CN112063892B - High-thermal-stability equiaxial nanocrystalline Ti-Zr-Mn alloy and preparation method thereof - Google Patents
High-thermal-stability equiaxial nanocrystalline Ti-Zr-Mn alloy and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229910000914 Mn alloy Inorganic materials 0.000 title claims abstract description 21
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 12
- 239000010936 titanium Substances 0.000 claims abstract description 8
- 239000000956 alloy Substances 0.000 claims abstract description 7
- 238000005242 forging Methods 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 238000003723 Smelting Methods 0.000 claims description 2
- 239000002707 nanocrystalline material Substances 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- BULVZWIRKLYCBC-UHFFFAOYSA-N phorate Chemical compound CCOP(=S)(OCC)SCSCC BULVZWIRKLYCBC-UHFFFAOYSA-N 0.000 claims 1
- 239000002159 nanocrystal Substances 0.000 abstract description 8
- 230000000052 comparative effect Effects 0.000 description 28
- 239000000463 material Substances 0.000 description 17
- 238000000034 method Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 8
- 239000007769 metal material Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010274 multidirectional forging Methods 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
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- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
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Abstract
The invention relates to the field of titanium alloy materials, in particular to an equiaxial nanocrystalline Ti-Zr-Mn alloy with high thermal stability and a preparation method thereof. The titanium alloy comprises the following chemical components (in weight percent): zr: 12.0 to 18.0; mn: 0.01 to 4.8; the balance being Ti. The preparation method of the titanium alloy comprises the following steps: firstly, after preserving heat for a period of time above 870 ℃, rapidly cooling to room temperature to obtain a nano-batten precursor; then, the nano-lath precursor is subjected to temperature of 650-780 ℃ and strain rate of 0.01-2 s‑1The total strain amount is more than or equal to 70 percent, so that the nano lath precursor is converted into an equiaxed nano crystal structure. The high-thermal stability nanocrystalline Ti-Zr-Mn alloy prepared by the invention has excellent comprehensive mechanical properties, and can be widely applied to a plurality of important fields of aerospace, biomedical treatment, petrochemical industry, automobile industry, ocean engineering and the like.
Description
Technical Field
The invention relates to the field of titanium alloy materials, in particular to an equiaxial nanocrystalline Ti-Zr-Mn alloy with high thermal stability and a preparation method thereof.
Background
Titanium alloys are widely used in important fields such as aerospace, biomedical, petrochemical, automotive industry and marine engineering due to their high strength, low density, excellent corrosion resistance and good biocompatibility. With the rapid development of economic technologies in recent years, development of a novel titanium alloy material having higher performance is required. Compared with the traditional coarse-grain titanium alloy, the nanocrystalline titanium alloy has excellent comprehensive mechanical properties such as higher strength and plasticity, larger fatigue strength, high-temperature superplasticity and the like, and also has good wear resistance, excellent biocompatibility and a plurality of unique physical and chemical properties, which are very attractive in practical application, and the preparation of the nanocrystalline titanium alloy opens up a new way for optimizing the performance of the traditional titanium alloy.
At present, the preparation of bulk nanocrystalline metal materials is mainly achieved by a large plastic deformation (SPD) method. Common large plastic deformation methods comprise Equal Channel Angular Pressing (ECAP), accumulative composite rolling (ARB), Multidirectional Forging (MF), High Pressure Torsion (HPT) and the like, all of which need high-power equipment and expensive dies, and the prepared material has smaller size and cannot meet the requirement of large-scale industrial production. In addition, the structural thermal stability of nanocrystalline metal materials is another important bottleneck that restricts the application and development of nanocrystalline metal materials. When the grain size is refined to nano level, the number of the interfaces in the material is much higher than that of the traditional coarse-crystal material, the thermal stability of the structure is obviously reduced due to the increase of the interface energy, and the structure recovery and grain growth of some nano-crystal metal materials can occur even under the room temperature condition, so that the materials lose the original excellent performance.
The invention provides a nanocrystalline Ti-Zr-Mn alloy with high thermal stability, which realizes the low-cost and large-scale preparation of nanocrystalline titanium alloy and brings new foundation and opportunity for the development of titanium industry.
Disclosure of Invention
The invention aims to provide an equiaxed nanocrystalline Ti-Zr-Mn alloy with high thermal stability, and in order to achieve the aim, the technical scheme of the invention is as follows:
an equiaxed nanocrystalline Ti-Zr-Mn alloy with high thermal stability comprises the following chemical components in percentage by weight: zr: 12.0 to 18.0 (preferably 14.2 to 16.5); mn: 0.01 to 4.8 (preferably 2.1 to 3.6); the balance being Ti.
The preparation method of the equiaxial nanocrystalline Ti-Zr-Mn alloy with high thermal stability comprises the following steps: smelting for multiple times by adopting a vacuum consumable furnace to obtain a raw material ingot, polishing the ingot, cogging and forging at the temperature of above 1050 ℃, carrying out precision forging to obtain a blank, and then carrying out thermal deformation to obtain the equiaxed nanocrystalline Ti-Zr-Mn alloy.
After preserving the temperature of the blank obtained by the precision forging processing for a period of time above 870 ℃, rapidly cooling to room temperature to obtain a nano-lath precursor; and thermally deforming the obtained nano lath precursor to finally obtain the equiaxial nano-crystalline Ti-Zr-Mn alloy.
As a preferred technical scheme:
and keeping the temperature above 870 ℃ for a holding time t ═ (3.2-3.7) D min, wherein D is the effective thickness of the sample and the unit is millimeter mm.
The obtained blank is quickly cooled to room temperature after being kept at 870-1250 ℃ for a period of time.
The cooling rate of the rapid cooling is 25-300 ℃/s.
The nano-lath precursor has the strain rate of 0.01-2 s at the temperature of 650-780 DEG C-1Is thermally deformed within the range of (1), and the total strain amount is 70% or more. Preferably: the heat distortion temperature is 670-720 ℃, and the strain rate is 0.03-0.2 s-1The total strain is 90-95%.
The microstructure of the nanocrystalline material prepared by the method is an equiaxial alpha structure, and the grain size is 18-150 nm; the crystal grains are not coarsened and grown within 5 hours of aging at the temperature of 650 ℃ and below.
The invention has the beneficial effects that:
(1) different from the situation of the prior art, the titanium alloy provided by the invention can realize the preparation of the nanocrystalline titanium alloy through conventional thermal deformation without depending on high-power equipment and expensive dies.
(2) The method can greatly improve the thermal stability of the nanocrystalline titanium alloy structure.
(3) The bulk nanocrystalline metal material prepared by the method is not limited by size, and compared with the prior art, the bulk nanocrystalline metal material with larger size can be prepared, so that the requirement of large-scale industrial production is met.
(4) The method can obviously improve the comprehensive mechanical property of the titanium alloy material, and can be widely applied to a plurality of important fields of aerospace, biomedical treatment, petrochemical industry, automobile industry, ocean engineering and the like. Under the conditions of optimized alloy components (Zr content is 14.2-16.5%, Mn content is 2.1-3.6%) and thermal deformation (thermal deformation temperature is 670-720 ℃, strain rate is 0.03-0.2 s)-1The total strain is 90-95%), the tensile strength of the prepared nanocrystalline Ti-Zr-Mn alloy is up to 1220-1360 MPa, the elongation is 11-16%, and the Vickers hardness is 380-440.
Drawings
FIG. 1 TEM photograph of a nanostring precursor.
FIG. 2 is a TEM photograph of an equiaxed nanocrystalline structure formed by thermally deforming a nanostring precursor.
Detailed Description
In order to make the purpose, technical solution and effect of the present application clearer and clearer, the present application is further described in detail below with reference to the accompanying drawings and examples.
The invention provides a novel titanium alloy, which comprises the following chemical components: zr: 12.0 to 18.0; mn: 0.01 to 4.8; the balance being Ti. The content of impurity elements in the alloy meets the corresponding requirements in the national standard of titanium alloy.
Please refer to fig. 1-2. Fig. 1 is a nano-lath precursor formed by rapidly cooling the material of example 7 of the present invention, and it can be seen from the TEM tissue photograph that the widths of all laths are less than 100 nm. FIG. 2 shows an equiaxed nanocrystalline structure formed by thermally deforming the nano-slab precursor of example 7 of the present invention, and it can be seen from the TEM photograph that the grain size is between 18 nm and 100 nm.
The present application will now be illustrated and explained by means of several groups of specific examples and comparative examples, which should not be taken to limit the scope of the present application.
Example (b): examples 1 to 9 are Ti — Zr — Mn alloys that were smelted according to the chemical composition range provided by the present invention, in which the contents of Zr and Mn elements were gradually increased, and the corresponding preparation processes were also appropriately adjusted within the technical parameter ranges specified by the present invention. The size of the prepared bulk nanocrystalline metal material is 120X 30 mm.
Comparative example: the chemical composition of Zr and Mn in comparative example 1 is below the lower limit of the chemical composition range provided by the present invention, and the chemical composition of Zr and Mn in comparative example 9 is above the upper limit of the chemical composition range provided by the present invention, and the effect of the Zr and Mn content on the nanocrystal preparation is illustrated by comparing with example 1 and example 9, respectively. Comparative example 2, in which the amount of strain is below the lower limit of the amount of strain provided by the present invention, illustrates the effect of the amount of strain on nanocrystal production by comparison with example 2. The effect of strain rate on nanocrystal production is illustrated by comparing the strain rate of comparative example 3, which is higher than the upper limit of the strain rate provided by the present invention, and the strain rate of comparative example 4, which is lower than the lower limit of the strain rate provided by the present invention, with example 3 and example 4, respectively. Comparative example 5 slowly cooled to room temperature after heat treatment, and the effect of cooling rate after heat treatment on nanocrystal preparation is illustrated by comparison with example 5. Comparative example 6, in which the heat treatment temperature is lower than the lower limit of the heat treatment temperature provided by the present invention, illustrates the effect of the heat treatment temperature on the nanocrystal preparation by comparison with example 6. Comparative example 7, in which the heat distortion temperature is higher than the upper limit of the heat distortion temperature provided by the present invention and comparative example 8, in which the heat distortion temperature is lower than the lower limit of the heat distortion temperature provided by the present invention, illustrates the influence of the heat distortion temperature on the preparation of nanocrystals by comparing with example 7 and example 8, respectively. The comparative example 10 is nanocrystalline pure titanium prepared by an ECAP process, and the structural evolution of the comparative examples 1-9 and the comparative example 10 in the high-temperature aging process shows that the nanocrystalline titanium alloy provided by the invention has good structural thermal stability.
TABLE 1 chemical composition, pretreatment Process and Hot Rolling Process of example and comparative materials
1. Hardness test
The hardness of the materials of the examples and comparative examples were tested. The Vickers hardness of the annealed material samples was measured using an HTV-1000 type durometer. Before testing, the sample surface was polished. The sample was a thin sheet with dimensions of 10mm diameter and 2mm thickness. The test loading force is 9.8N, the pressurizing duration is 15s, and the hardness value is automatically calculated by measuring the diagonal length of the indentation through computer hardness analysis software. The final hardness values were averaged over 15 points and three replicates were selected for each set of samples.
2. Tensile Property test
The room temperature tensile mechanical properties of the comparative and example materials were tested using an Instron model 8872 tensile tester at a tensile rate of 0.5 mm/min. Before testing, a lathe is adopted to process the material into standard tensile samples with the thread diameter of 10mm, the gauge length of 5mm and the gauge length of 30mm, three parallel samples are taken from each group of heat treatment samples, and the mechanical properties obtained by the experiment comprise tensile strength, yield strength and elongation, and the results are shown in table 2.
3. Grain size statistics
The material was characterized using a Transmission Electron Microscope (TEM) and the grain size of the material was counted using a line cut. The preparation method of the TEM sample comprises the following steps: firstly, manually grinding and thinning a sample to be less than 40 mu m by using No. 2000 abrasive paper, and preparing the sample by using a punching machine
A sheet of (a); and then, thinning the sample by adopting a Tenupol-5 chemical double-spraying thinning instrument, wherein the double-spraying liquid is 6% perchloric acid, 30% butanol and 64% methanol, and the double-spraying thinning temperature is-25 ℃. And (3) observing the double-sprayed thinned sample by using a TECNAI20 transmission electron microscope, wherein the working voltage during TEM observation is 200kV, and the alpha and beta angle rotation ranges are +/-30 degrees by using a double-inclined magnetic sample table. Drawing parallel fixed-length straight lines on the TEM picture, and calculating the grain size of the material according to the number of the fixed-length straight lines passing through the grains.
TABLE 2 texture characteristics and mechanical Properties of the materials of the examples and comparative examples
TABLE 3 texture Change of the example and comparative example materials after incubation for 5h at different temperatures
As can be seen from the results in Table 2, examples 1-9 are equiaxed nanocrystalline structures, which make them have higher strength, good plasticity and greater hardness. Within the Zr and Mn content range specified in the invention, as the Zr and Mn content increases, the grain size of the material gradually decreases, the strength and hardness of the material are improved, and the elongation and the reduction of area are gradually reduced.
In comparative example 1, the contents of Zr and Mn are low, and a nano lath precursor cannot be obtained after rapid cooling, so that an equiaxed nanocrystalline structure cannot be obtained by performing thermal deformation with the precursor as an original structure. The higher Zr and Mn contents in comparative example 9 resulted in obtaining a coarse all- β structure after rapid cooling and failed to prepare an equiaxed nanocrystalline structure after hot deformation.
The strain of comparative example 2 was small, and the structure of the nanoslabs remained after the deformation, and the preparation of the equiaxed nanocrystalline structure could not be achieved.
The strain rate of comparative example 3 was large and preparation of an equiaxed nanocrystalline structure could not be achieved. The strain rate of comparative example 4 is small, and the grains are coarsened during the thermal deformation, so that the preparation of the equiaxed nanocrystalline structure is not achieved.
Comparative example 5 was slowly cooled to room temperature after heat treatment, and comparative example 6 had a lower heat treatment temperature, and their precursors were coarse lamellar structures, not the nano lath structure provided by the present invention, and thus the preparation of equiaxed nanocrystalline structures could not be achieved.
The temperature ranges for hot deformation of the nanoslab precursors of comparative examples 7 and 8 were outside the ranges provided by the present invention and preparation of equiaxed nanocrystalline structures could not be achieved.
From the results in table 3, it can be seen that examples 1 to 9 have good thermal stability of the structure during aging at 650 ℃ and below, and the grain size does not change significantly after aging. While comparative example 10 exhibited significant coarsening and growth of grains.
The above description is only for the purpose of illustrating embodiments of the present application and is not intended to limit the scope of the present application, and all modifications of equivalent structures and equivalent processes, which are made by the contents of the specification and the drawings of the present application or are directly or indirectly applied to other related technical fields, are also included in the scope of the present application.
Claims (7)
1. An equiaxed nanocrystalline Ti-Zr-Mn alloy with high thermal stability, which is characterized in that: the titanium alloy comprises the following chemical components in percentage by weight: zr: 12.0 to 18.0; mn: 0.01 to 4.8; the balance being Ti;
the preparation method of the alloy comprises the following steps:
smelting for multiple times by using a vacuum consumable furnace to obtain a raw material ingot, polishing the ingot, cogging and forging at a temperature of more than 1050 ℃, performing finish forging to obtain a blank, preserving the temperature of the blank obtained by the finish forging for a period of time at a temperature of more than 870 ℃, and rapidly cooling to room temperature to obtain a nano-lath precursor; thermally deforming the obtained nano lath precursor to finally obtain equiaxial nano-crystalline Ti-Zr-Mn alloy;
the cooling rate of the rapid cooling is between 25 and 300 ℃ per second.
2. A high thermal stability equiaxed nanocrystalline Ti-Zr-Mn alloy according to claim 1, characterized in that: the Zr content ranges from 14.2 to 16.5 in percentage by weight; the Mn content ranges from 2.1 to 3.6; the balance being Ti.
3. A high thermal stability equiaxed nanocrystalline Ti-Zr-Mn alloy according to claim 1, characterized in that: keeping the temperature above 870 ℃ for a period of timet= (3.2-3.7)Dmin, wherein,Dis the effective thickness of the sample in mm.
4. A high thermal stability equiaxed nanocrystalline Ti-Zr-Mn alloy according to claim 1, characterized in that: and (3) keeping the temperature of the obtained blank at 870-1250 ℃ for a period of time, and rapidly cooling to room temperature.
5. A high thermal stability equiaxed nanocrystalline Ti-Zr-Mn alloy according to claim 1, characterized in that: the nano-lath precursor has a temperature of 650-780 ℃ and a strain rate of 0.01-2 s-1Is thermally deformed within the range of (1), and the total strain amount is 70% or more.
6. A high thermal stability equiaxed nanocrystalline Ti-Zr-Mn alloy according to claim 5, characterized in that: the heat distortion temperature is 670-720 ℃, and the strain rate is 0.03-0.2 s-1The total strain is 90-95%.
7. A high thermal stability equiaxed nanocrystalline Ti-Zr-Mn alloy according to claim 5 or 6, characterized in that: the microstructure of the prepared nanocrystalline material is an equiaxial alpha structure, and the grain size is 18-150 nm; the crystal grains are not coarsened and grown within 5 hours of aging at the temperature of 650 ℃ or below.
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| JPH06128669A (en) * | 1992-09-07 | 1994-05-10 | Kobe Steel Ltd | Anode member made of titanium alloy |
| JP2004130541A (en) * | 2002-10-08 | 2004-04-30 | Tdk Corp | Phase change material target and manufacturing method therefor |
| CN109112356A (en) * | 2018-08-03 | 2019-01-01 | 燕山大学 | A kind of high-strength corrosion-resistant erosion titanium alloy and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH06128669A (en) * | 1992-09-07 | 1994-05-10 | Kobe Steel Ltd | Anode member made of titanium alloy |
| JP2004130541A (en) * | 2002-10-08 | 2004-04-30 | Tdk Corp | Phase change material target and manufacturing method therefor |
| CN109112356A (en) * | 2018-08-03 | 2019-01-01 | 燕山大学 | A kind of high-strength corrosion-resistant erosion titanium alloy and preparation method thereof |
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