CN115463965B - Gradient micro-nano structure Ti-TiZnXLayered composite material and method for producing the same - Google Patents
Gradient micro-nano structure Ti-TiZnXLayered composite material and method for producing the same Download PDFInfo
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- CN115463965B CN115463965B CN202211040391.0A CN202211040391A CN115463965B CN 115463965 B CN115463965 B CN 115463965B CN 202211040391 A CN202211040391 A CN 202211040391A CN 115463965 B CN115463965 B CN 115463965B
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- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000011701 zinc Substances 0.000 claims abstract description 52
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 51
- 239000010936 titanium Substances 0.000 claims abstract description 49
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 47
- 238000005098 hot rolling Methods 0.000 claims abstract description 16
- 238000005096 rolling process Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000009792 diffusion process Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000005097 cold rolling Methods 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000005520 cutting process Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- YJVLWFXZVBOFRZ-UHFFFAOYSA-N titanium zinc Chemical compound [Ti].[Zn] YJVLWFXZVBOFRZ-UHFFFAOYSA-N 0.000 abstract description 6
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 13
- 239000013078 crystal Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229910001069 Ti alloy Inorganic materials 0.000 description 3
- 230000004071 biological effect Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 210000000988 bone and bone Anatomy 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- 238000005260 corrosion Methods 0.000 description 2
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- 238000005553 drilling Methods 0.000 description 2
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 2
- 239000007943 implant Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
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- 230000001105 regulatory effect Effects 0.000 description 2
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- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 206010028851 Necrosis Diseases 0.000 description 1
- 206010029350 Neurotoxicity Diseases 0.000 description 1
- 206010044221 Toxic encephalopathy Diseases 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000036528 appetite Effects 0.000 description 1
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- 238000006731 degradation reaction Methods 0.000 description 1
- 239000004053 dental implant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
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- 230000004927 fusion Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
-
- 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
- C22F1/165—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 of zinc or cadmium or alloys based thereon
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
- B21B2001/386—Plates
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention relates to the field of material processing, in particular to a gradient micro-nano structure Ti-TiZn X layered composite material and a preparation method thereof, comprising the following steps: cutting pure titanium sheets and pure zinc sheets into the same size, cleaning the surfaces, sequentially stacking at intervals, and fixing to obtain laminated sheets; subjecting the obtained laminated sheet to clad-rolling treatment: firstly hot rolling at a certain temperature, and then cold rolling to realize the preliminary combination of pure titanium and pure zinc sheets, thus obtaining a pure titanium-pure zinc combined sample; and performing diffusion heat treatment on the rolled pure titanium-pure zinc combined sample at a certain temperature to form gradient micro-nano structures of TiZn 3 and TiZn X compounds in a zinc layer area in the middle of adjacent pure titanium sheets, thus obtaining the Ti-TiZn X layered composite material with the gradient micro-nano structure. The pure titanium matrix of the composite layer prepared by the invention has strong binding force with the compound layer, a composite region of titanium zinc element is formed between the pure titanium layers, and the components and tissues in the composite region are distributed in a gradient way.
Description
Technical Field
The invention relates to the field of material processing, in particular to a gradient micro-nano structure Ti-TiZn X layered composite material and a preparation method thereof.
Background
Titanium and titanium alloys are widely used in the aerospace field because of their low density and high specific strength. In addition, due to the characteristics of light weight, low elastic modulus, excellent comprehensive mechanical properties, no toxicity, good corrosion resistance, biocompatibility and the like, titanium is widely used in the scenes of bone grafting materials, dental implants, interventional therapy stents and the like, and is also a good raw material for surgical instruments. However, the titanium material has the defects of slightly higher elastic modulus compared with human bone, poor surface activity and the like, which affect the exertion of the biocompatibility of the titanium and can not meet various requirements of clinical application, and the alloying process is an effective way for reducing the elastic modulus of the pure titanium and improving the strength of the material.
Zinc is one of the essential microelements in human body, plays an important role in promoting the growth and development of human body, synthesizing various necessary enzymes of human body, enhancing the immunity of human body, maintaining the normal appetite of human body and the like, and enjoys the reputation of 'flowers of life', 'sources of intelligence' and the like. Zinc has good biocompatibility, and has no obvious chronic inflammatory reaction, necrosis or hyperplasia reaction after being implanted into human body. Meanwhile, zinc can be spontaneously degraded and disappear in the human environment, and no hydrogen is generated while the zinc is degraded. Zinc is widely used as a human implant material, playing a significant role in human repair, thanks to its good biological and degradable properties. However, the mechanical properties of zinc are poor, and the performance requirements of the bearing parts after implantation cannot be met; meanwhile, the degradation speed of zinc in a human body is difficult to control, and when the content of Zn + in the human body exceeds a threshold value, neurotoxicity is caused; these in turn limit the free medical use of zinc.
The mechanical property, corrosion resistance and biological property of degradable metallic zinc of the organic combination titanium or titanium alloy are important and hot points of research in the field of biomedical metals at present, and are urgent demands for the application of medical metals at home and abroad, such as high strength, low elasticity and effective growth and fusion of cells. Studies have shown that zinc ions have the effect of "promoting bone formation" and "improving the stability of titanium implants" when titanium and zinc are implanted together in a carrier into an organism. However, titanium and zinc are truly composite and still a blind spot for research in the field of medical materials. Therefore, a composite structure which is uniform in phase, can exert good mechanical effect of titanium and controllable to exert biological effect of zinc as a necessary trace element of human body and can exert mutual promotion function of the titanium and the zinc is developed between titanium and zinc, and a clear composite structure preparation method is formed, so that the preparation method is a problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a preparation method of a Ti-TiZn X layered composite material with a gradient micro-nano structure, solve the problem that the existing liquid forming mode is difficult to prepare a titanium-zinc compound, so that the two materials are difficult to realize composite medical use, and provide a composite structure with gradient distribution of different metal compound layers among titanium and zinc and grain sizes at micro-nano level and a preparation method thereof.
The second purpose of the invention is to provide a gradient micro-nano structure Ti-TiZn X layered composite material, wherein nano-scale gradient layered structures of titanium-zinc compounds with different atomic ratios such as TiZn 3、TiZnX are formed in zinc layer areas of adjacent pure titanium sheets.
The scheme adopted by the invention for achieving one of the purposes is as follows: a preparation method of a gradient micro-nano structure Ti-TiZn X layered composite material comprises the following steps:
(1) Cutting pure titanium sheets and pure zinc sheets into the same size, cleaning the surfaces, sequentially stacking at intervals, and fixing to obtain laminated sheets;
(2) Subjecting the laminated sheet obtained in the step (1) to a clad-rolling treatment: firstly hot rolling at a certain temperature, and then cold rolling to realize the preliminary combination of pure titanium and pure zinc sheets, thus obtaining a pure titanium-pure zinc combined sample;
(3) And performing diffusion heat treatment on the rolled pure titanium-pure zinc combined sample at a certain temperature to form gradient micro-nano structures of TiZn 3 and TiZn X compounds in a zinc layer area in the middle of adjacent pure titanium sheets, thus obtaining the Ti-TiZn X layered composite material with the gradient micro-nano structure.
Preferably, in the step (1), the thickness of the pure titanium sheet and the pure zinc sheet is 0.3-0.5mm.
Preferably, in the step (1), the outermost side of the laminated sheet is a pure titanium sheet.
Preferably, in the step (2), the hot rolling temperature is 3503400 ℃.
Hot rolling is selected when the laminated sheet has poor surface flatness or the boundary is cracked.
Preferably, in the step (2), the obtained pure titanium-pure zinc bonded sample is reduced from the original thickness of the laminated sheet to 1/331/10 of the original thickness.
Preferably, in the step (2), the specific operation of clad-rolling is as follows: the fixed laminated sheet is placed in a thin steel plate folded into two pages, and hot rolling is carried out firstly by adopting a double rolling mill, and then cold rolling is carried out, wherein the hardness of double rollers of the double rolling mill is higher than that of the pure titanium sheet and the thin steel plate. Firstly, hot rolling, during which the fixed laminated sheet is placed in a thin steel plate folded into two pages, preheated at 350-400 ℃, clamped and taken out, and immediately passed through a double-roller slit of a rolling mill. According to the bonding degree of the sheets, hot rolling and cold rolling are alternately performed, the first hot rolling is performed, the second cold rolling is performed for a plurality of times, and when the surface flatness of the laminated sheet is poor or the boundary is cracked, the hot rolling is selected, and then the cold rolling is performed.
Preferably, the rotation speed of the double rollers is uniform at 2310r/min in the rolling process, and the directions are opposite.
Preferably, in the step (3), the diffusion heat treatment is performed by heating to 3503400 ℃ under an air atmosphere or an inert gas atmosphere, and maintaining the temperature for 236h.
Preferably, in the step (3), X in TiZn X compounds ranges from 3 to 7.
The scheme adopted by the invention for achieving the second purpose is as follows: the gradient micro-nano structure Ti-TiZn X layered composite material is prepared by adopting the preparation method.
The mechanism of the invention is as follows:
The titanium sheet and the zinc sheet are subjected to composite rolling after being laminated, so that preliminary mechanical and chemical combination is realized between the titanium sheet and the zinc sheet, meanwhile, the pure titanium and the pure zinc are refined, and the volume fraction of the grain boundary is increased sharply.
Subsequently, the laminated and clad-rolled pure titanium-pure zinc bonded sample was subjected to diffusion heat treatment. The high volume fraction grain boundaries provide favorable channels for atomic diffusion, thereby accelerating the diffusion and reaction of titanium and zinc atoms at high temperature, and finally forming a nano-scale gradient layered structure of the titanium-zinc compound with TiZn 3、TiZnX different atomic ratios in the zinc layer region of adjacent pure titanium sheets.
The invention has the following advantages and beneficial effects:
1. the Ti-TiZn X composite layer is prepared, and the pure titanium matrix and the compound layer have strong binding force and are not easy to crack; namely, a composite material which has uniform phase, excellent mechanical property and good biological property is prepared among titanium and zinc elements.
2. The invention forms a composite region of titanium and zinc elements between pure titanium layers, and the components and the tissues in the composite region are distributed in a gradient way, namely a gradient layered structure of TiZn 3、TiZnX and other compounds with different atomic ratios is formed; tiZn 3 layers are organized into equiaxed crystals, and the grain size is in the nanometer scale.
3. The structure and the thickness of the titanium-zinc compound layer in the composite region can be regulated and controlled by changing the thickness of the zinc layer, the diffusion heat treatment temperature and the diffusion heat treatment time; the concentration of zinc is controllable after the zinc is implanted into organisms by changing the thickness of the zinc layer and regulating and controlling the content of zinc, so that the zinc is safer for medical use.
4. The invention is simple and convenient to operate.
Drawings
FIG. 1 is the EDS spectrum corresponding to the composition detection of the Ti-TiZn X composite layer in example 1;
FIG. 2 is an SEM image of the Ti-TiZn X composite layer of example 1, (a) a low magnification wide field of view SEM image of a gradient micro-nano Ti-TiZn X composite layer; (b) Is an SEM image of the appearance of the boundary between pure titanium and TiZn 3; (c) A TiZn 3 region morphology SEM image; (d) SEM images of the junction of TiZn 3 and TiZn X;
FIG. 3 is a SEM image of the boundary between TiZn 3 and TiZn X of example 2;
Fig. 4 is a SEM image of the morphology of the boundary of TiZn 3 and TiZn X in comparative example 1.
Detailed Description
For a better understanding of the present invention, the following examples are further illustrative of the present invention, but the contents of the present invention are not limited to the following examples only.
Example 1:
4 annealed pure titanium sheets with the thickness of 0.5mm and 3 rolled pure zinc sheets with the thickness of 0.3mm are selected (in other embodiments, pure titanium sheets and pure zinc sheets with proper thickness and types can be selected as required, the effect of the prepared material is not affected), the annealed pure titanium sheets and the rolled pure zinc sheets are cut into the same size, are distributed in a lamination mode at intervals, and the outermost side is the titanium sheet. Drilling holes in four corners of the sheet by using a mechanical drilling tool, and riveting by using an aluminum strip to realize mechanical fixation between the sheets.
Firstly, hot rolling is carried out, during hot rolling, a fixed laminated sheet is placed in a thin steel plate folded into two pages, and the sheet is heated for 1h (5 min-2h, selected according to requirements) at 400 ℃ (the common hot rolling temperature is 350-400 ℃ and the preferential temperature is 400 ℃ in the embodiment), and immediately taken out through a double-roller slit of a rolling mill after clamping. According to the degree of sheet bonding, hot rolling and cold rolling are alternately performed, and hot rolling is performed 3 times and cold rolling is performed tens of times. The initial thickness of the sample was about 3mm and the final average thickness was 1mm.
Intercepting the part of the sample with better macroscopic combination, cleaning, placing in a furnace chamber of a box-type furnace, heating to 350 ℃ and preserving heat for 2 hours.
The EDS spectrum corresponding to the detection of the sample components in example 1 is shown in FIG. 1 after the clad-rolling and diffusion heat treatment. In the composite region of the element titanium zinc, a gradient layered structure of TiZn 3、TiZnX different intermetallic compounds was formed, and the value of X in the TiZn X layer in this example was about 5.7 on average.
The structure of the sample in example 1 after clad-rolling and diffusion heat treatment is shown in fig. 2. Wherein (a) is a low-power wide-field SEM image of a gradient micro-nano Ti/TiZn X composite layer, and a TiZn 3 region is formed between two layers of pure titanium near the pure titanium, and then a TiZn X region is formed; (b) Is an SEM image of the appearance of the boundary between pure titanium and TiZn 3; (c) The SEM image of TiZn 3 area is used for observing that the tissue is nano equiaxed crystal and has twin crystal distribution; (d) SEM images of the morphology of the boundary between TiZn 3 and TiZn X are obtained.
Example 2:
the process flow and other process parameters of this example were the same as those of example 1, except that the heating and holding temperature was 400℃in the box furnace.
Fig. 3 is a SEM image of the morphology of the boundary between TiZn 3 and TiZn X in example 2, in which the structure of the TiZn 3 region is nano-scale equiaxed crystals, and the value of X in the TiZn X layer in this example is about 7.
Comparative example 1:
the process flow and other process parameters of this example were the same as those of example 1, except that the heating and holding temperature was 450℃in the box furnace.
Fig. 4 is a SEM image of the morphology of the boundary of TiZn 3 and TiZn X in comparative example 1. The microstructure of the TiZn 3 region is seen as nanoscale equiaxed crystals, the X value in the TiZn X layer in this example is about 7, but significant voids are observed in the TiZn 7 layer, which reduces the mechanical properties of the material.
While the invention has been described with respect to the preferred embodiments, it will be understood that the invention is not limited thereto, but is capable of modification and variation without departing from the spirit of the invention, as will be apparent to those skilled in the art.
Claims (7)
1. The preparation method of the gradient micro-nano structure Ti-TiZn X layered composite material is characterized by comprising the following steps of:
(1) Cutting pure titanium sheets and pure zinc sheets into the same size, cleaning the surfaces, sequentially stacking at intervals, and fixing to obtain laminated sheets;
(2) Subjecting the laminated sheet obtained in the step (1) to a clad-rolling treatment: firstly, hot rolling is carried out at 350-400 ℃, and then cold rolling is carried out, so that the primary combination of pure titanium and pure zinc sheets is realized, and a pure titanium-pure zinc combined sample is obtained;
(3) Performing diffusion heat treatment on the rolled pure titanium-pure zinc combined sample at a certain temperature, and forming gradient micro-nano structures of TiZn 3 and TiZn X compounds in a zinc layer area in the middle of adjacent pure titanium sheets to obtain the Ti-TiZn X layered composite material with the gradient micro-nano structure;
In the step (3), the diffusion heat treatment is to heat to 350-400 ℃ in an air atmosphere or an inert gas atmosphere, and keep the temperature for 2-6 hours; the range of X in TiZn X compounds is 3-7.
2. The method for preparing the gradient micro-nano structure Ti-TiZn X layered composite material according to claim 1, wherein in the step (1), the thickness of the pure titanium sheet and the pure zinc sheet are both 0.3-0.5mm.
3. The method for preparing a Ti-TiZn X layered composite material with a gradient micro-nano structure according to claim 1, wherein in the step (1), the outermost side of the laminated sheet is a pure titanium sheet.
4. The method for preparing a Ti-TiZn X layered composite material with a gradient micro-nano structure according to claim 1, wherein in the step (2), the obtained pure titanium-pure zinc combined sample is reduced from the original thickness of the laminated sheet to 1/3-1/10 of the original thickness.
5. The method for preparing the Ti-TiZn X layered composite material with the gradient micro-nano structure according to claim 1, wherein in the step (2), the specific operation of the clad-rolling is as follows: the fixed laminated sheet is placed in a thin steel plate folded into two pages, and hot rolling is carried out firstly by adopting a double rolling mill, and then cold rolling is carried out, wherein the hardness of double rollers of the double rolling mill is higher than that of the pure titanium sheet and the thin steel plate.
6. The method for preparing the gradient micro-nano structure Ti-TiZn X layered composite material according to claim 5, wherein the rotation speed of the double rollers is consistent in the rolling process and is 2-10 r/min, and the directions are opposite.
7. A gradient micro-nano structure Ti-TiZn X layered composite material is characterized in that: prepared by the preparation method of any one of claims 1-6.
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