CN118268556B - A modified 17-4PH high-toughness stainless steel material and preparation method thereof - Google Patents
A modified 17-4PH high-toughness stainless steel material and preparation method thereof Download PDFInfo
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Abstract
本申请涉及金属材料领域，具体公开了一种改性17‑4PH高韧性不锈钢材料及其制备方法。一种改性17‑4PH高韧性不锈钢材料，包括以下重量份的原料：100份不锈钢粉末、6‑8份粘结剂、0.1‑0.4份钛粉、0.2‑1份铝粉和0.15‑0.2份石墨烯，不锈钢粉末包括质量比为7‑9:1‑3的17‑4PH不锈钢粉末和304不锈钢粉末。本申请的改性17‑4PH高韧性不锈钢材料通过将304不锈钢粉末和17‑4PH不锈钢粉末配合作用，能结合奥氏体不锈钢材料和马氏体沉淀硬化不锈钢材料的优点，制成的不锈钢材料具有较好的韧性和塑性，而且耐腐蚀性强。The present application relates to the field of metal materials, and specifically discloses a modified 17‑4PH high-toughness stainless steel material and a preparation method thereof. A modified 17‑4PH high-toughness stainless steel material comprises the following raw materials in parts by weight: 100 parts of stainless steel powder, 6‑8 parts of binder, 0.1‑0.4 parts of titanium powder, 0.2‑1 parts of aluminum powder and 0.15‑0.2 parts of graphene, and the stainless steel powder comprises 17‑4PH stainless steel powder and 304 stainless steel powder in a mass ratio of 7‑9:1‑3. The modified 17‑4PH high-toughness stainless steel material of the present application combines the advantages of austenitic stainless steel material and martensitic precipitation hardening stainless steel material by combining 304 stainless steel powder and 17‑4PH stainless steel powder, and the prepared stainless steel material has good toughness and plasticity, and strong corrosion resistance.
Description
Technical Field
The application relates to the technical field of metal materials, in particular to a modified 17-4PH high-toughness stainless steel material and a preparation method thereof.
Background
The 17-4PH stainless steel is typical martensitic precipitation hardening stainless steel, has the characteristics of excellent corrosion resistance, high temperature resistance, wear resistance, creep resistance, good appearance luster and the like, has high forming strength, can meet the processing requirements of large-size 3D printing parts, and has wide application in various fields of medical appliances, automobiles, military industry, aviation, nuclear industry and the like.
Metal Injection Molding (MIM) is a molding method in which a mixture of metal powder and binder is injected into a mold, first, the selected metal powder and binder are mixed, then the mixture is granulated, and then injection molded into a desired shape. The binder imparts its viscous flow characteristics to the mix, while helping uniformity in forming, cavity filling and powder loading. Removing the binder after forming, sintering the degreased blank, and further densification treatment, heat treatment or machining the sintered product. The sintered product not only has the same complex shape and high precision as the product obtained by the plastic injection molding method, but also has physical, chemical and mechanical properties close to those of the forging. MIM technology combines the advantages of two technologies of powder metallurgy and plastic injection molding, breaks through the limitation of the traditional metal powder compression molding technology on the shape of the product, and simultaneously utilizes the characteristic that the plastic injection molding technology can form parts with complex shapes in a large batch with high efficiency, thereby becoming a molding technology for manufacturing high-quality precision parts in modern times, and having the advantages which are incomparable with the conventional processing methods of powder metallurgy, machining, precision casting and the like.
However, due to the tissue characteristics of 17-4PH, the toughness is poor, the rigidity is strong, and the shaping is difficult to correct deformation, so that when the blank is repaired after injection molding, the blank is fragile and has low toughness, the product is broken, the reject ratio is increased, and the operation efficiency is affected.
Disclosure of Invention
In order to improve the toughness of a 17-4PH material, improve the shaping effect of a product and improve the operation efficiency, the application provides a modified 17-4PH high-toughness stainless steel material and a preparation method thereof.
In a first aspect, the application provides a modified 17-4PH high-toughness stainless steel material, which adopts the following technical scheme:
A modified 17-4PH high-toughness stainless steel material comprises, by weight, 100 parts of stainless steel powder, 6-8 parts of a binder, 0.1-0.4 part of titanium powder, 0.2-1 part of aluminum powder and 0.15-0.2 part of graphene, wherein the stainless steel powder comprises 17-4PH stainless steel powder and 304 stainless steel powder in a mass ratio of 7-9:1-3.
By adopting the technical scheme, the mixture of the 17-4PH stainless steel powder and the 304 stainless steel powder is used as a base material, the 17-4PH stainless steel powder has better strength and hardness, and the 304 stainless steel powder belongs to an austenitic stainless steel material and has higher toughness and plasticity, so that the toughness and plasticity of a 17-4PH stainless steel product can be improved, brittleness is reduced, in addition, the introduction of graphene can play a role in obstructing grain boundary migration and refining grains, when the stainless steel material breaks, the breaking of graphene, the conversion of crack pieces and the extraction of graphene can enable the graphene to consume the expansion energy of cracks in various forms in the material, thereby increasing the crack expansion path in the stainless steel material, improving the crack expansion resistance, improving the fracture toughness, improving the compactness of the stainless steel material, improving the hardness and the impact resistance, fully strengthening a matrix by the titanium powder, being capable of reacting with nickel in the 17-4PH stainless steel powder, and obtaining a disordered oxidation-resistant aluminum oxide layer through stronger bond bonding and complex atomic arrangement by becoming ordered metal compounds in the stainless steel material, thereby having higher oxidation-free property and improving the oxidation-free property when the oxidation-resistant layer is formed on the stainless steel material; the titanium powder and the aluminum powder are matched, so that the toughness of the stainless steel material can be effectively improved, titanium carbide can be formed after the titanium powder and the graphene are sintered, the titanium powder and the graphene are in a quasi-continuous network division, load can be borne, grain boundaries are reinforced, the plastic deformation of a large degree is realized, good interface strength is ensured, a network structure has good bearing capacity, main load can be borne, and the strength and the elastic modulus are improved.
Optionally, the graphene is subjected to the following modification pretreatment:
adding graphene into absolute ethyl alcohol, adding a dispersing agent, and performing ultrasonic dispersion to obtain graphene suspension;
Adding nano titanium nitride and yttrium oxide into the suspension, performing ultrasonic dispersion for 20-30min, performing ball milling for 20-24h, and performing vacuum drying to obtain graphene, nano titanium nitride and yttrium oxide in a ratio of 1:10-15:0.15-0.2.
By adopting the technical scheme, polyvinylpyrrolidone is used as a dispersing agent, the dispersing effect of graphene can be improved through the synergistic effect of an electrostatic dispersing mechanism and a steric hindrance dispersing mechanism, nano titanium nitride can promote grain growth, prevent crack growth, enhance the toughness of a material, and yttrium oxide can play a role in pinning and inhibit grain boundary diffusion and surface diffusion of grains so as to inhibit growth of the grains, so that the effect of graphene on promoting grain growth of a stainless steel material can be improved by utilizing nano titanium nitride and yttrium oxide, the comprehensive performance of the stainless steel material can be improved, and the yttrium oxide can play a role in strengthening a bonding phase, thereby improving the corrosion resistance of the stainless steel material.
Optionally, the adding amount of the titanium powder is 9% -30% of the total mass of the titanium powder and the aluminum powder.
By adopting the technical scheme, the using amount of the titanium powder and the aluminum powder is in the above range, so that the brittleness of the stainless steel material can be effectively reduced, and the toughness and the plasticity can be increased.
Optionally, the binder comprises polyethylene glycol, polyvinylidene fluoride, sodium silicate and stearic acid in a mass ratio of 7-8:2-3:1-1.5:0.5-1.
Through adopting above-mentioned technical scheme, liquid sodium silicate has lubrication action and anticorrosion effect, when mixing with stainless steel powder, can be with stainless steel powder composition hydrophilic, make stainless steel powder have better mobility and lubricity, more be fit for injection molding, the green body appearance of shaping is complete, the inside hole is less, the internal structure is regular, and still can keep original shape and external defect free after degreasing, but sodium silicate belongs to hydrophilic structure, the long-term anticorrosive action of stainless steel material can be influenced to too high hygroscopicity, so use the polyvinylidene fluoride of hydrophobic structure to cooperate sodium silicate, polyvinylidene fluoride can not take place the moisture absorption phenomenon under humid environment, so both complementary in the aspect of moisture resistance and corrosion resistance, when promoting stainless steel material corrosion resistance, reduce the moisture absorption rate.
Optionally, the binder further comprises an auxiliary impregnating compound, the mass ratio of the auxiliary impregnating compound to the polyethylene glycol is 0.2-0.8:1, and the preparation method of the auxiliary impregnating compound is as follows:
Mixing silicon powder and crystalline flake graphite, grinding for 15-20min, adding NaCl-NaF mixed salt, continuously grinding for 15-20min, heating to 1300-1350 ℃ under argon atmosphere, preserving heat for 2.5-3h, cooling to room temperature, washing with distilled water, and drying at 100-110 ℃ for 12-14h, wherein the mass ratio of the silicon powder to the crystalline flake graphite is 1:2-3.
According to the technical scheme, the fused salt is used as a medium, the mass transfer speed is remarkably improved based on the dissolution of silicon in the fused salt, meanwhile, the silicon carbide uniformly diffuses to the graphite surface and generates nano silicon carbide in situ, the graphite powder is coated by the silicon carbide, a large number of silicon carbide crystal nuclei exist on the silicon carbide coated graphite surface, the wettability between the stainless steel powder and the binder is improved, the binding force between the stainless steel powder and the binder is improved, firm binding is formed after heat treatment, the reinforced and toughened stainless steel material has a reinforcing and toughening effect, and when the stainless steel material is subjected to external force, the expansion path of cracks can be effectively increased due to the debonding, crack deflection, bridging, pulling-out and the like of the internal nano silicon carbide, so that the mechanical property of the stainless steel material can be increased.
Optionally, the grain size of the silicon powder is 1-9 mu m, and the grain size of the crystalline flake graphite is 45-75 mu m.
By adopting the technical scheme, the silicon powder with smaller grain diameter can be rapidly diffused onto the crystalline flake graphite with larger grain diameter under the molten salt medium, and the silicon carbide whisker can be formed by in-situ growth on the surface of the crystalline flake graphite.
Optionally, the particle size of the 17-4PH stainless steel powder is 15-53 mu m.
Optionally, the tap density of the 304 stainless steel powder is 3.9-4.2g/cm 3, the fluidity is less than or equal to 30s/50g, and the compressibility is more than or equal to 6.55g/cm 3.
In a second aspect, the application provides a preparation method of a modified 17-4PH high-toughness stainless steel material, which adopts the following technical scheme:
a preparation method of a modified 17-4PH high-toughness stainless steel material comprises the following steps:
Adding titanium powder and graphene into absolute ethyl alcohol, performing ultrasonic mixing, performing ball milling, then heating to 550-600 ℃, and performing heat preservation for 4-6min under the pressure of 40-50MPa to prepare premix;
uniformly mixing the premix with stainless steel powder and aluminum powder, and banburying for 20-30min at 100-160 ℃ to obtain mixed powder;
mixing the mixed powder with binder, stirring at 160-165 deg.C, granulating, injection molding, degreasing, and heat treating.
Through adopting above-mentioned technical scheme, the graphite alkene exists stronger interlaminar van der Waals 'force, have relatively poor chemical compatibility and wettability with titanium powder, aluminium powder etc. for graphite alkene is easy to agglomerate, disperse unevenly, consequently be difficult to guarantee stainless steel material's compactness first, so mix graphite alkene with titanium powder earlier, after the sintering of low temperature, the grain can refine, the grain of refinement plays fine-grained reinforcement effect on the one hand, on the other hand can improve plasticity, powder grain boundary usually evolves into the grain boundary, so graphite alkene on powder particle surface is located the grain boundary after sintering often, graphite alkene in grain boundary department obstructs the migration of grain boundary, make graphite alkene strengthen titanium powder, consequently, can also further increase titanium powder's plasticity when improving graphite alkene homogeneity, thereby improve stainless steel material's bearing capacity, improve toughness.
Optionally, the specific method of the heat treatment is that solution treatment is carried out for 1-2h at 925-1040 ℃, and cryogenic treatment is carried out for 1-2h at (-10-0) °c.
By adopting the technical scheme, the porosity of the degreased product after heat treatment is reduced, grains can be refined, dislocation movement is prevented, the strength of the degreased product is improved, and the corrosion resistance effect is improved.
In summary, the application has the following beneficial effects:
1. According to the application, the toughness of the 17-4PH stainless steel powder is improved by adopting the 304 stainless steel powder, and a certain amount of titanium powder, aluminum powder and graphene are added, so that titanium carbide can be formed by the titanium powder and the graphene, a continuous network division is presented in the stainless steel material, the bearing capacity of the stainless steel material is improved, the titanium powder can fully strengthen a matrix, the aluminum powder can be used for layering ordered metal compounds, and a compact aluminum oxide protective layer is generated during high-temperature mixing, so that the plasticity and fracture toughness of the stainless steel material are improved.
2. According to the application, the graphene is preferably pretreated by adopting the nano titanium nitride and the yttrium oxide, the grains of the titanium nitride and the yttrium oxide can be refined, and the structure of the stainless steel material is more uniform and compact, so that the hardness and fracture toughness of the material are improved, and the corrosion resistance of the material can be further improved by the yttrium oxide.
3. In the application, polyethylene glycol, polyvinylidene fluoride, sodium silicate and stearic acid are preferably adopted to prepare the adhesive, so that the fluidity and filling property of stainless steel powder can be improved, the corrosion resistance of a stainless steel material can be improved by mixing the sodium silicate and the polyvinylidene fluoride, and in addition, a certain auxiliary impregnating agent is added into the adhesive, so that the impregnating capability of the adhesive on the stainless steel powder can be improved, the interface bonding effect can be improved, and the compactness can be improved.
Detailed Description
The following examples illustrate the application in further detail.
Examples
The modified 17-4PH high-toughness stainless steel material is shown in the table 1, wherein the stainless steel powder comprises 80kg of 17-4PH stainless steel powder mixed with 20kg of 304 stainless steel powder, the particle size of the 17-4PH stainless steel powder is 53 mu m, and the modified 17-4PH high-toughness stainless steel material comprises the following components, by mass, of Cr17.5wt%, ni5wt%, cu5wt%, nb0.45wt%, C0.07wt%, si1.0wt%, mn1.0wt%, P0.04wt%, S0.03wt%, the balance being Fe, the tap density of 304 stainless steel powder is 4.2g/cm 3, the fluidity is less than or equal to 30S/50g, the compressibility is more than or equal to 6.55g/cm 3, and the modified 17-4PH stainless steel material comprises the following components, by mass, cr20wt%, ni12wt%, mn0.2wt%, si0.8wt%, C <0.03wtt wt%, P0.03 wt%, S0.02 wt%, O <0.3wt%, the balance being Fe < 7:20000.0 wt%, the vinyl alcohol powder is mixed with the polyvinyl butyral solution, the vinyl alcohol powder is prepared by mixing, the vinyl alcohol powder is 70 kg of polyvinyl butyral cement, the polyvinyl alcohol powder is prepared by adding the polyvinyl alcohol powder, the polyvinyl alcohol powder is equal to 2000 kg, and the total weight of the polyvinyl alcohol powder is equal to or 7kg, and the polyvinyl alcohol powder is equal to or 70 kg of the polyvinyl alcohol powder;
the preparation method of the modified 17-4PH high-toughness stainless steel material comprises the following steps:
S1, adding titanium powder and graphene into absolute ethyl alcohol, performing ultrasonic mixing, performing ball milling, then heating to 600 ℃, and performing heat preservation for 6min under the pressure of 40MPa to obtain a premix;
s2, uniformly mixing the premix with stainless steel powder and aluminum powder, and banburying for 20min at 160 ℃ to obtain mixed powder;
S3, mixing the mixed powder with a binder, stirring at 160 ℃, and granulating to obtain a spare material with the tap density of 4.68g/cm 3;
S4, injecting and forming the standby material on an injection machine to obtain an injection blank, wherein the injection temperature is 200 ℃, the injection pressure is 100MPa, and the mold temperature is 120 ℃;
S5, catalytically degreasing the injection blank by using nitric acid to obtain a degreased blank, wherein the degreasing temperature is 110 ℃, the acid flux is 3.5ml/min, and the acid flux time is 2 hours;
s6, carrying out heat treatment on the degreased blank, wherein the heat treatment process is that solution treatment is carried out for 1h at 1040 ℃ and deep cooling treatment is carried out for 1h at 0 ℃.
TABLE 1 raw material amounts of modified 17-4PH stainless Steel materials in examples 1-4
| Raw materials/kg | Example 1 | Example 2 | Example 3 | Example 4 |
| Stainless steel powder | 100 | 100 | 100 | 100 |
| Adhesive agent | 8 | 8 | 8 | 6 |
| Titanium powder | 0.1 | 0.4 | 0.4 | 0.1 |
| Aluminum powder | 1 | 1 | 0.2 | 0.2 |
| Graphene | 0.2 | 0.2 | 0.2 | 0.15 |
Examples 2-4A modified 17-4PH high toughness stainless steel material was different from example 1 in that the raw materials were used in the amounts shown in Table 1.
Example 5A modified 17-4PH high toughness stainless steel material, differing from example 1 in that graphene was subjected to the following modification pretreatment:
adding 0.2kg of graphene into 5kg of absolute ethyl alcohol, adding 0.02kg of dispersing agent, and performing ultrasonic dispersion to obtain graphene suspension, wherein the dispersing agent is polyvinylpyrrolidone;
Adding nano titanium nitride and yttrium oxide into the suspension, performing ultrasonic dispersion for 30min at the power of 200W, performing ball milling for 24h, wherein the ball-material ratio is 5:1, the ball milling rotating speed is 300r/min, and performing vacuum drying at 100 ℃ for 2h, wherein the particle size of the nano titanium nitride is 20nm, and the particle size of the yttrium oxide is 1.5 mu m, and the particle size of the graphene, the nano titanium nitride and the yttrium oxide is 1:15:0.2.
Example 6A modified 17-4PH high toughness stainless steel material, differing from example 1 in that graphene was subjected to the following modification pretreatment:
adding 0.2kg of graphene into 5kg of absolute ethyl alcohol, adding 0.02kg of dispersing agent, and performing ultrasonic dispersion to obtain graphene suspension, wherein the dispersing agent is polyvinylpyrrolidone;
adding nano titanium nitride and yttrium oxide into the suspension, performing ultrasonic dispersion for 20min at the power of 200W, performing ball milling for 20h, wherein the ball-material ratio is 5:1, the ball milling rotating speed is 300r/min, and performing vacuum drying for 2h at 100 ℃, wherein the particle size of the nano titanium nitride is 20nm, and the particle size of the yttrium oxide is 1.5 mu m, and the graphene, the nano titanium nitride and the yttrium oxide are 1:10:0.15.
Example 7A modified 17-4PH high toughness stainless Steel Material, differing from example 5 in that no nano titanium nitride was added when modification pretreatment was performed on graphene
Example 8A modified 17-4PH high toughness stainless steel material is different from example 5 in that yttrium oxide is not added when modification pretreatment is performed on graphene.
Example 9A modified 17-4PH high toughness stainless steel material, which is different from example 5 in that the binder comprises polyethylene glycol, polyvinylidene fluoride, sodium silicate and stearic acid in a mass ratio of 7:2:1.5:1, polyethylene glycol 20000 is selected from Jiangsu Heng chemical industry Co., ltd., product number is P045, and the binder is prepared by adding 7kg polyethylene glycol into water to form a 70% solution, adding 2kg polyvinyl butyral, 1.5kg liquid sodium silicate and 1kg stearic acid, and mixing uniformly.
Example 10A modified 17-4PH high toughness stainless steel material, differing from example 5 in that the binder comprises polyethylene glycol, polyvinylidene fluoride, sodium silicate and stearic acid in a mass ratio of 8:3:1:0.5, polyethylene glycol 20000 is selected from Jiangsu Heng chemical Co., ltd., product number P045, and the binder is prepared by adding 8kg polyethylene glycol into water to form a 70% strength solution, adding 3kg polyvinylidene fluoride, 1kg liquid sodium silicate and 0.5kg stearic acid, and mixing uniformly.
Example 11A modified 17-4PH high toughness stainless steel material, which is different from example 9 in that the binder is prepared by adding 7kg of polyethylene glycol into water to form a solution with the concentration of 70%, adding 2kg of polyvinyl butyral, 1.5kg of liquid sodium silicate and 1kg of stearic acid, uniformly mixing, then adding an auxiliary impregnating compound, uniformly mixing, wherein the mass ratio of the auxiliary impregnating compound to the polyethylene glycol is 0.8:1, and the auxiliary impregnating compound is prepared by the following steps:
Mixing silicon powder and crystalline flake graphite, grinding for 15min, adding NaCl-NaF mixed salt, continuously grinding for 15min, heating to 1300 ℃ under argon atmosphere, preserving heat for 3h, cooling to room temperature, washing with distilled water repeatedly until the salt disappears, drying for 12h at 110 ℃, wherein the mass ratio of the silicon powder to the crystalline flake graphite is 1:3, the grain diameter of the silicon powder is 9 mu m, and the grain diameter of the crystalline flake graphite is 45 mu m.
Example 12A modified 17-4PH high toughness stainless steel material, which is different from example 9 in that the binder is prepared by adding 7kg of polyethylene glycol into water to form a solution with the concentration of 70%, adding 2kg of polyvinyl butyral, 1.5kg of liquid sodium silicate and 1kg of stearic acid, uniformly mixing, then adding an auxiliary sizing agent, uniformly mixing, wherein the mass ratio of the auxiliary sizing agent to the polyethylene glycol is 0.2:1, and the auxiliary sizing agent is prepared by the following steps:
Mixing silicon powder and crystalline flake graphite, grinding for 20min, adding NaCl-NaF mixed salt, continuously grinding for 20min, heating to 1350 ℃ under argon atmosphere, preserving heat for 2.5h, cooling to room temperature, washing with distilled water repeatedly until the salt disappears, drying at 100 ℃ for 14h, wherein the mass ratio of the silicon powder to the crystalline flake graphite is 1:2, the grain size of the silicon powder is 9 mu m, and the grain size of the crystalline flake graphite is 45 mu m.
Comparative example
Comparative example 1A modified 17-4PH high toughness stainless steel material is different from example 1 in that titanium powder, aluminum powder and graphene are not added.
Comparative example 2 a modified 17-4PH high toughness stainless steel material was distinguished from example 1 in that no graphene was added.
Comparative example 3a modified 17-4PH high toughness stainless steel material was distinguished from example 1 in that no aluminum powder was added.
Comparative example 4A method for preparing a modified 17-4PH high toughness stainless steel material is different from example 1 in that step S1 is to uniformly mix titanium powder and graphene to prepare a premix.
Comparative example 5A method for preparing a modified 17-4PH high toughness stainless steel material is different from example 1 in that the heat treatment of step S6 is not performed.
Comparative example 6A method for producing a modified 17-4PH high toughness stainless steel material is different from example 1 in that the heat treatment in step S6 is not performed with the cryogenic treatment.
Comparative example 7A method for preparing a modified 17-4PH high toughness stainless steel material is different from example 1 in that the heat treatment process in step S6 is solution treatment at 1040 ℃ for 1 hour and failure treatment at 550 ℃ for 1 hour.
Comparative example 8A method for preparing a stainless steel mixed material feed, (1) taking 304 stainless steel powder 1kg and 17-4PH stainless steel powder 19kg, uniformly mixing the two materials, pouring the materials into a mixer, preheating the materials at 180 ℃ for 25min while uniformly stirring the materials, and (2) adding 1.6kg of binder (polyoxymethylene resin POM: high density polyethylene: ethylene-vinyl acetate: wax: stearic acid=88:7:2:2:1), carrying out banburying for 40min, extruding and granulating to prepare the feed.
Performance test
The preparation of the modified 17-4PH high toughness stainless steel material was carried out according to the methods of examples and comparative examples, and at the time of injection molding, 51 mm. Times.34 mm. Times.12 mm specimens were prepared, and then performance test was carried out on each group of specimens according to the following method, 5 specimens were taken for each example or comparative example, the test results were averaged, and the test results were recorded in Table 2.
1. Tensile Strength referring to GB/T228.1-2010 section 1 Metal Material tensile test method at room temperature, test on WDW-300E tensile tester;
2. the elongation after break is detected by referring to GB/T228.1-2010 section 1 of tensile test of metallic materials, namely room temperature test method;
3. yield strength is detected by referring to GB/T228.1-2010 section 1 of tensile test of metallic materials, namely room temperature test method;
4. the electrochemical corrosion performance comprises the steps of cutting a wafer with the dimension phi of 16mm multiplied by 2mm from the center line of a sample, polishing a test surface to a mirror surface, installing the wafer in a laminated electrochemical cell, carrying out electrochemical impedance and electrokinetic polarization test by using a German Zahner Zennium Peo electrochemical workstation, adopting a classical three-electrode system, taking a platinum mesh as a point-to-electrode (CE), taking a Saturated Calomel Electrode (SCE) as a Reference Electrode (RE), taking the sample as a Working Electrode (WE), and carrying out test scanning at a speed of 1mV/s and a working electrode exposure area of 1cm < 2 >. The Open Circuit Potential (OCP) time is set to 3000s before testing, the EIS test initiation cross-linking positive frequency (AC) is 5mV, and the scanning frequency range is 105-10-2 Hz. The used anti-corrosion medium is sodium chloride solution with the mass fraction of 3.5wt%, and is prepared by adopting ultrapure water and molecular pure sodium chloride without deoxidization treatment. The experiment is carried out at room temperature (25 ℃), the data of the impedance spectrum are analyzed and processed by software, and each group of experiment is repeatedly tested for 3 times under the same environment, so that the reliability of the test data is ensured, and the lower the current density is, the stronger the corrosion resistance is.
TABLE 2
| Project | Tensile Strength/MPa | Yield strength/MPa | Elongation after break/% | Corrosion current Density (μA/cm 2) |
| Example 1 | 971 | 751 | 12.4 | 0.587 |
| Example 2 | 966 | 748 | 12.1 | 0.592 |
| Example 3 | 953 | 740 | 11.3 | 0.597 |
| Example 4 | 961 | 745 | 11.7 | 0.589 |
| Example 5 | 1044 | 837 | 15.4 | 0.434 |
| Example 6 | 1039 | 833 | 15.2 | 0.438 |
| Example 7 | 997 | 795 | 13.8 | 0.436 |
| Example 8 | 1011 | 804 | 14.3 | 0.521 |
| Example 9 | 1074 | 959 | 16.8 | 0.345 |
| Example 10 | 1072 | 955 | 16.5 | 0.349 |
| Example 11 | 1257 | 1074 | 18.2 | 0.215 |
| Example 12 | 1251 | 1068 | 18.0 | 0.218 |
| Comparative example 1 | 786 | 568 | 9.7 | 0.768 |
| Comparative example 2 | 812 | 638 | 10.5 | 0.704 |
| Comparative example 3 | 802 | 594 | 10.1 | 0.731 |
| Comparative example 4 | 838 | 684 | 10.7 | 0.623 |
| Comparative example 5 | 787 | 583 | 8.9 | 0.798 |
| Comparative example 6 | 821 | 675 | 10.8 | 0.654 |
| Comparative example 7 | 813 | 654 | 10.7 | 0.641 |
| Comparative example 8 | 765 | 554 | 8.5 | 0.842 |
As can be seen from the data in table 1, the titanium powder mass/(titanium powder mass+aluminum powder mass) in example 1 was 9.09%, the titanium powder mass/(titanium powder mass+aluminum powder mass) in example 2 was 28.57%, the titanium powder mass/(titanium powder mass+aluminum powder mass) in example 3 was 66.67%, and the titanium powder mass/(titanium powder mass+aluminum powder mass) in example 4 was 33.33%, as compared with the modified 17-4PH stainless steel materials prepared in example 1 and example 2, which had higher tensile strength and yield strength, and higher toughness and crack resistance.
Compared with example 1, example 5 and example 6 also use nanometer titanium nitride and yttrium oxide to pretreat graphene, thus obtaining modified 17-4PH stainless steel material with more excellent tensile strength, yield strength and elongation after break, better visible toughness, reduced corrosion current density and enhanced corrosion resistance.
Compared with the example 5, the example 7 and the example 8 are not added with nano titanium nitride and yttrium oxide respectively when the graphene is pretreated, the corrosion current density in the example 7 is not changed greatly, but the toughness is obviously reduced, and the corrosion current density in the example 8 is increased, the tensile strength and other performances are reduced to some extent, which indicates that the pretreatment of the graphene by the nano titanium nitride and the yttrium oxide not only can improve the toughness of the modified 17-4PH stainless steel material, but also can improve the corrosion resistance effect.
Examples 9 and 10 use polyvinylidene fluoride, sodium silicate, polyethylene glycol and stearic acid to prepare a binder, and it is shown in table 2 that the modified 17-4PH stainless steel materials prepared in examples 9 and 10 have improved mechanical properties such as tensile strength and yield strength, improved toughness, reduced corrosion current density, and improved corrosion resistance, as compared with example 5.
In example 11 and example 12, an auxiliary impregnating agent was further added to the binder, and it is shown in table 2 that each of the modified 17-4PH stainless steel materials prepared in example 11 and example 12 was improved in mechanical properties and enhanced in corrosion resistance, as compared with example 9.
Titanium powder, aluminum powder and graphene are not added in comparative example 1, graphene is not added in comparative example 2, aluminum powder is not added in comparative example 3, and the mechanical properties of the modified 17-4PH stainless steel materials prepared in comparative examples 1-3 are reduced and the corrosion resistance is reduced as shown in table 2.
In comparative example 4, the titanium powder and the graphene are not subjected to ball milling and low-temperature sintering, and the corrosion resistance of the prepared modified 17-4PH stainless steel material is reduced, which shows that the titanium powder and the graphene are subjected to pretreatment, so that the dispersibility of the titanium powder and the graphene can be improved, and the compactness is increased.
Comparative example 5 the properties such as tensile strength of the resulting modified 17-4PH stainless steel material were remarkably lowered as compared with example 1, without heat treatment of the resulting degreased blank.
Comparative example 6 was not subjected to the cryogenic treatment compared with example 1, whereas comparative example 7 was subjected to the cryogenic treatment instead of the high-temperature failure compared with example 1, and it is shown in table 2 that the properties such as tensile strength, yield strength, etc. of the modified 17-4PH stainless steel materials prepared in example 6 and example 7 were significantly lowered.
Comparative example 8 shows that the stainless steel blend material feed prepared in the prior art has inferior tensile strength and the like compared with example 1, and has poor toughness and corrosion resistance.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
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| CN109604584A (en) * | 2018-12-17 | 2019-04-12 | 中山市奥博精密科技有限公司 | Stainless steel mixed material feed and preparation method thereof |
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