CN114737080A - Method for preparing porous titanium alloy nano material by shearing forging - Google Patents
Method for preparing porous titanium alloy nano material by shearing forging Download PDFInfo
- Publication number
- CN114737080A CN114737080A CN202210532238.3A CN202210532238A CN114737080A CN 114737080 A CN114737080 A CN 114737080A CN 202210532238 A CN202210532238 A CN 202210532238A CN 114737080 A CN114737080 A CN 114737080A
- Authority
- CN
- China
- Prior art keywords
- titanium alloy
- blank
- shearing
- forging
- nano material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J1/00—Preparing metal stock or similar ancillary operations prior, during or post forging, e.g. heating or cooling
- B21J1/02—Preliminary treatment of metal stock without particular shaping, e.g. salvaging segregated zones, forging or pressing in the rough
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/26—Acidic compositions for etching refractory metals
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/32—Alkaline compositions
- C23F1/38—Alkaline compositions for etching refractory metals
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention discloses a method for preparing a porous titanium alloy nano material by shearing forging, which is characterized by mixing titanium alloy material powder or particles, obtaining superfine composite powder by mechanical ball milling, then carrying out vacuum sintering on a titanium alloy blank obtained from the composite powder, annealing, then repeatedly shearing forging the titanium alloy blank by a shearing forging machine through pushing a sliding sheet, keeping the cross section of the blank unchanged in the shearing deformation process, realizing repeated severe plastic deformation of the titanium alloy blank, and finally corroding the titanium alloy blank to obtain the porous titanium alloy nano material with high porosity. In the shearing and forging process of each pass, the blank does not need to be removed and reinstalled, so that the process time is saved, and the production efficiency is improved; the obtained material has reliable strength, hardness, good corrosion resistance, mechanical property similar to human skeleton and human affinity.
Description
Technical Field
The invention relates to a novel method and equipment for preparing a massive porous titanium alloy nano material, in particular to a method for preparing a porous titanium alloy nano material by shearing forging.
Background
Titanium, a transition metal, is characterized by light weight, high strength, and metallic luster. Titanium has stable chemical properties, good high temperature resistance, low temperature resistance, high strength and low density. Titanium has a high specific strength, is a high strength but low quality metal, and has a relatively good ductility (especially in an oxygen-free environment). Titanium has a relatively high melting point (above 1,649 degrees celsius) and is a preferred refractory material. The excellent performance of the titanium alloy makes the titanium alloy play a great role in the aerospace field, and meanwhile, the titanium has 'parent-biological properties' and is widely applied to the medical field. With the rapid development of composite materials, the requirements for the performance of titanium alloy materials are gradually increased, and high strength and good plasticity become the mainstream of current research.
At present, severe plastic deformation methods such as Equal Channel Angular Pressing (ECAP), cumulative rolling bonding (ARB) and High Pressure Torsion (HPT) are widely spotlighted because they can apply very high strain amount to the material to obtain ultra-fine grained material. However, the above method has a large disadvantage in terms of material utilization and production efficiency. Meanwhile, the metals and alloys used in medical science at present mainly comprise medical stainless steel, medical cobalt-based alloys, medical magnesium alloys and other metals and alloys, and the traditional medical metals and alloys have the defects of easy corrosion, poor mechanical properties, poor wear resistance, incapability of effectively inducing bone tissue growth and the like. Therefore, there is a need in the medical field for superior performance metal and alloy materials to replace traditional medical metals and alloys.
The rapid development of the metal porous material is in the late 80 s of the 20 th century, the metal porous material has excellent physical properties and good mechanical properties, and is a novel engineering material. Patent numbers: 201310518895.3A process for preparing porous biomedical titanium alloy by powder metallurgy includes vacuum degreasing, and repeated heating for sintering. Patent numbers: 201710519226.6A method for preparing porous titanium alloy with repeated gradient for promoting bone fusion comprises preparing matrix material by 3D printing, and constructing Hydroxyapatite (HA) coating with bioactivity on the surface of porous titanium alloy with repeated gradient by plasma spraying technique to promote migration and growth of osteocyte, with high cost and low production efficiency. Patent numbers: 201811361192.3 discloses a method for preparing a medical porous titanium or titanium alloy material with a tantalum coating coated on the surface, which adopts a 3D printing method to prepare the material, and the process needs high-temperature sintering and is long in technological process. Patent numbers: 201911134266.4 discloses a method for preparing antibacterial porous titanium alloy, the preparation process needs vacuum sintering, the porous titanium alloy obtained has poor mechanical properties.
Disclosure of Invention
The purpose of the invention is: aiming at a series of problems of material waste, low productivity, improvement of the performance requirement of the titanium alloy material in the medical field and increase of the demand in the existing severe plastic deformation method, the porous titanium alloy nano material with high porosity, excellent mechanical property, good corrosion resistance, good human body affinity and good capability of inducing the growth of bone tissues is provided.
The invention is realized by the following technical scheme:
the method comprises the steps of mixing titanium alloy material powder or particles, obtaining superfine composite powder through mechanical ball milling, then carrying out vacuum sintering on a titanium alloy blank obtained from the composite powder, after annealing, repeatedly shearing and forging the titanium alloy blank through pushing a sliding sheet by a shearing and forging machine, keeping the cross section of the blank unchanged in the shearing and deformation process, realizing repeated severe plastic deformation of the titanium alloy blank, and finally corroding the titanium alloy blank to obtain the porous titanium alloy nano material with high porosity.
The invention provides a method for preparing a porous titanium alloy nano material by shearing forging, which comprises the following steps:
(1) preparing materials and preparing a blank: the titanium alloy blank comprises the following chemical components in percentage by mass: the titanium alloy blank comprises the following components in percentage by mass: al: 19.5% -21.75%, V: 1.5% -2.5%, Ag: 0.5% -1.25%, Si: 21.5% -23.5%, Zr: 2.5 to 3.5 percent, and the balance of Ti. Firstly, mixing the powder or the particles of the materials with the purity of 99.99 percent according to a certain mass fraction, and carrying out mechanical ball milling for 9-14 hours after mixing to obtain the superfine composite powder. Mixing the composite powder and isopropanol in a weight ratio of 1.5%, stirring for 5 minutes, putting into an extrusion device for extrusion, and obtaining a rectangular strip-shaped titanium alloy blank with a cross section of 8 multiplied by 50mm in geometric dimension after extrusion forming3The extruded blank is put into a vacuum sintering furnace, the temperature is kept for 90 minutes at the temperature of 1000 ℃, then the titanium alloy blank is softened and annealed, the annealing temperature is 600 ℃, the blank is cooled in the air after being kept for 4 hours, and then the blank is washed for 2 to 3 times in warm water at the temperature of 50 ℃. Finally, the titanium alloy blank with the rectangular cross section which is easy to form is obtained.
(2) Obtaining the titanium alloy nano material: putting the processed titanium alloy blank between two groups of sliding sheets; the hydraulic transmission block is driven by a hydraulic machine, the hydraulic transmission block drives the parallel rotation side lever, so that the slide sheet is pushed to perform shearing forging on the titanium alloy blank, shearing is stopped when the parallel rotation side lever pushes the inclined angle of the slide sheet to be 45 degrees (the rotation angular speed is 4 rad/s), and the first plastic deformation of the titanium alloy blank can be realized; reversely pushing the parallel rotating side rods through the hydraulic rotating piece, further pushing the other group of sliding pieces to enable the titanium alloy blank to complete reverse deformation, and stopping shearing (the rotating angular speed is 4 rad/s) when the parallel rotating side rods push the inclined angle of the sliding pieces to be 45 degrees, so that the secondary plastic deformation of the titanium alloy blank can be realized; finally, the slide sheet is pushed to change the parallelogram cross section into the original rectangular cross section (the rotating angular speed is 4 rad/s), and the third plastic deformation of the titanium alloy blank can be realized. In the process of shearing deformation, the cross section of the blank is kept unchanged, namely the bottom and the height of the original rectangular cross section are equal to those of the four parallel sides in each deformation stage, so that severe plastic deformation of the titanium alloy material can be realized, and the titanium alloy nano material is obtained.
(3) Material forming a porous structure with high porosity: soaking the obtained titanium alloy nano material in 6L potassium hydroxide (KOH) water solution at 60 ℃ for 12 hours to remove Si, and then soaking the titanium alloy nano material after Si removal in 6L nitric acid (HNO) at room temperature3) Taking out the titanium alloy for 6 hours, washing the titanium alloy, cleaning the titanium alloy by using an ultrasonic technology, repeatedly cleaning the titanium alloy for 2 to 3 times, and drying the titanium alloy in the air for 24 hours to finally obtain the porous titanium alloy nano material with the high porosity of more than 50 percent.
Reaction for removal of Si: si（s）+ 2KOH（aq）+ H2O（aq） = K2SiO3(aq) + 2H2（g）
Reaction for removing Al: 2Al（s）+ 6HCl（aq）= 2AlCl3（aq）+ 3H2（g）
Silicon in the alloy component can form a porous structure with high porosity after being corroded by alkali solution; the aluminum can reduce the overall hardness of the titanium alloy to a certain extent, the difficulty of subsequent shearing forging of the titanium alloy is reduced, and pores can be formed in the titanium alloy nano material after hydrochloric acid corrosion; titanium and vanadium can be well combined, so that the material has reliable strength, hardness, wear resistance and good comprehensive performance; the existence of zirconium can further improve the corrosion resistance of the material, so that the porous titanium alloy nano material has mechanical properties similar to human bones; the presence of pores provides ample space for the growth of bone tissue; silver element can play a role in resisting bacteria and killing viruses; the obtained titanium alloy nano material is respectively put into an alkali solution and an acid solution to be corroded to form the porous titanium alloy nano material with high porosity, the obtained material has reliable strength, hardness, corrosion resistance and human body affinity, and the mechanical property of the material is close to that of human bones.
The invention provides a method for preparing a porous titanium alloy nano material by shearing forging, and compared with the existing medical alloy material, the obtained porous titanium alloy nano material has the advantages that:
1. firstly, the innovation on the formula is as follows: titanium, silicon, aluminum, vanadium, zirconium and silver are mixed according to a certain percentage, and the titanium has excellent mechanical property and good human body affinity and can provide enough mechanical strength; silicon is used as a space material and does not cause cytotoxicity, and can be corroded by alkali solution to form a material with a porous structure with high porosity at the later stage; the aluminum is soft, the integral hardness of the titanium alloy can be reduced after the aluminum is added into the titanium alloy, so that the difficulty of shearing and forging the titanium alloy is reduced, the activity of the aluminum is good, and pores can be formed by the reaction of the aluminum and an acid solution; the vanadium can be well combined with the titanium, so that the material has reliable strength, hardness, wear resistance and good comprehensive performance; the corrosion resistance of the material can be further improved due to the existence of zirconium; silver element has good antibacterial and antivirus effects. The porous titanium alloy nano material prepared by the formula has high strength, hardness, corrosion resistance and human body affinity, the mechanical property of the material is close to that of human skeleton, and the porous structure provides possibility for bone tissue growth.
2. Secondly, the preparation process is innovative: the material is subjected to severe plastic deformation by adopting a shearing and forging method, and in the shearing process, the shearing deformation is expanded to the whole section of the blank by using a plurality of sliding sheets, so that the deformation is more uniform, the mechanical property of the block nano titanium alloy is further improved, and high strength and good toughness are achieved on the premise of ensuring high density. The cross section size of the titanium alloy blank is not changed in the deformation process, and the geometric shape of the blank is not changed, so that the nano equiaxial of the titanium alloy material grains can be realized. The method is not only beneficial to ensuring the geometric dimension and the shape precision of the titanium alloy nano material, but also does not need to remove and reinstall the blank in the shearing process of each pass, thereby saving the process time and greatly improving the production efficiency. Compared with methods such as equal channel angular extrusion, accumulative rolling combination, high-pressure torsion and the like, the method reduces material waste caused by friction, improves the material utilization rate and reduces the production cost.
3. Innovation of forming material morphological structure: and putting the titanium alloy nano material formed by shearing and forging into an alkali solution to corrode silicon in the material, and putting the titanium alloy nano material into an acid solution to corrode aluminum to form a porous structure nano material with high porosity, so as to obtain the titanium alloy nano material with the mechanical property similar to that of human skeleton.
4. The preparation method of the invention is simple in process, and the shear forging machine mainly comprises a hydraulic transmission block, a parallel rotation side lever, a slip sheet, an upper supporting piece and a lower supporting piece. The distance between the two groups of sliding sheets is adjustable, and the height is adjustable. The method comprises the following steps of putting a titanium alloy blank with a rectangular cross section between two groups of sliding sheets, driving a hydraulic transmission block through a hydraulic press so as to drive parallel rotation side rods and further drive the sliding sheets to perform shear forging on the blank, so that severe plastic deformation of the titanium alloy blank is realized, the blank does not need to be removed or reinserted in the process of each pass, and repeated shear forging of the titanium alloy blank can be realized; the method introduces high strain value, so that the titanium alloy blank realizes severe plastic deformation, refines crystal grains, obtains the titanium alloy nano material, and simultaneously reduces the friction effect in the extrusion process, thereby improving the material utilization rate; in the process, the blank does not need to be removed and reinstalled among all the passes, so that the process time is shortened, and the process productivity is obviously improved; meanwhile, in the shearing process, the shearing deformation is expanded to the whole section of the blank by using the plurality of sliding sheets, so that the deformation is more uniform, the mechanical property of the block nano titanium alloy is further improved, and the high strength and the good toughness are realized on the premise of ensuring high density. The method can be used for processing on a simple shearing forging machine, has high processing efficiency and low cost, is easy for batch production, and can be used as a substitute material for related bones in the medical field.
Description of the drawings:
the following is a detailed description of specific embodiments of the present invention with reference to the accompanying drawings and examples.
FIG. 1 is a schematic view of a shear forging tool set according to the present invention;
FIG. 2 is a schematic view of the principle process of shear forging of the present invention;
FIG. 3 is a schematic view of an embodiment of the shear forging apparatus of the present invention.
The labels in the above figures are:
FIG. 1 shows the upper support plate 1, the sliding blade 2, and the lower support plate 3 of the shear forging tool set of the present invention.
Fig. 3 is a schematic view of a shear forging machine of the present invention, showing 1, a hydraulic transmission block, 2, parallel rotation side bars, 3, a guide rail, 4, support side bars, 5, a support base, 6, an upper support, 7, a slide, and 8, a lower support.
The specific embodiment is as follows:
the titanium alloy blank comprises the following chemical components in percentage by mass: the titanium alloy blank comprises the following components in percentage by mass: al: 19.5%, V: 1.5%, Ag: 1.25%, Si: 22.5%, Zr: 2.5 percent, and the balance being Ti.
The powder or the particles of the materials with the purity of 99.99 percent are mixed according to a certain mass fraction, and are mechanically ball-milled for 12 hours after being mixed, so as to obtain the superfine composite powder. Mixing the composite powder and isopropanol in a weight ratio of 1.5%, stirring for 5 minutes, putting into an extrusion device for extrusion, and obtaining a rectangular strip-shaped titanium alloy blank with a cross section of 8 multiplied by 50mm in geometric dimension after extrusion forming3The extruded blank is put into a vacuum sintering furnace, the temperature is kept at 1000 ℃ for 90 minutes, then the titanium alloy blank is softened and annealed, the annealing temperature is 600 ℃, the blank is cooled in the air after being kept for 4 hours, and then the blank is washed in warm water at 50 ℃ for 2 to 3 times. Then washing in warm water at 50 deg.C for 2-3 times. Finally, the titanium alloy blank with the rectangular cross section which is easy to form is obtained. Putting the processed titanium alloy blank between the sliding sheets 7; the hydraulic transmission block 1 is driven by the hydraulic press, the hydraulic transmission block 1 drives the parallel rotation side rod 2, and therefore the slip sheet 7 is pushed to close the titaniumShearing and forging the gold blank, and stopping shearing (the rotating angular speed is 4 rad/s) when the inclined angle of the sliding sheet 7 is pushed to be 45 degrees by rotating the side rod 2 in parallel, so that the first plastic deformation of the titanium alloy blank can be realized; the parallel rotating side lever 2 is pushed reversely by the hydraulic rotating piece 1, and then the sliding sheet 7 is pushed to enable the titanium alloy blank to complete reverse deformation, when the parallel rotating side lever 2 pushes the inclined angle of the sliding sheet 7 to be 45 degrees, shearing is stopped (the rotating angular speed is 4 rad/s), and secondary plastic deformation of the titanium alloy blank can be realized; finally, the slide sheet 7 is pushed to change the parallelogram cross section into the original rectangular cross section (the rotation angular speed is 4 rad/s), so that the third plastic deformation of the titanium alloy blank can be realized. In the shearing forging process, the upper support piece 6 and the lower support piece 8 limit the slide sheet 7 to move up and down to play a role in fixing and supporting; the guide rail 3 limits the front and back movement of the parallel rotating side rods 2 to enable the parallel rotating side rods to move along the track direction; the supporting side rod 4 plays a role in fixing the guide rail 3; the supporting base 5 plays a role in supporting the whole device. In the process of shearing deformation, the cross section of the blank is kept unchanged, namely the bottom and the height of the original rectangular cross section are equal to those of the four parallel sides in each deformation stage, so that severe plastic deformation of the titanium alloy material can be realized, and the titanium alloy nano material can be obtained. Soaking the obtained titanium alloy nano material in 6L potassium hydroxide (KOH) water solution at 60 ℃ for 12 hours to remove Si, and then soaking the titanium alloy nano material after Si removal in 6L nitric acid (HNO) at room temperature3) And taking out the titanium alloy for 6 hours, washing the titanium alloy, cleaning the titanium alloy by using an ultrasonic technology, repeatedly cleaning the titanium alloy for 2 to 3 times, and drying the titanium alloy in the air for 24 hours to finally obtain the porous titanium alloy nano material with high porosity of 53 percent.
The required equipment of the invention is a hydraulic press.
The devices adopted by the invention have simple structure, can adopt the prior art, and the invention is not limited to the specific implementation forms listed above, and the improvement which can be obtained by the technicians in the field without creative work belongs to the protection scope of the invention.
Claims (4)
1. A method for preparing a porous titanium alloy nano material by shearing forging is characterized by comprising the following steps: mixing titanium alloy material powder or particles, obtaining superfine composite powder through mechanical ball milling, then carrying out vacuum sintering on a titanium alloy blank obtained from the composite powder, after annealing, repeatedly shearing and forging the titanium alloy blank by a shearing and forging machine through pushing a sliding sheet, wherein in the shearing and deforming process, the cross section of the blank is kept unchanged, so that repeated severe plastic deformation of the titanium alloy blank is realized, and finally, the titanium alloy blank is corroded to obtain the porous titanium alloy nano material with high porosity, and the technical scheme is as follows:
(a) preparing materials and preparing a blank: the titanium alloy blank comprises the following chemical components in percentage by mass: the titanium alloy blank comprises the following components in percentage by mass: al: 19.5% -21.75%, V: 1.5% -2.5%, Ag: 0.5% -1.25%, Si: 21.5% -23.5%, Zr: 2.5 to 3.5 percent of Ti, and the balance of Ti; firstly, mixing the powder or the particles of the materials with the purity of 99.99 percent according to a certain mass fraction, and carrying out mechanical ball milling for 9-14 hours after mixing to obtain superfine composite powder; mixing the composite powder and isopropanol in a weight ratio of 1.5%, stirring for 5 minutes, putting into an extrusion device for extrusion, and obtaining a rectangular strip-shaped titanium alloy blank with a cross section of 8 multiplied by 50mm in geometric dimension after extrusion forming3The extruded blank is put into a vacuum sintering furnace, the temperature is kept for 90 minutes at the temperature of 1000 ℃, then the titanium alloy blank is softened and annealed, the annealing temperature is 600 ℃, the blank is cooled in the air after being kept for 4 hours, and then the blank is washed for 2 to 3 times in warm water at the temperature of 50 ℃; finally obtaining an easily formed titanium alloy blank with a rectangular cross section;
(b) obtaining the titanium alloy nano material: placing the processed titanium alloy blank between two groups of sliding sheets; the hydraulic transmission block is driven by a hydraulic machine, the hydraulic transmission block drives the parallel rotation side lever, so that the slide sheet is pushed to perform shearing forging on the titanium alloy blank, shearing is stopped when the parallel rotation side lever pushes the inclined angle of the slide sheet to be 45 degrees (the rotation angular speed is 4 rad/s), and the first plastic deformation of the titanium alloy blank can be realized; reversely pushing the parallel rotating side rods through the hydraulic rotating piece, further pushing the other group of sliding pieces to enable the titanium alloy blank to complete reverse deformation, and stopping shearing (the rotating angular speed is 4 rad/s) when the parallel rotating side rods push the inclined angle of the sliding pieces to be 45 degrees, so that the secondary plastic deformation of the titanium alloy blank can be realized; finally, pushing the sliding sheet to change the parallelogram cross section into an initial rectangular cross section (the rotating angular speed is 4 rad/s), so that the third plastic deformation of the titanium alloy blank can be realized; in the process of shearing deformation, the cross section of the blank is kept unchanged, namely the bottom and the height of the cross section of the initial rectangle are equal to those of the four parallels in each deformation stage, so that severe plastic deformation of the titanium alloy material can be realized, and the titanium alloy nano material is obtained;
(c) material forming a porous structure with high porosity: the obtained titanium alloy nanomaterial was immersed in 6L of potassium hydroxide (KOH) aqueous solution at 60 ℃ for 12 hours to remove Si, and then the Si-removed titanium alloy nanomaterial was immersed in 6L of nitric acid (HNO) at room temperature3) Taking out the titanium alloy for 6 hours, washing the titanium alloy, cleaning the titanium alloy by using an ultrasonic technology, repeatedly cleaning the titanium alloy for 2 to 3 times, and drying the titanium alloy in the air for 24 hours to finally obtain the porous titanium alloy nano material with the high porosity of more than 50 percent.
2. The method for preparing the porous titanium alloy nano material by shearing forging as claimed in claim 1, wherein the method comprises the following steps: the shearing forging machine mainly comprises a hydraulic transmission block, a parallel rotation side rod, a slip sheet, an upper supporting piece and a lower supporting piece.
3. The method for preparing the porous titanium alloy nano material by shear forging as claimed in claim 1, wherein the method comprises the following steps: the method comprises the following steps of putting a titanium alloy blank with a rectangular cross section between two groups of sliding sheets, driving a hydraulic transmission block through a hydraulic machine to drive parallel rotation side rods so as to drive the sliding sheets to perform shear forging on the blank, so that severe plastic deformation of the titanium alloy blank is realized, the blank does not need to be removed or reinserted in the process of each pass, and the repeated shear forging of the titanium alloy blank can be realized; according to the method, the high strain value is introduced, so that the titanium alloy blank realizes severe plastic deformation, the crystal grains are refined, the titanium alloy nano material is obtained, and meanwhile, the friction effect based on the extrusion process is reduced, so that the material utilization rate is improved; in the process, the blank does not need to be removed and reinstalled among all the passes, so that the process time is shortened, and the process productivity is obviously improved; meanwhile, in the shearing process, the shearing deformation is expanded to the whole section of the blank by using the plurality of sliding sheets, so that the deformation is more uniform, the mechanical property of the block nano titanium alloy is further improved, and the high strength and the good toughness are realized on the premise of ensuring high density.
4. The method for preparing the porous titanium alloy nano material by shear forging as claimed in claim 1, wherein the method comprises the following steps: the distance between the two groups of sliding sheets is adjustable, and the height is adjustable.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210532238.3A CN114737080B (en) | 2022-05-17 | 2022-05-17 | Method for preparing porous titanium alloy nano material by shearing forging |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210532238.3A CN114737080B (en) | 2022-05-17 | 2022-05-17 | Method for preparing porous titanium alloy nano material by shearing forging |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114737080A true CN114737080A (en) | 2022-07-12 |
| CN114737080B CN114737080B (en) | 2022-09-16 |
Family
ID=82285515
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210532238.3A Active CN114737080B (en) | 2022-05-17 | 2022-05-17 | Method for preparing porous titanium alloy nano material by shearing forging |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114737080B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59107002A (en) * | 1982-12-11 | 1984-06-21 | Toyota Motor Corp | Production of sintered parts |
| US5148965A (en) * | 1990-08-09 | 1992-09-22 | Ladish Co., Inc. | Method of shear forge bonding and products produced thereby |
| CN103540784A (en) * | 2013-10-29 | 2014-01-29 | 昆明理工大学 | Preparation method of biomedical porous titanium alloy |
| CN107349472A (en) * | 2017-06-30 | 2017-11-17 | 浙江德康医疗器械有限公司 | A kind of preparation method of the gradient porous titanium alloy of repetition of promotion bone fusion |
| CN108193071A (en) * | 2018-02-07 | 2018-06-22 | 山东建筑大学 | A kind of continuously extruded preparation method of the renewable porous nano composite material of titanium-based |
| CN109261958A (en) * | 2018-11-15 | 2019-01-25 | 西北有色金属研究院 | Surface coats the medical porous titanium of tantalum coating or the preparation method of titanium alloy material |
| CN111014664A (en) * | 2019-11-19 | 2020-04-17 | 昆明理工大学 | Preparation method of antibacterial porous titanium alloy |
-
2022
- 2022-05-17 CN CN202210532238.3A patent/CN114737080B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59107002A (en) * | 1982-12-11 | 1984-06-21 | Toyota Motor Corp | Production of sintered parts |
| US5148965A (en) * | 1990-08-09 | 1992-09-22 | Ladish Co., Inc. | Method of shear forge bonding and products produced thereby |
| CN103540784A (en) * | 2013-10-29 | 2014-01-29 | 昆明理工大学 | Preparation method of biomedical porous titanium alloy |
| CN107349472A (en) * | 2017-06-30 | 2017-11-17 | 浙江德康医疗器械有限公司 | A kind of preparation method of the gradient porous titanium alloy of repetition of promotion bone fusion |
| CN108193071A (en) * | 2018-02-07 | 2018-06-22 | 山东建筑大学 | A kind of continuously extruded preparation method of the renewable porous nano composite material of titanium-based |
| CN109261958A (en) * | 2018-11-15 | 2019-01-25 | 西北有色金属研究院 | Surface coats the medical porous titanium of tantalum coating or the preparation method of titanium alloy material |
| CN111014664A (en) * | 2019-11-19 | 2020-04-17 | 昆明理工大学 | Preparation method of antibacterial porous titanium alloy |
Non-Patent Citations (2)
| Title |
|---|
| 张志雄等: "钛合金多向锻造工艺研究进展", 《塑性工程学报》 * |
| 张文井等: "钛及钛合金剧烈塑性变形研究进展", 《钛工业进展》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114737080B (en) | 2022-09-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110284089B (en) | Isothermal superplastic deformation method for micro/nano particle reinforced titanium-based composite material | |
| US11634333B2 (en) | Boron-containing titanium-based composite powder for 3D printing and method of preparing same | |
| CN106521238B (en) | Y containing nanometer2O3The high-strength TiAl alloy of fine grain and preparation method thereof | |
| CN101368242B (en) | Amorphous particle reinforced magnesium-base composite material and manufacture process | |
| CN107541615B (en) | A kind of high tough titanium alloy of ocean engineering | |
| WO2020119074A1 (en) | Dental titanium alloy and preparation method therefor | |
| CN111534772A (en) | Preparation method of TC4 titanium alloy finished bar with short process and low cost | |
| CN108977693B (en) | A kind of recrystallization high-strength titanium alloy and preparation method thereof | |
| CN106319282B (en) | A kind of low cost, high-ductility, seawater corrosion resistance titanium alloy | |
| CN114737080B (en) | Method for preparing porous titanium alloy nano material by shearing forging | |
| CN114411072B (en) | Aluminum alloy material with gradient structure and preparation method thereof | |
| CN112522673B (en) | Biomedical magnesium alloy surface rare earth composite film and preparation method thereof | |
| CN109338252A (en) | A kind of zirconium base porous amorphous alloy and preparation method | |
| CN108893654A (en) | A kind of full α phase fine grain high-strength anticorrosion titanium alloy and preparation method thereof | |
| CN1219105C (en) | Micron fine-grained titanium-nickel alloy block material isodiametric corner extrusion preparing method | |
| CN1209477C (en) | Micro fine-grained titanium-nickel-niobium shape memory alloy block material preparing method | |
| Xia et al. | Thermo-mechanical processing, microstructure and mechanical properties of TiZrB alloy | |
| CN112342431B (en) | High-thermal-stability equiaxial nanocrystalline Ti6Al4V-Cu alloy and preparation method thereof | |
| CN112195366B (en) | High-thermal-stability equiaxial nanocrystalline Ti-Zr-Ag alloy and preparation method thereof | |
| CN114934206A (en) | Multi-element aluminide reinforced aluminum-based composite material and preparation method and application thereof | |
| CN108913945B (en) | A kind of high-strength titanium alloy and preparation method thereof | |
| CN1228465C (en) | Micro grain titanium-nickel-palladium-base high-temperature shape memory alloy preparing method | |
| CN113512668A (en) | Boron-containing shape memory alloy and preparation method thereof | |
| CN108070801B (en) | Method for preparing low-cost centimeter-level zirconium-based amorphous alloy by adopting industrial-level sponge zirconium | |
| CN114214584B (en) | Low-temperature 1800 MPa-level ultrahigh-strength pure titanium and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |