CN113720663A - Method for preparing high-strength-toughness isomeric nickel by regulating and controlling rolling annealing process - Google Patents
Method for preparing high-strength-toughness isomeric nickel by regulating and controlling rolling annealing process Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 39
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 33
- 238000005096 rolling process Methods 0.000 title claims abstract description 22
- 238000000137 annealing Methods 0.000 title claims abstract description 18
- 230000001105 regulatory effect Effects 0.000 title claims abstract description 10
- 230000001276 controlling effect Effects 0.000 title claims abstract description 9
- 238000005498 polishing Methods 0.000 claims abstract description 22
- 244000137852 Petrea volubilis Species 0.000 claims abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 9
- 210000000988 bone and bone Anatomy 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 5
- 238000005868 electrolysis reaction Methods 0.000 claims description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003792 electrolyte Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 230000001186 cumulative effect Effects 0.000 claims description 2
- 238000010998 test method Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 210000001519 tissue Anatomy 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000001953 recrystallisation Methods 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 239000002159 nanocrystal Substances 0.000 abstract description 2
- 235000013339 cereals Nutrition 0.000 description 25
- 229910000831 Steel Inorganic materials 0.000 description 7
- 239000010959 steel Substances 0.000 description 7
- 238000003825 pressing Methods 0.000 description 6
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 238000009864 tensile test Methods 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000005482 strain hardening Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001887 electron backscatter diffraction Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 235000020985 whole grains Nutrition 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/026—Specifications of the specimen
- G01N2203/0298—Manufacturing or preparing specimens
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Abstract
The invention discloses a method for preparing high-strength and high-toughness heterogeneous nickel by regulating and controlling a rolling annealing process, which comprises the following steps of repeatedly rolling a coarse-crystal pure nickel plate at room temperature, cutting a dog bone tensile sample on the rolled plate, polishing the sample by using a polishing machine, annealing the sample for 1-10min at the temperature of 510-650 ℃, and using 1 multiplied by 10 to prepare the heterogeneous nickel on a stretching machine‑3s‑1The strain rate of the sample is stretched, the sample after stretching deformation is polished by sand paper, then the polishing machine is used for polishing, and finally the sample is electrically polishedAnd (5) solving. The method can obtain the heterostructure material with excellent matching of strength and ductility, balance the defects of low strength of coarse crystals and low ductility of ultra-fine crystals and nano crystals, and obtain heterostructure tissues with different recrystallization ratios by regulating and controlling the heat treatment process, thereby obtaining the heterostructure tissues with different performances and greatly coordinating the strength and the ductility.
Description
Technical Field
The invention relates to the technical field of preparation of isomeric nickel, in particular to a method for preparing high-strength and high-toughness isomeric nickel by regulating and controlling a rolling annealing process.
Background
Pure nickel is widely used in engineering fields, but the ductility of the pure nickel is greatly lost while high strength is obtained by traditional rolling to refine grains. Since ultra-fine grain (UFG) and Nanostructured (NS) metals have low strain hardening capabilities, recovery of ductility of these materials by annealing often requires sacrificing significant strength, a tradeoff between strength and ductility, and the scholars propose heterogeneous lamellar structures. The heterogeneous lamellar structure is characterized by a soft microchip layer embedded in a hard ultrafine wafer layer matrix. The non-uniform layered structure can produce an unprecedented combination of properties that are as strong as ultra-fine grained metals, while being as tough as conventional coarse grained metals. The excellent mechanical properties observed in the lamellae and graded materials are attributed to back stress strengthening and back stress work hardening caused by stacking of geometrically essential dislocations (GNDs) at the internal interfaces. Unusually high strength is obtained with the help of high back stress due to inhomogeneous yield, while high ductility is due to back stress hardening and dislocation hardening. High strength is becoming paramount in the current energy crisis and global warming challenges, and stronger materials can help make transportation vehicles lighter to improve their energy efficiency. However, good ductility is also required to prevent catastrophic failure during service. In recent years, the research of heterogeneous lamellar structures shows that an optimal layer thickness nonuniform lamellar structure can obtain the optimal mechanical property, and the process is still under search. The process of heat treatment annealing is suitable for low-cost large-scale industrial production and may be applicable to other metal systems.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for preparing high-strength and high-toughness heterogeneous nickel by regulating and controlling a rolling annealing process.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing high-strength and high-toughness isomeric nickel by regulating and controlling a rolling annealing process is characterized in that the strength of the isomeric nickel prepared by the annealing process is improved by 16-198MPa compared with a coarse crystal structure, and the ductility is improved by 4-47% compared with a rolled structure; the preparation method comprises the following steps:
s1, repeatedly rolling the coarse-crystal pure nickel plate at room temperature;
s2, cutting a dog bone tensile sample on the rolled plate;
s3, polishing the sample by a polishing machine;
s4, annealing the sample at the temperature of 510-650 ℃ for 1-10 min.
Preferably, in the step S1, the deformation of each pass of rolling is less than or equal to 5%; the cumulative rolling deformation was 90%.
Preferably, the scale distance dimension of the dog bone tensile specimen in the step S2 is 7.5 × 3 × 0.5 mm.
Preferably, the grinding in step S3 is performed by using sand paper; the sand paper is 800#, 1200#, 1500# or 2000 #.
Preferably, the polishing time in the step S3 is 10-15 min.
A test method of the isomeric nickel prepared by the method comprises the step of using the prepared isomeric nickel on an instron3382 tensile testing machine by 1 x 10-3s-1The strain rate of the sample is stretched, the sample after stretching deformation is polished by sand paper, then the polishing machine is used for polishing, and finally the sample is electrolyzed.
Preferably, the polishing time is 10-15 min.
Preferably, the electrolyte for electrolysis contains perchloric acid: anhydrous ethanol ═ 1: 3: 4.
preferably, the electrolysis time is 50s, the temperature is-20 ℃, and the current density is 2.4A/dm2。
The invention has the beneficial effects that: the method can obtain the heterostructure material with excellent matching of strength and ductility, balance the defects of low strength of coarse crystals and low ductility of ultra-fine crystals and nano crystals, and obtain heterostructure tissues with different recrystallization ratios by regulating and controlling the heat treatment process, thereby obtaining the heterostructure tissues with different performances and greatly coordinating the strength and the ductility.
Drawings
FIG. 1 is a graph of engineering stress-strain curves obtained after stretching of sample tissues in examples 1-3 of the present invention;
FIG. 2 is an electron micrograph of a sample tissue obtained in examples 1 to 3 of the present invention after electrolysis;
FIG. 3 is a statistical chart of grain size and recrystallized grains of samples obtained in examples 1-3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Repeatedly rolling the industrial pure nickel at room temperature, wherein the pressing amount is not more than 5% each time, the final pressing amount is 90%, cutting a heat-treated sample on a rolled nickel plate, placing the dog bone-shaped sample with the gauge length of 7.5mm, the width of 3mm and the thickness of 0.5mm into a muffle furnace heated to 510 ℃ for 10min, and polishing the heat-treated sample by using sand paper until the surface is smooth. The test specimens were clamped by uniaxial tensile tests (tensile on an instrin 3382 tensile tester, with two clamping segments, using a 1X 10 tensile test-3s-1Elongation at strain rate) of the steel sheet was improved by 4.05% in ductility as compared with a rolled structure (CR).
Example 2
The industrial pure nickel is repeatedly rolled at room temperature, the pressing amount is not more than 5% each time, the final pressing amount is 90%, and a heat treatment sample is cut on a rolled nickel plate, wherein the gauge length section is 7.5mm, the width section is 3mm, and the thickness section is 0.5mm, dog bone shape, placing the dog bone sample into a muffle furnace heated to 610 ℃ for 1min, and polishing the heat-treated sample with sand paper until the surface is smooth. The test specimens were clamped by uniaxial tensile tests (tensile on an instrin 3382 tensile tester, with two clamping segments, using a 1X 10 tensile test-3s-1Elongation at strain rate) of the steel sheet, the ductility of the steel sheet is improved by 18.5% compared with that of a rolled structure, and the yield strength of the steel sheet is improved by 198.37MPa compared with that of a coarse-grain structure.
Example 3
Repeatedly rolling the industrial pure nickel at room temperature, wherein the pressing amount is not more than 5% each time, the final pressing amount is 90%, cutting a heat-treated sample on a rolled nickel plate, placing the dog bone-shaped sample with the gauge length of 7.5mm, the width of 3mm and the thickness of 0.5mm into a muffle furnace heated to 650 ℃ for 1min, and polishing the heat-treated sample by using abrasive paper until the surface is smooth. The test specimens were clamped by uniaxial tensile tests (tensile on an instrin 3382 tensile tester, with two clamping segments, using a 1X 10 tensile test-3s-1Elongation at strain rate) of the steel sheet, the ductility of the steel sheet is improved by 47.9% compared with that of a rolled structure, and the yield strength of the steel sheet is improved by 16.84MPa compared with that of a coarse-grain structure.
As shown in fig. 1, the engineering stress-strain curves of the sample structures obtained in examples 1 to 3 after stretching are processed by different heat treatment parameters to obtain a heterogeneous structure with a strength higher than that of Coarse Grains (CG) and a ductility better than that of a rolled structure (CR), and the yield strength is about 330MPa, the tensile strength is about 500MPa, and the ductility is about 25% in 610-1 min, so that the strength and the ductility are greatly coordinated.
The following table is a supplement to fig. 1 and accounts for the yield strength, ultimate tensile strength, and uniform elongation of each heat treated sample, as shown in the following table:
the performance test method comprises the following steps: the samples after heat treatment and tensile deformation of example 1, example 2 and example 3 were sanded with 800#, 1200#, 1500#, respectivelyAnd # 2000, polishing the polished sample by using a polishing machine for 10-15min, electrolyzing the polished sample, wherein the electrolyte is prepared from perchloric acid: anhydrous ethanol ═ 1: 3: 4 proportion, the electrolysis time is 50s, the temperature is-20 ℃, and the current density is 2.4A/dm2The electrolyzed sample heterogeneous structure is observed by an EBSD system under an FEI Quanta FEG 250 scanning electron microscope to obtain the structure shown in figure 2, no obvious recrystallized grains are generated after treatment for 510-10 min, but recovery occurs, so that the ductility of the property is improved compared with that of a rolled structure, 610-1 min is a typical heterogeneous structure, recrystallized grains are embedded in the rolled grains, the structure has an excellent synergistic deformation mechanism, the strength and the plasticity are good, the proportion of 650-1 min recrystallization is further increased, the rolled deformed grains are gradually reduced, but the yield strength is slightly improved compared with coarse grains, but the ductility is higher than that of the coarse grains.
As shown in fig. 3, it is a statistical graph of grain size and recrystallized grain size of the sample structure, and different heat treatment processes have different ratios of recrystallized grains and different grain sizes, and the ratios of recrystallized grains in the three heat treatment processes are increased in sequence, and the grain sizes are gradually increased. The isomerous structure is regulated and controlled by a heat treatment process after rolling, the proportion of recrystallized grains and deformed grains is very important, the proportion of the recrystallized grains to the deformed grains is very high in 510-10 min, the deformed grains is very large, the whole grains are small, the yield strength is high in a mechanical property diagram, the ductility is low, the recrystallized grains are increased in 610-1 min, the grain size is slightly increased, the mechanical property is that the ductility is increased, the yield strength is slightly reduced, the strength is well matched with the ductility, the yield strength is increased to 61.21% in 650-1 min, the yield strength is increased to a limited extent, but the ductility is greatly improved and even higher than that of coarse grains, and the special coordinated deformability of the isomerous structure is benefited.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (9)
1. A method for preparing high-strength and high-toughness isomeric nickel by regulating and controlling a rolling annealing process is characterized by comprising the following steps of: compared with a coarse crystal structure, the strength of the isomeric nickel prepared by the annealing process is improved by 16-198MPa, and the ductility is improved by 4-47% compared with a rolled structure; the preparation method comprises the following steps:
s1, repeatedly rolling the coarse-crystal pure nickel plate at room temperature;
s2, cutting a dog bone tensile sample on the rolled plate;
s3, polishing the sample by a polishing machine;
s4, annealing the sample at the temperature of 510-650 ℃ for 1-10 min.
2. The method for preparing the high-strength and high-toughness isomeric nickel by the controlled rolling annealing process according to claim 1, which is characterized in that: in the step S1, the deformation of each pass of rolling is less than or equal to 5 percent; the cumulative rolling deformation was 90%.
3. The method for preparing the high-strength and high-toughness isomeric nickel by the controlled rolling annealing process according to claim 1, which is characterized in that: the gauge length of the dog bone tensile specimen in the step S2 is 7.5 × 3 × 0.5 mm.
4. The method for preparing the high-strength and high-toughness isomeric nickel by the controlled rolling annealing process according to claim 1, which is characterized in that: the polishing in the step S3 is performed by using sand paper; the sand paper is 800#, 1200#, 1500# or 2000 #.
5. The method for preparing the high-strength and high-toughness isomeric nickel by the controlled rolling annealing process according to claim 1, which is characterized in that: the polishing time in the step S3 is 10-15 min.
6. A method according to any one of claims 1 to 5The test method of the prepared isomeric nickel is characterized by comprising the following steps: the prepared isomeric nickel is used on a stretcher by 1 × 10-3s-1The strain rate of the sample is stretched, the sample after stretching deformation is polished by sand paper, then the polishing machine is used for polishing, and finally the sample is electrolyzed.
7. The method for testing nickel isomerate according to claim 6, wherein: the polishing time is 10-15 min.
8. The method for testing nickel isomerate according to claim 6, wherein: the electrolyte for electrolysis contains perchloric acid: anhydrous ethanol ═ 1: 3: 4.
9. the method for testing nickel isomerate according to claim 6, wherein: the electrolysis time is 50s, the temperature is-20 ℃, and the current density is 2.4A/dm2。
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| CN116024512A (en) * | 2022-12-13 | 2023-04-28 | 西南交通大学深圳研究院 | Preparation method of high-performance ultrafine-grain heterogeneous metastable beta titanium alloy |
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| CN116024512A (en) * | 2022-12-13 | 2023-04-28 | 西南交通大学深圳研究院 | Preparation method of high-performance ultrafine-grain heterogeneous metastable beta titanium alloy |
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