ni and Al is as follows: (Ni-8%)/Al-3.2.
The heat treatment mode after forging is as follows:
(1) firstly, solid solution is carried out at 1070 ℃ for 0.5 hour, and air cooling is carried out;
(2) then, carrying out primary aging heat treatment at 800 ℃, wherein the aging time is 5 hours, and air cooling;
(3) finally, carrying out secondary aging heat treatment at 680 ℃, wherein the aging time is 3 hours, and air cooling.
The content relation of Ni and Al is as follows: (Ni-8%)/Al 3.2>3, and the bactericidal rate and mechanical properties were measured as shown in Table 1. Comparative example 4, which has the same chemical composition as example 1 but the aging heat treatment process is not subjected to low temperature aging, has not optimized strength although good antibacterial properties are obtained.
Comparative example 5
The steel comprises the following chemical components in percentage by weight: c: 0.023%; si: 0.32 percent; mn: 0.25 percent; cu: 3.75 percent; ni: 11.5 percent; al: 1.35 percent; cr: 18.2 percent; n: 0.004%; s: 0.008 percent; p: 0.07 percent; the balance being Fe. The content relation of Ni and Al is as follows: (Ni-8%)/Al 2.6.
The heat treatment mode after forging is as follows:
(1) firstly, carrying out solid solution at 1070 ℃ for 1.0 hour, and cooling in air;
(2) secondly, carrying out primary aging heat treatment at 800 ℃, wherein the aging time is 3 hours, and air cooling;
(3) then, carrying out secondary aging heat treatment at 680 ℃ for 5 hours, and air-cooling;
(4) and finally, carrying out third aging heat treatment at 500 ℃ for 10 hours, and cooling in air.
The content relation of Ni and Al is as follows: (Ni-8%)/Al 2.6<3, and the microstructure shown in fig. 2 is an austenite + martensite structure. The sterilization rate and mechanical property tests are shown in table 1. The steel of comparative example 5, although having excellent antibacterial properties and high strength values, had poor elongation and greatly decreased corrosion resistance because complete austenite was not obtained.
TABLE 1 mechanical properties and antibacterial sterilizing rates of examples and comparative examples
Table 2 chemical composition of stainless steel according to example 3
Test specimen | C | Si | Mn | Cu | Ni | Al | Cr | N | S | P |
1# | 0.018 | 0.58 | 0.56 | 4.20 | 12.8 | 1.48 | 18.8 | 0.003 | 0.007 | 0.10 |
2# | 0.030 | 0.02 | 0.01 | 3.68 | 11.9 | 1.11 | 17.9 | 0.004 | 0.008 | 0.06 |
3# | 0.025 | 0.31 | 0.22 | 3.89 | 12.5 | 1.37 | 18.0 | 0.003 | 0.007 | 0.08 |
It can be seen that the chemical composition design and heat treatment process according to the present invention can achieve excellent antibacterial properties and high strength values.
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 (7)
1. The high-strength austenitic antibacterial stainless steel is characterized by comprising the following chemical components in percentage by weight:
c: less than or equal to 0.03 percent; si: less than or equal to 1.0 percent; mn: less than or equal to 1.0 percent; cu: 3.5-4.5%; ni: 11.0-13.0%; al: 1.0-1.5%; cr: 17.0-19.0%; n: less than or equal to 0.005 percent; s is less than or equal to 0.010 percent; p: 0.05-0.10%; the balance being Fe.
2. The high strength austenitic antimicrobial stainless steel of claim 1, wherein the Ni and Al contents in the stainless steel satisfy, in weight percent: (Ni-8%)/Al is greater than or equal to 3.
3. A method for preparing the high strength austenitic antibacterial stainless steel of claim 1, comprising the steps of:
(1) mixing raw materials according to the requirements of chemical components, and obtaining a steel ingot through vacuum induction smelting and pouring;
(2) and (3) carrying out heat preservation on the steel ingot at 1250-1300 ℃ for more than 4 hours, and then forging: the initial forging temperature is 1150-1200 ℃, the final forging temperature is 1000-1100 ℃, the forging process is carried out with large rolling reduction in the longitudinal-transverse-longitudinal directions, the first rolling reduction is not more than 10%, other single rolling reduction is more than 20%, the total forging ratio is more than 12, and the forging is carried out with air cooling to the room temperature;
(3) and carrying out solid solution treatment and graded aging heat treatment after forging.
4. A method for manufacturing a high strength austenitic antimicrobial stainless steel according to claim 3, wherein the solution treatment and the step heat treatment process in the step (3) are:
1) firstly, solid solution is carried out at 1050-1100 ℃ for 0.5-2 hours, and air cooling is carried out;
2) secondly, carrying out first aging at 760-860 ℃ for 2-4 hours, and air cooling;
3) then, carrying out secondary aging at 650-700 ℃, wherein the aging time is 4-6 hours, and air cooling;
4) and finally, carrying out third aging at 450-550 ℃, wherein the aging time is 8-12 hours, and carrying out air cooling.
5. A method of manufacturing a high strength austenitic antimicrobial stainless steel according to claim 3 or 4, wherein the microstructure of the stainless steel is austenite.
6. A method for preparing a high-strength austenitic antibacterial stainless steel as claimed in claim 3 or 4, characterized in that the yield strength of the stainless steel is more than or equal to 400MPa, the tensile strength is more than or equal to 1000MPa, and the elongation is more than or equal to 40.0%.
7. A method of making a high strength austenitic antimicrobial stainless steel as claimed in claim 3 or 4, wherein the stainless steel has an antimicrobial rate of > 99% against E.coli and > 99% against Staphylococcus aureus.
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