CN114921739A - Preparation method of high-thermal-stability surface nanocrystalline titanium material - Google Patents
Preparation method of high-thermal-stability surface nanocrystalline titanium material Download PDFInfo
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- CN114921739A CN114921739A CN202210687711.5A CN202210687711A CN114921739A CN 114921739 A CN114921739 A CN 114921739A CN 202210687711 A CN202210687711 A CN 202210687711A CN 114921739 A CN114921739 A CN 114921739A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
A preparation method of a high-thermal stability surface nanocrystalline titanium material belongs to the field of nanocrystalline metal materials. The invention aims to solve the problem that the prior nanocrystalline titanium metal loses excellent performance due to recovery and grain coarsening at high temperature. The method comprises the following steps: firstly, mechanically grinding the surface; secondly, annealing in situ. The method is used for preparing the nanocrystalline titanium material with the high-thermal stability surface.
Description
Technical Field
The invention belongs to the field of nanocrystalline metal materials.
Background
Titanium and titanium alloys have high specific strength and excellent corrosion resistance, and are widely used in the engineering and medical fields, including aerospace, marine engineering, petrochemical, automotive, dental and bone implants. Compared with the traditional coarse-grain material, the bulk nanocrystalline material has higher strength, hardness and fatigue life, so the titanium and the titanium alloy with the nanocrystalline structure can obviously improve the service performance of the bulk nanocrystalline material and even broaden the application field of the bulk nanocrystalline material. However, the introduction of a high volume fraction of grain boundaries provides a strong driving force for inducing grain growth, which causes the degradation of properties with the grain coarsening behavior that occurs very easily, and appears to be less stable with smaller grains. In some low melting nanocrystalline metals, such as copper and aluminum, the temperature at which the grains grow significantly drops even to room temperature. Thus, the inherent thermal instability is an inherent short slab of nanomaterial, limiting the use of nanocrystalline Ti metal at high temperatures.
The severe plastic deformation of the surface is an effective way to obtain the nanocrystalline structure on the surface of the bulk metal and the alloy thereof. Common surface severe plastic deformation methods comprise surface mechanical grinding, high-energy ball milling, shot blasting, supersonic particle bombardment, laser shock, surface mechanical grinding, rolling surface strengthening and the like, the surface nanocrystalline layer directly prepared by the methods is usually low in thermal stability, and the nanocrystalline remarkably recovers and coarsens at a lower temperature, so that the beneficial effect of the surface nanocrystalline layer on the matrix metal is ineffective, and particularly for pure metal with severe plastic deformation, the coarsening temperature of the nanocrystalline is lower than 0.3T m (melting point of metal) which results in nanostructured pure metals often not being able to withstand thermal loads.
Disclosure of Invention
The invention aims to solve the problem that the prior nanocrystalline titanium metal loses excellent performance due to recovery and grain coarsening at high temperature, and further provides a preparation method of a high-thermal-stability surface nanocrystalline titanium material.
A method for preparing a high-thermal-stability surface nanocrystalline titanium material comprises the following steps:
firstly, surface mechanical grinding treatment:
the method comprises the following steps of (1) adhering the back of a surface to be processed of a titanium piece to be processed to the upper surface inside an upper cover of a sample storage tank, placing a zirconium oxide impact ball on the lower surface inside the sample storage tank, wherein the distance from the center of the impact ball to the surface of the titanium piece to be processed is 8-10.5 mm, placing the sample storage tank on a vertical vibration test bed, and impacting the titanium piece to be processed for 120-300 min under the conditions of room temperature, the vibration frequency of the impact ball being 20-80 Hz and the output power of the vibration bed being 3-5 kw, so as to obtain the titanium piece with an amorphous layer on the surface;
secondly, in-situ annealing:
heating the titanium piece with the surface being an amorphous layer to 600-650 ℃ at the heating rate of 5-15 ℃/min, and completely converting the amorphous layer into nano-crystals to obtain the high-heat-stability surface nano-crystal titanium material.
The beneficial effects of the invention are:
1. the impact ball is made of zirconia balls, the surface mechanical grinding technology and in-situ annealing are utilized to prepare an equiaxial nanocrystalline structure with an average grain size of less than 100nm and a low-energy interface on the surface of titanium metal, possible impurity elements are not introduced in the processing process, and the element composition of the prepared nanocrystalline layer is consistent with that of an original parent metal.
2. Has a surface nanocrystalline layer with high thermal stability. The nano-crystalline titanium metal still keeps good thermal stability at the temperature of 750 ℃ (45 percent of the melting point of the parent metal) and keeps excellent mechanical or physical properties of the nano-crystalline, so that the nano-crystalline titanium metal can be applied at high temperature.
3. The preparation method can be directly used in a working environment with the temperature higher than 350-400 ℃ without annealing treatment, and the surface layer can be spontaneously converted into a high-thermal-stability nanocrystalline structure from an amorphous state.
4. The preparation method is simple to operate, safe and efficient. The invention can complete the improvement of the surface structure of the titanium metal by using a common vertical vibration test bed, and has lower cost.
Description of the drawings:
FIG. 1 is a microstructure diagram of a titanium article with an amorphous layer on the surface, prepared in the first step of the example, (a) is a transmission electron microscopy bright field image of the microstructure of the titanium article with the amorphous layer on the surface in the depth direction, A is an amorphous layer, B is a nanocrystalline layer, and (B) is a selected area electron diffraction pattern of the dotted line frame in the diagram;
FIG. 2 is a diagram showing the energy spectrum analysis of the nanocrystalline layer element from the outermost surface to the inside of the amorphous layer of a titanium article having an amorphous layer on the surface thereof prepared in one step one of the embodiment, wherein 1 is Ti element and 2 is impurity element;
FIG. 3 is a transmission electron microscopy bright field image of the microstructure of the surface layer heated to 354 ℃ during one step two in situ annealing according to an example;
FIG. 4 is a transmission electron microscope bright field image of the microstructure of the surface layer heated to 611 ℃ during the in situ annealing process of the second step of the example;
FIG. 5 is a transmission electron microscope bright field image of the microstructure in the depth direction of the high thermal stability surface nanocrystalline titanium material prepared in the first embodiment after heating at 750 ℃ for 30 min;
FIG. 6 is a high resolution image of the vicinity of grain boundaries of nanocrystals formed by amorphous crystallization of the layer A of FIG. 5;
FIG. 7 is a graph showing the distribution of grain sizes, (a) shows the distribution of grain sizes of nanocrystals below an amorphous layer in a titanium article having an amorphous layer on the surface prepared in the first step of the example, (b) shows the distribution of grain sizes of nanocrystals below an original amorphous layer in a highly thermally stable surface-nanocrystalline titanium material prepared in the first step of the example after being heated at 750 ℃ for 30 min;
fig. 8 is a microstructure diagram of a titanium article with a surface of a nanocrystal prepared in a first comparative experiment, (a) is a transmission electron microscope bright field image of a microstructure in a depth direction of the titanium article with a surface of a nanocrystal, and (b) is a selected area electron diffraction pattern of a dashed line frame position in the diagram.
Detailed Description
The first embodiment is as follows: the embodiment provides a preparation method of a high-thermal-stability surface nanocrystalline titanium material, which comprises the following steps:
firstly, surface mechanical grinding treatment:
the method comprises the following steps of (1) adhering the back of a surface to be processed of a titanium piece to be processed to the upper surface of the inner part of an upper cover of a sample storage tank, placing a zirconium oxide impact ball on the lower surface of the inner part of the sample storage tank, enabling the distance from the center of the impact ball to the surface of the titanium piece to be processed to be 8-10.5 mm, placing the sample storage tank on a vertical vibration test bed, and impacting the titanium piece to be processed for 120-300 min under the conditions that the room temperature, the vibration frequency of the impact ball are 20-80 Hz and the output power of the vibration bed is 3-5 kw, so as to obtain the titanium piece with an amorphous layer on the surface;
secondly, in-situ annealing:
heating the titanium piece with the surface being an amorphous layer to 600-650 ℃ at the heating rate of 5-15 ℃/min, and completely converting the amorphous layer into nano-crystals to obtain the high-heat-stability surface nano-crystal titanium material.
The beneficial effects of the embodiment are as follows:
1. the impact ball is made of zirconia balls, the surface mechanical grinding technology and in-situ annealing are utilized to prepare an equiaxial nanocrystalline structure with an average grain size of less than 100nm and a low-energy interface on the surface of titanium metal, possible impurity elements are not introduced in the processing process, and the element composition of the prepared nanocrystalline layer is consistent with that of an original parent metal.
2. Has a surface nanocrystalline layer with high thermal stability. The nano-crystalline titanium metal still keeps good thermal stability at the temperature of 750 ℃ (45 percent of the melting point of the parent metal) and keeps excellent mechanical or physical properties of the nano-crystalline, so that the nano-crystalline titanium metal can be applied at high temperature.
3. The preparation method of the embodiment can be directly used in a working environment with the temperature higher than 350-400 ℃ without annealing treatment, and the surface layer can be spontaneously converted from an amorphous state into a high-thermal-stability nanocrystalline structure.
4. The preparation method of the embodiment is simple to operate, safe and efficient. The embodiment can complete the improvement of the surface structure of the titanium metal by using a common vertical vibration test bed, and has lower cost.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the diameter of the zirconia impact ball in the step one is 3 mm-8 mm. The rest is the same as the first embodiment.
The third concrete implementation mode: this embodiment is different from the first or second embodiment in that: the adding amount of the zirconia impact balls in the step one is 100-450. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: and in the first step, the inner lower surface of the sample storage tank is fully paved with the zirconium oxide impact balls. The others are the same as in the first to third embodiments.
The fifth concrete implementation mode is as follows: the difference between this embodiment and one of the first to fourth embodiments is: the thickness of the amorphous layer in the first step is 0.2-0.3 μm, and a nanocrystalline layer is arranged below the amorphous layer. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the titanium piece to be processed in the step one is made of titanium or titanium alloy. The rest is the same as the first to fifth embodiments.
The seventh concrete implementation mode: the difference between this embodiment and one of the first to sixth embodiments is: and step two, the nanocrystalline in the nanocrystalline titanium material with the high-thermal-stability surface is of an equiaxial structure with a low-energy interface, and the grain size is smaller than 100 nm. The others are the same as the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: in the first step, the distance from the center of the impact ball to the surface of the titanium piece to be processed is 9.5-10.5 mm. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: in the first step, the titanium piece to be processed is impacted for 240-300 min under the conditions of room temperature, the vibration frequency of the impacting ball is 50-80 Hz, and the output power of the vibration table is 3-5 kw. The other points are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is that: in the second step, the titanium piece with the amorphous layer on the surface is heated to 600-650 ℃ at the heating rate of 10-15 ℃/min. The other points are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a method for preparing a high-thermal-stability surface nanocrystalline titanium material comprises the following steps:
firstly, surface mechanical grinding treatment:
the method comprises the following steps of (1) adhering the back of a surface to be processed of a titanium piece to be processed to the upper surface of the inner part of an upper cover of a sample storage tank, placing a zirconium oxide impact ball on the lower surface of the inner part of a lower cover of the sample storage tank, enabling the distance from the center of the impact ball to the surface of the titanium piece to be processed to be 9.5mm, placing the sample storage tank on a vertical vibration test bed, and impacting the titanium piece to be processed for 240min under the conditions of room temperature, the vibration frequency of the impact ball being 50Hz and the output power of the vibration bed being 3kw to obtain the titanium piece with an amorphous layer on the surface;
secondly, in-situ annealing:
heating the titanium piece with the surface being an amorphous layer to 611 ℃ at the heating rate of 10 ℃/min, and completely converting the amorphous layer into the nanocrystalline to obtain the high-heat-stability surface nanocrystalline titanium material.
The diameter of the zirconia impact ball in the step one is 5 mm.
The adding amount of the zirconia impact balls in the step one is 250, and the zirconia impact balls are paved on the lower surface of the inner part of the sample storage tank.
The titanium piece to be processed in the step one is made of TA2 commercial titanium material, and the thickness is 3 mm.
The vertical vibration test bed in the step one is a common commercial vertical vibration bed.
In order to homogenize the structure and eliminate the adverse effect caused by mechanical processing, the titanium piece to be processed in the step one is heated for 2 hours at the temperature of 700 ℃, and the average grain size of the titanium piece to be processed is 50 microns.
FIG. 1 is a microstructure diagram of a titanium article with an amorphous layer on the surface, prepared in a first step of an embodiment, (a) is a transmission electron microscope bright field image of the microstructure in the depth direction of the titanium article with the amorphous layer on the surface, A is an amorphous layer, B is a nanocrystalline layer, and (B) is an electron diffraction pattern of a selected area at the position of a dashed line frame in the diagram. As shown in FIG. b, the surface layer A was an amorphous layer, and as shown in FIG. a, an amorphous structure layer with a thickness of 0.28 μm was obtained on the surface layer of TA2 commercial titanium material after the surface mechanical polishing process, and a nanocrystalline layer was formed below the amorphous layer.
FIG. 2 is a diagram showing the energy spectrum analysis of the nanocrystalline layer element from the outermost surface to the inside of the amorphous layer of a titanium article having an amorphous layer on the surface thereof prepared in one step one of the embodiment, wherein 1 is Ti element and 2 is impurity element; as can be seen, the only elements that remain uniformly distributed are Ti, and impurity elements such as C, O and Zr are almost undetectable, indicating that the machining process does not introduce impurity elements that may be present.
In the second step of the embodiment, the titanium piece with the amorphous layer on the surface is placed under a transmission electron microscope for in-situ annealing, and the change of the amorphous structure on the surface in the heating and temperature rising process is recorded by video.
FIG. 3 is a transmission electron microscopy bright field image of the microstructure of the surface layer heated to 354 ℃ during one step two in situ annealing of the example. As can be seen, the surface amorphous structure starts to undergo nano-crystallization transformation at 354 ℃.
FIG. 4 is a transmission electron microscopy bright field image of the microstructure of the surface layer heated to 611 ℃ during the in situ annealing process of the second step of the example. As can be seen, the surface amorphous structure substantially completes the nano crystallization transformation at 611 ℃, and is an equiaxed structure with the crystal grains smaller than 100 nm.
And (3) heating the high-thermal-stability surface nanocrystalline titanium material prepared in the first embodiment for 30min at the temperature of 750 ℃, and verifying the thermal stability of the nanocrystalline. FIG. 5 is a transmission electron microscope bright field image of the microstructure in the depth direction of the high thermal stability surface nanocrystalline titanium material prepared in the first embodiment after heating at 750 ℃ for 30 min. As can be seen from the figure, the surface layer nanocrystals maintained a stable nanocrystal structure at a high temperature of 750 ℃, and the crystal grain size was substantially unchanged from that of fig. 4.
FIG. 6 is a high resolution image of the A layer of FIG. 5 formed by amorphization near the grain boundaries of the nanocrystals formed; as can be seen from the figure, the grain boundaries are relaxed, and the grain boundaries have low energy and are in a low energy state.
FIG. 7 is a graph showing the distribution of grain sizes, (a) shows the distribution of grain sizes of nanocrystals below an amorphous layer in a titanium article having an amorphous layer on the surface prepared in the first step of the example, (b) shows the distribution of grain sizes of nanocrystals below an original amorphous layer in a highly thermally stable surface-nanocrystalline titanium material prepared in the first step of the example after being heated at 750 ℃ for 30 min; as can be seen, the original nanocrystal grains are obviously coarsened after annealing at 750 ℃ for 30 min.
Comparison experiment one: the comparative experiment differs from the first example in that: impacting the titanium piece to be processed for 120min in the first step; and (5) obtaining the titanium piece with the surface being the nanocrystalline in the first step, and eliminating annealing in the second step. The rest is the same as the first embodiment.
Fig. 8 is a microstructure diagram of a titanium article with a surface of a nanocrystal prepared in a first comparative experiment, (a) is a transmission electron microscope bright field image of a microstructure in a depth direction of the titanium article with a surface of a nanocrystal, and (b) is a selected area electron diffraction pattern of a dashed line frame position in the diagram. As can be seen from the graph (b), the surface layer is nanocrystalline, that is, only the nanocrystalline structure can be directly generated on the surface layer by using a short impact time, and the nanocrystalline structure directly obtained by the single plastic deformation method is often poor in thermal stability.
Claims (10)
1. A preparation method of a high-thermal-stability surface nanocrystalline titanium material is characterized by comprising the following steps:
firstly, surface mechanical grinding treatment:
the method comprises the following steps of (1) adhering the back of a surface to be processed of a titanium piece to be processed to the upper surface inside an upper cover of a sample storage tank, placing a zirconium oxide impact ball on the lower surface inside the sample storage tank, wherein the distance from the center of the impact ball to the surface of the titanium piece to be processed is 8-10.5 mm, placing the sample storage tank on a vertical vibration test bed, and impacting the titanium piece to be processed for 120-300 min under the conditions of room temperature, the vibration frequency of the impact ball being 20-80 Hz and the output power of the vibration bed being 3-5 kw, so as to obtain the titanium piece with an amorphous layer on the surface;
secondly, in-situ annealing:
heating the titanium piece with the surface being an amorphous layer to 600-650 ℃ at the heating rate of 5-15 ℃/min, and completely converting the amorphous layer into nano-crystals to obtain the high-heat-stability surface nano-crystal titanium material.
2. The method for preparing a high thermal stability surface nano-crystalline titanium material according to claim 1, wherein the diameter of the zirconia impact ball in step one is 3mm to 8 mm.
3. The method for preparing a surface-nanocrystalline titanium material with high thermal stability as claimed in claim 1, wherein the addition amount of the zirconia impact balls in the step one is 100 to 450.
4. The method for preparing nano-crystalline titanium material with high thermal stability surface as claimed in claim 1, wherein the first step is performed by filling the inner lower surface of the sample storage tank with the zirconium oxide impact balls.
5. The method for preparing a nanocrystalline titanium material with a high thermal stability surface according to claim 1, wherein the thickness of the amorphous layer in the step one is 0.2 μm to 0.3 μm, and a nanocrystalline layer is arranged below the amorphous layer.
6. The method according to claim 1, wherein the titanium member to be processed in the step one is made of titanium or titanium alloy.
7. The method as claimed in claim 1, wherein the nanocrystals in the nano-crystalline titanium material with high thermal stability surface in the second step have equiaxial structure with low energy interface, and the crystal size is smaller than 100 nm.
8. The method for preparing a high thermal stability surface nano-crystalline titanium material according to claim 1, wherein the distance from the center of the impacting ball to the surface of the titanium member to be processed in the first step is 9.5mm to 10.5 mm.
9. The method for preparing a high thermal stability surface nano-crystalline titanium material according to claim 1, characterized in that in the first step, the titanium piece to be processed is impacted for 240-300 min at room temperature under the conditions that the vibration frequency of the impacting ball is 50-80 Hz and the output power of the vibration table is 3-5 kw.
10. The method for preparing a high thermal stability surface nano-crystalline titanium material as claimed in claim 1, wherein in the second step, the temperature of the titanium piece with the amorphous layer on the surface is raised to 600-650 ℃ at a temperature raising rate of 10-15 ℃/min.
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| WO2005079209A2 (en) * | 2003-11-26 | 2005-09-01 | The Regents Of The University Of California | Nanocrystalline material layers using cold spray |
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