CN112935265A - Preparation method of high-strength powder austenitic stainless steel - Google Patents
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Abstract
A preparation method of high-strength powder austenitic stainless steel belongs to the field of powder metallurgy. The invention takes titanium-containing stainless steel powder prepared by water-gas combined atomization as a raw material, zirconium hafnium powder is added as a carbon fixing agent and an oxygen fixing agent, and the zirconium hafnium powder and the atomized steel powder are subjected to high-energy ball milling, forming, sintering and heat treatment to obtain a high-strength powder stainless steel product. Zirconium, hafnium and titanium belong to the same group of elements, the chemical properties are similar, when the zirconium, hafnium and titanium are added into a stainless steel system, intergranular corrosion can be further prevented, and meanwhile, three elements of Ti, Zr (Hf) and O form an ordered phase in the sintering and heat treatment processes, so that the effects of reducing the oxygen content of a steel matrix and strengthening a second phase are achieved, the plasticity of the steel matrix is improved, the material strength is greatly improved, and further, a high-strength powder stainless steel product is obtained. The invention has the advantages of simple preparation process, no need of additional equipment, high production efficiency, no pollution and impurities, excellent performance and the like.
Description
Technical Field
The invention belongs to the field of powder metallurgy, and provides a preparation method of high-strength powder austenitic stainless steel.
Background
The high-strength stainless steel has excellent obdurability matching and corrosion resistance, is widely applied to the field of equipment manufacturing of national civilians in relation to aerospace, ocean engineering, energy and the like, such as main bearing members of airplanes, fasteners, satellite gyroscopes, airship shells, ocean oil platforms, automobile industry, nuclear energy industry, gear and bearing manufacturing and the like, and is a preferred material for lightweight design, energy conservation and emission reduction of future equipment parts.
At present, much research and development on high-strength stainless steel is focused on martensitic precipitation hardening stainless steel, maraging steel and the like, and the main strengthening modes are low-carbon martensitic transformation strengthening and NiAl and Ni3Strengthening intermetallic compounds such as Ti. In austenitic stainless steels, however, since there is no transformation in the heating temperature range, the steel cannot be subjected to transformation strengthening by heat treatment, and generally, strengthening is performed only by cold working, and uniform precipitation strengthening of carbides occurs by aging after cold deformation. However, carbide precipitation may cause the generation of chromium-poor regions to deteriorate the intergranular corrosion performance thereof, and thus it is important how to avoid the generation of chromium-poor regions and effectively improve the strength of austenitic stainless steel.
In addition, the presence of oxygen in stainless steel adversely affects its yield and performance. The oxygen content in the powder metallurgy stainless steel product is mainly determined by powder raw materials, and the content is generally much higher than that of the stainless steel product prepared by the traditional fusion casting method, so that a certain method is needed to effectively fix the oxygen and the oxygen is required to exist in the stainless steel as a strengthening phase.
Disclosure of Invention
The invention aims to provide a preparation method of high-strength powder austenitic stainless steel. The method takes titanium-containing stainless steel powder prepared by water-gas combined atomization as a raw material, zirconium hafnium powder as a carbon fixing agent and an oxygen fixing agent is added, and the zirconium hafnium powder and the atomized powder are subjected to high-energy ball milling, forming, sintering and heat treatment to obtain a high-strength powder stainless steel product. Firstly, Zr, Hf and Ti belong to the same group elements and have similar chemical properties, and the performance of the titanium-containing stainless steel is not adversely affected by adding a small amount of zirconium and hafnium into the titanium-containing stainless steel matrix. Secondly, the zirconium hafnium powder is used as a carbon fixing agent, and under the synergistic action of titanium in the stainless steel, the absorption and fixation effects on carbon are greatly enhanced, and a chromium-poor area is avoided, so that the intergranular corrosion resistance of the steel is further improved. Meanwhile, in the sintering process, three elements of Ti, Zr (Hf) and O form an ordered phase, so that the effects of reducing the oxygen content in a steel matrix and strengthening a second phase are achieved. In this case, even if the oxygen content in the powdered stainless steel article is high, the oxygen element in the steel matrix is deprived by Zr, Hf and Ti elements to form a Ti-Zr (Hf) -O ordered phase, so that the oxygen content in the steel matrix is greatly reduced. Moreover, the Ti-Zr (Hf) -O ordered phase can play a role in strengthening the stainless steel, so that the strength of the material is greatly improved. In addition, the Zr content and the Hf content in the system can be regulated and controlled according to application requirements, oxygen in the stainless steel is fixed to the maximum extent, adverse effects of solid dissolved oxygen on ductility are reduced, ordered strengthening phases are generated, and then a high-strength powder stainless steel product is obtained. The method has the advantages of simple process, no need of additional equipment, high production efficiency and contribution to promoting the development of the powdered stainless steel industry.
In order to obtain the preparation method of the high-strength powder austenitic stainless steel, the preparation method is characterized in that zirconium and hafnium are added into a titanium-containing stainless steel system as a carbon fixing agent and an oxygen fixing agent, so that the dual improvement of the corrosion resistance and the mechanical property is realized, and the specific preparation steps are as follows:
(1) preparing Ti-containing stainless steel powder by water-gas combined atomization, wherein the Ti-containing stainless steel powder comprises 316Ti (0Cr18Ni12Mo2Ti) or 321(0Cr18Ni10Ti) and the like;
(2) weighing atomized stainless steel powder and zirconium hafnium powder in a glove box protected by argon according to the mass ratio of 99.6:0.4-97:3, loading into a mixing tank, and then carrying out high-energy ball milling for 12-36h, wherein the ball-material ratio is 10:1-30:1, so as to obtain uniform mechanical alloying powder;
(3) carrying out high-temperature vacuum annealing on the mechanical alloying powder at the annealing temperature of 800-950 ℃, keeping the temperature for 2-4h, fully removing the work hardening brought by high-energy ball milling of the powder, and then crushing and screening to obtain the required alloy powder;
(4) alloy powder is filled into a cold isostatic pressing sheath and compacted, cold isostatic pressing forming is carried out after sealing, the pressing pressure is 180-400MPa, and the pressure maintaining time is 1-4min, so as to obtain a green body;
(5) placing the green body in a sintering furnace for vacuum sintering with a vacuum degree of 10-2-10-1Pa, the sintering temperature is 1320 ℃ at 1200 and the temperature is kept for 2-4h and then taken out;
(6) and putting the taken sintered sample into an argon furnace for solution treatment, and cooling to finally obtain the high-strength powder metallurgy stainless steel product.
Further, the stainless steel powder in step (1) has a particle size in the range of 8-30 μm and an oxygen content of 480-960 ppm.
Further, the zirconium hafnium powder in the step (2) is one or two of pure zirconium powder and pure hafnium powder, the purity of the powder is more than or equal to 99.5%, and the granularity is 1-10 μm.
Further, the sheath in the step (4) is a polyurethane, rubber or silica gel elastic sheath, and the shape of the sheath is designed and manufactured according to actual production needs.
Further, the solution treatment temperature in the step (6) is 900-.
The key points of the technology of the invention are as follows: (1) through a large number of experiments, the mass percent of the zirconium and the hafnium sponge is determined to be 0.4-3 wt% by combining the carbon content and the oxygen content of the atomized stainless steel powder and the comprehensive performance of the final product. (2) In order to reduce the influence of the added elements on the characteristics of the stainless steel, the grade of the stainless steel containing titanium is selected as a system as far as possible. (3) In order to reduce the adverse effect of the carbon content and the oxygen content in the atomized powder on the stainless steel, zirconium and hafnium are used as a carbon fixing agent and an oxygen fixing agent, and the characteristics of similar properties of zirconium, hafnium and titanium are utilized to cooperate with carbon fixing and oxygen fixing in a steel matrix to mainly generate a Ti-Zr (Hf) -O ordered phase, so that the oxygen content in the matrix is reduced, the matrix strengthening effect is realized, and the Zr content and the Hf content in a system can be flexibly regulated and controlled to ensure that the carbon content and the oxygen content in the matrix are fixed to the maximum extent. (4) The high-strength powder stainless steel product is prepared by a powder metallurgy process, the problem of high oxygen in stainless steel powder is effectively solved, the dispersion strengthening effect of nano oxides is realized, and a new thought is provided for preparing the powder metallurgy high-strength stainless steel.
The invention has the advantages that:
1. the added zirconium, hafnium and titanium have similar properties, and the titanium-containing stainless steel is not adversely affected when a small amount of the zirconium, hafnium and titanium is added.
2. The zirconium hafnium powder is used as a carbon fixing agent, and under the synergistic action of titanium in the stainless steel, the carbon fixing effect is enhanced, and a chromium-poor area is avoided, so that the intergranular corrosion resistance of the steel is further improved.
3. The zirconium hafnium powder is used as an oxygen fixing agent, and can form a Ti-Zr (Hf) -O ordered phase with titanium and oxygen elements in the stainless steel powder in the sintering process, so that the oxygen content in a steel matrix is greatly reduced, and meanwhile, the ordered phase can play a role in strengthening and effectively improve the mechanical property of the material.
4. According to application requirements, the Zr content and the Hf content in the system can be flexibly regulated and controlled, oxygen in the stainless steel can be fixed to the maximum extent, adverse effects of solid dissolved oxygen on ductility of a steel matrix can be reduced, and a high-strength powder metallurgy stainless steel product can be obtained.
5. The method has the advantages of simple preparation process, no need of additional equipment and process steps, strong applicability and suitability for large-scale industrial production.
Detailed Description
Example 1:
(1) preparing 316Ti alloy powder by water-gas combined atomization, wherein the granularity of the powder is 25 mu m, and the oxygen content of the powder is 540 ppm;
(2) weighing atomized stainless steel powder and 5-micron zirconium powder in a weight ratio of 99.5:0.5 in an argon-protected glove box, loading into a mixing tank, and then performing high-energy ball milling for 20 hours according to a ball-to-material ratio of 10:1 to obtain uniform mechanical alloying powder;
(3) carrying out vacuum annealing on the mechanical alloying powder at 900 ℃ for 2h, fully removing work hardening brought by high-energy ball milling of the powder, and then crushing and screening to obtain the required alloy powder;
(4) filling alloy powder into a silica gel sheath, compacting, sealing, and performing cold isostatic pressing at a pressing pressure of 200MPa for 2min to obtain a green body;
(5) placing the green body in a sintering furnace for vacuum sintering with a vacuum degree of 10-2Pa, the sintering temperature is 1250 ℃, and the sintering temperature is taken out after heat preservation for 3 hours;
(6) and (3) carrying out solution treatment on the taken out sintered sample in an argon furnace for 1000-4 h, and air cooling to finally obtain a high-strength powder stainless steel product.
Example 2:
(1) 321 alloy powder is prepared by water-gas combined atomization, the particle size of the powder is 10 mu m, and the oxygen content of the powder is 820 ppm;
(2) weighing atomized stainless steel powder and 8-micron hafnium powder in a 98.0:2.0 mass ratio in an argon-protected glove box, loading into a mixing tank, and performing high-energy ball milling for 12 hours according to a ball-to-material ratio of 15:1 to obtain uniform mechanical alloying powder;
(3) carrying out vacuum annealing on the mechanical alloying powder at 930 ℃ for 3h, fully removing work hardening brought by high-energy ball milling of the powder, and then crushing and screening to obtain the required alloy powder;
(4) filling alloy powder into a rubber sheath, compacting, sealing, and performing cold isostatic pressing at 300MPa for 1.5min to obtain a green body;
(5) placing the green body in a sintering furnace for vacuum sintering with a vacuum degree of 10-2Pa, the sintering temperature is 1300 ℃, and the sintering temperature is kept for 2 hours and then taken out;
(6) and (3) performing solid solution treatment on the taken sintering sample in an argon furnace for 1050-3 h, and air cooling to finally obtain a high-strength powder stainless steel product.
Claims (5)
1. A preparation method of high-strength powder austenitic stainless steel is characterized in that zirconium and hafnium are added into a titanium-containing stainless steel system as a carbon fixing agent and an oxygen fixing agent, so that double improvement of corrosion resistance and mechanical property is realized, and the preparation method specifically comprises the following steps:
(1) preparing Ti-containing stainless steel powder by water-gas combined atomization, wherein the Ti-containing stainless steel powder comprises 316Ti (0Cr18Ni12Mo2Ti) or 321(0Cr18Ni10 Ti);
(2) weighing atomized stainless steel powder and zirconium hafnium powder in a glove box protected by argon according to the mass ratio of 99.6:0.4-97:3, loading into a mixing tank, and then carrying out high-energy ball milling for 12-36h, wherein the ball-material ratio is 10:1-30:1, so as to obtain uniform mechanical alloying powder;
(3) carrying out high-temperature vacuum annealing on the mechanical alloying powder at the annealing temperature of 800-950 ℃, keeping the temperature for 2-4h, fully removing the work hardening brought by high-energy ball milling of the powder, and then crushing and screening to obtain the required alloy powder;
(4) alloy powder is filled into a cold isostatic pressing sheath and compacted, cold isostatic pressing forming is carried out after sealing, the pressing pressure is 180-400MPa, and the pressure maintaining time is 1-4min, so as to obtain a green body;
(5) placing the green body in a sintering furnace for vacuum sintering with a vacuum degree of 10-2-10-1Pa, the sintering temperature is 1320 ℃ at 1200 and the temperature is kept for 2-4h and then taken out;
(6) and putting the taken sintered sample into an argon furnace for solution treatment, and cooling to finally obtain the high-strength powder metallurgy stainless steel product.
2. A method of making a high strength powdered austenitic stainless steel as claimed in claim 1, wherein: the stainless steel powder in the step (1) has a particle size range of 8-30 μm and an oxygen content of 480-960 ppm.
3. A method of making a high strength powdered austenitic stainless steel as claimed in claim 1, wherein: the zirconium hafnium powder in the step (2) is one or two of pure zirconium powder and pure hafnium powder, the purity of the powder is more than or equal to 99.5%, and the granularity is 1-10 mu m.
4. A method of making a high strength powdered austenitic stainless steel as claimed in claim 1, wherein: the sheath in the step (4) is a polyurethane, rubber or silica gel elastic sheath, and the shape of the sheath is designed and manufactured according to actual production needs.
5. A method of making a high strength powdered austenitic stainless steel as claimed in claim 1, wherein: the solution treatment temperature in the step (6) is 900-1150 ℃, the temperature is kept for 2-4h, and the cooling mode is air cooling.
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| CN113500196A (en) * | 2021-07-14 | 2021-10-15 | 燕山大学 | Method for improving high-temperature oxidation resistance of austenitic stainless steel by regulating and controlling nano-network distribution of Si |
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