CN112517910A - Method for improving strength of high-porosity layered porous titanium and titanium alloy - Google Patents
Method for improving strength of high-porosity layered porous titanium and titanium alloy Download PDFInfo
- Publication number
- CN112517910A CN112517910A CN202011272103.5A CN202011272103A CN112517910A CN 112517910 A CN112517910 A CN 112517910A CN 202011272103 A CN202011272103 A CN 202011272103A CN 112517910 A CN112517910 A CN 112517910A
- Authority
- CN
- China
- Prior art keywords
- freezing
- slurry
- porosity
- titanium alloy
- titanium
- 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.)
- Pending
Links
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 33
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000010936 titanium Substances 0.000 title claims abstract description 28
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 27
- 238000007710 freezing Methods 0.000 claims abstract description 93
- 230000008014 freezing Effects 0.000 claims abstract description 93
- 239000002002 slurry Substances 0.000 claims abstract description 43
- 239000012784 inorganic fiber Substances 0.000 claims abstract description 30
- 238000000498 ball milling Methods 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 239000011148 porous material Substances 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 239000002270 dispersing agent Substances 0.000 claims description 15
- 239000000835 fiber Substances 0.000 claims description 14
- 239000011230 binding agent Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 239000002923 metal particle Substances 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 8
- 239000004800 polyvinyl chloride Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000011810 insulating material Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000011268 mixed slurry Substances 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 4
- 229920000058 polyacrylate Polymers 0.000 claims description 4
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 abstract description 10
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 6
- 239000000956 alloy Substances 0.000 description 6
- 210000000988 bone and bone Anatomy 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 238000009777 vacuum freeze-drying Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- 235000010493 xanthan gum Nutrition 0.000 description 3
- 229920001285 xanthan gum Polymers 0.000 description 3
- 239000000230 xanthan gum Substances 0.000 description 3
- 229940082509 xanthan gum Drugs 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000001054 cortical effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 208000006386 Bone Resorption Diseases 0.000 description 1
- 241000764238 Isis Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 230000024279 bone resorption Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 239000006194 liquid suspension Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Images
Classifications
-
- 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
- B22F3/11—Making porous workpieces or articles
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- 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
- B22F3/1007—Atmosphere
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
- C22C49/10—Refractory metals
- C22C49/11—Titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a method for improving the strength of high-porosity layered porous titanium and titanium alloy, which comprises the following steps: step by stepStep 1, preparing slurry; step 2, performing ball milling treatment on the slurry obtained in the step 1; step 3, freezing the slurry obtained in the step 2 to obtain a cylindrical composite frozen body Fn(ii) a Step 4, the cylindrical composite frozen body F obtained in the step 3 is processednFreeze-drying under vacuum to obtain cylindrical composite frozen body FnSublimating the solvent crystal to obtain a porous blank; and 5, sintering the porous blank obtained in the step 4 in vacuum to obtain the inorganic fiber reinforced layered titanium alloy porous material. The invention solves the problem of low compressive strength of the high-porosity layered titanium alloy prepared by the existing method.
Description
Technical Field
The invention belongs to the technical field of material preparation, and relates to a method for improving the strength of high-porosity layered porous titanium and titanium alloy.
Background
Titanium and titanium alloys are widely used in the biomedical field due to their low density, high strength, excellent corrosion resistance and good biocompatibility. However, the mismatch in young's modulus between titanium alloys and bone presents problems for their application. For example, the young's modulus of TC4 titanium alloy is about 110GPa, much higher than that of bone (<40 GPa). The large difference in modulus will lead to a "stress shielding" effect, further causing bone resorption and implant loosening. As most of the hole structures of cancellous bones of human bodies are lamellar structures, Torres Y et al, published in Materials and Design 2014, paper Design, processing and characterization of titanium coatings with graded porosity, and research on alternative to stress-shielding solutions, show that titanium and titanium alloys are subjected to porous treatment, and the generated hole structures are beneficial to reducing the stress shielding effect by reducing the modulus. Therefore, the porosity becomes an effective means for lowering the Young's modulus of the titanium alloy.
Freeze drying is a common method for preparing high-porosity layered porous materials, and the pore structure prepared by the method is similar to that of natural bones. The principle of the freeze-drying method is to freeze liquid suspension slurry (water-based and non-water-based) to convert the solvent in the slurry into special-shaped 'ice crystals', extrude solid powder particles to intercrystalline positions, sublimate the solvent from solid state to gaseous state under vacuum to remove the solidified phase solvent, obtain a loose porous material preform, and finally densify and sinter the preform to prepare the porous material. At home and abroad, the high-porosity layered porous titanium and titanium alloy are prepared by adopting a freeze-drying method, but the strength of the titanium and titanium alloy is far lower than the compressive strength (about 200MPa) of cortical bone. Published literature: a report on porous structures and mechanical properties of porous titanium by bidirectional compressive casting, published by Yan et al, selected from Materials Science and Engineering C2017, volume 75, page 335, 340, produced a layered porous titanium with a porosity of 67% and a compressive strength of 58MPa by two-way freeze-drying. The paper "structural-processing coatings and mechanical properties in front of Ti-6Al-4V with high aligned porosity and a light weight Ti-6Al-4V-PMMA composition with excellent energy absorption capacity", published by Weaver et Al, is selected from Acta Materialia 2017, volume 132, page 182 and page 192, and the porous Ti6Al4V alloy is prepared by freeze-oriented freeze-drying method, and the mechanical property test result shows that the quasi-static compressive strength is 83MPa when the porosity is 64%. Although the layered porous titanium and titanium alloy with high porosity are prepared, the compressive strength is lower than that of cortical bone.
Disclosure of Invention
The invention aims to provide a method for improving the strength of high-porosity layered porous titanium and titanium alloy, and solves the problem of low compressive strength of high-porosity layered titanium alloy prepared by the conventional method.
The technical scheme adopted by the invention is that the method for improving the strength of the high-porosity layered porous titanium and the titanium alloy specifically comprises the following steps:
step 1, preparing slurry;
step 2, performing ball milling treatment on the slurry obtained in the step 1;
step 3, freezing the slurry obtained in the step 2 to obtain a cylindrical composite frozen body;
step 4, freezing and drying the cylindrical composite frozen body obtained in the step 3 in a vacuum environment to sublimate solvent crystals in the cylindrical composite frozen body to obtain a porous blank body;
and 5, sintering the porous blank obtained in the step 4 in vacuum to obtain the inorganic fiber reinforced layered titanium alloy porous material.
The invention is also characterized in that:
the specific process of the step 1 is as follows:
sequentially adding a dispersing agent and a binder into a solvent, then adding inorganic fibers and metal particles, mixing to obtain slurry, and preparing ceramic slurry with n being more than or equal to 2 groups, wherein the mark is T1,T2,T3,…,Tn-1,TnWherein the volume ratio of the inorganic fibers in the n-th group of pulps is larger than the volume ratio of the solvent in the n-1 th group of pulps.
The solvent in the step 1 is deionized water;
the dispersing agent is any one of polyacrylate, polyvinylpyrrolidone, polyvinyl butyral and citric acid;
the inorganic fiber is any one of silicon carbide fiber, alumina fiber, silicon oxide fiber and carbon fiber.
In the step 1, the addition amount of the dispersing agent is 2 wt.%, the addition amount of the binder is 0.2 wt.%, and the addition amount of the inorganic fiber is 1-10 vol.%.
The specific process of the step 2 is as follows:
and (3) transferring the slurry obtained in the step (1) into a ball milling tank, and carrying out ball milling treatment in a roller ball mill to obtain stable mixed slurry, wherein the rotating speed of the ball mill is 300r/min, and the ball milling time is 24-48 h.
The specific process of the step 3 is as follows:
carrying out ultrasonic treatment on the slurry obtained in the step 2 to remove air bubbles in the slurry, and then carrying out freezing treatment, wherein directional freezing is adopted for freezing, a freezing mold is adopted for freezing, the side wall of the freezing mold is made of a tubular heat-insulating material, the bottom surface of the freezing mold is made of a heat-conducting metal, and the freezing direction is vertical to the ground and upward;
the total n of the freezing molds is more than or equal to 2 groups and respectively marked as M1,M2,M3,…,Mn-1,MnThe composite frozen bodies obtained after each freezing are respectively marked as F1,F2,F3,…,Fn-1,Fn(ii) a The directional freezing temperature is-20 to-10 ℃; the freezing mould is a cylindrical polyvinyl chloride pipe, and the freezing time t is more than or equal to 7 h.
The method for improving the strength of the layered porous titanium and the titanium alloy with high porosity has the beneficial effects that the inorganic fiber is introduced into the layered titanium alloy, so that the compressive strength of the porous material is improved on the premise of ensuring the porous functionality and not reducing the porosity of the porous titanium alloy, and the method has wide application prospect in the field of biological medical treatment.
Drawings
FIG. 1 is a cross-sectional view of an inorganic SiC fiber reinforced layered Ti6Al4V alloy prepared in a method for improving the strength of high-porosity layered porous titanium and titanium alloys.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a method for improving the strength of high-porosity layered porous titanium and titanium alloy, which comprises the following steps:
step 1, preparing slurry;
sequentially adding a dispersing agent and a binder into a solvent, then adding inorganic fibers and metal particles, mixing to obtain slurry, and preparing ceramic slurry with n being more than or equal to 2 groups, wherein the mark is T1,T2,T3,…,Tn-1,TnWherein the volume ratio of the inorganic fibers in the n-th group of pulps is larger than the volume ratio of the solvent in the n-1 th group of pulps.
The solvent is deionized water; the dispersing agent is any one of polyacrylate, polyvinylpyrrolidone, polyvinyl butyral and citric acid; the metal particles are Ti6Al4V alloy; the inorganic fiber is any one of silicon carbide fiber, alumina fiber, silicon oxide fiber and carbon fiber; the addition amount of the dispersant was 2 wt.%, and the addition amount of the binder was 0.2 wt.%; the overall solid content of the porous material is 20 vol.%, and the addition amount of the inorganic fibers is 1-10 vol.%.
Step 2, ball milling;
the slurry T obtained in the step 1 isnTransferring the mixture into a ball milling tank, and carrying out ball milling treatment in a roller ball mill to obtain stable mixed slurry. The rotating speed of the ball mill is 300r/min, and the ball milling time is 24-48 h.
Step 3, freezing;
and (3) carrying out ultrasonic treatment (30 minutes) on the slurry obtained in the step (2) to remove air bubbles in the slurry, and carrying out freezing treatment, wherein directional freezing is adopted for freezing, a freezing mold is adopted for freezing, the side wall of the freezing mold is made of a tubular heat-insulating material, the bottom surface of the freezing mold is made of a heat-conducting metal, and the freezing direction is vertical to the ground and is upward. The total n of the freezing molds is more than or equal to 2 groups and respectively marked as M1,M2,M3,…,Mn-1,MnThe composite frozen bodies obtained after each freezing are respectively marked as F1,F2,F3,…,Fn-1,Fn(ii) a The directional freezing temperature is-20 to-10 ℃; the freezing mould is a cylindrical polyvinyl chloride (PVC) pipe with the inner diameter of 21.5mm and the height of 45 mm. The freezing time t is more than or equal to 7 h; the bottom cold source is a heat-conducting copper plate.
Step 4, vacuum freeze drying
Freeze-drying the cylindrical composite frozen body obtained in the step (3) in a vacuum environment (the freezing time is different according to the amount of the slurry, and is generally 30min to 1 hour) to ensure that the cylindrical composite frozen body FnSublimating the solvent crystal to obtain a porous blank;
step 5, sintering
And (4) sintering the porous blank obtained in the step (4) at 1200 ℃ for 2 hours in vacuum to obtain the inorganic fiber reinforced layered titanium alloy porous material. The vacuum degree in the furnace should be kept at 1 × 10-2Pa below, to ensure that the sample is not oxidized.
According to the method for improving the strength of the high-porosity layered porous titanium, the inorganic fiber is introduced into the layered titanium alloy, the compressive strength of the porous material is improved on the premise that the porous functionality is ensured and the porosity of the porous titanium alloy is not reduced, the defect that the compression performance of the existing layered porous titanium is low under the high porosity is overcome, and the method has a wide application prospect in the field of biomedical science.
Example 1
The embodiment of the invention provides a method for improving the strength of high-porosity layered porous titanium and titanium alloy, which specifically comprises the following steps:
step 1, preparing slurry
Adding 2 wt.% of dispersant into 50ML solvent, fully stirring for 30min at 70 ℃, uniformly mixing, then adding 0.2 wt.% of binder, fully stirring for 2h, uniformly mixing, then adding inorganic fiber, performing ultrasonic dispersion for 1h, finally adding metal particles, and mixing to obtain slurry; the solvent is deionized water; the dispersant is polyacrylate; the binder is xanthan gum; the (metal particle) matrix is Ti6Al4V alloy; the inorganic fiber is silicon carbide fiber; the overall solid content of the porous material was 20 vol.%, and the amount of the inorganic fiber added was 1 vol.%.
Step 2, ball milling
And (3) transferring the slurry obtained in the step (1) to a ball milling tank, and carrying out ball milling treatment in a roller ball mill to obtain stable mixed slurry. The rotating speed of the ball mill is 300r/min, and the ball milling time is 24 h.
Step 3, freezing
And (3) carrying out ultrasonic treatment on the slurry obtained in the step (2) to remove air bubbles in the slurry, carrying out freezing treatment for 30 minutes, wherein directional freezing is adopted for freezing, the freezing temperature is-10 ℃, freezing is adopted for freezing by adopting a freezing mould, the side wall of the freezing mould is a tubular heat-insulating material, the bottom surface of the freezing mould is a heat-conducting metal, and the freezing direction is vertical to the ground and is upward. Freezing molds in 2 groups, respectively labeled as M1、M2The composite frozen bodies obtained after each freezing are respectively marked as F1、F2(ii) a The directional freezing temperature is-20 ℃; the freezing mould is a cylindrical polyvinyl chloride (PVC) pipe with the inner diameter of 21.5mm and the height of 45 mm. The freezing time t is 7 h; the cold source at the bottom of the freezing mould is a heat-conducting copper plate.
Step 4, vacuum freeze drying
Subjecting the cylindrical composite frozen body F obtained in the step 3 to1、F2Freeze-drying under vacuum for 30min to obtain cylindrical composite frozen body F1、F2Sublimating the solvent crystal to obtain a porous blank;
step 5, sintering
And (4) sintering the porous blank obtained in the step (4) in a vacuum furnace at 1200 ℃ and with the vacuum degree kept below 1 x 10 < -2 > Pa for 2 hours to obtain the inorganic fiber reinforced layered titanium alloy porous material.
The cross-sectional topography of the composite porous material of the inorganic SiC fiber reinforced layered titanium alloy prepared in this example is shown in fig. 1.
Example 2
The embodiment of the invention provides a method for improving the strength of high-porosity layered porous titanium and titanium alloy, which specifically comprises the following steps:
step 1, preparing slurry;
adding 2 wt.% of dispersant into 50ML solvent, fully stirring for 30min at 70 ℃, uniformly mixing, then adding 0.2 wt.% of binder, fully stirring for 2h, uniformly mixing, then adding inorganic fiber, performing ultrasonic dispersion for 1h, finally adding metal particles, and mixing to obtain slurry; the solvent is deionized water; the dispersing agent is polyvinyl butyral; the binder is xanthan gum; the (metal particle) matrix is Ti6Al4V alloy; the inorganic fiber is silicon carbide fiber; the overall solid content of the porous material was 20 vol.%, and the amount of the inorganic fiber added was 5 vol.%.
Step 2, ball milling;
and (3) transferring the slurry obtained in the step (1) to a ball milling tank, and carrying out ball milling treatment in a roller ball mill to obtain stable mixed slurry. The rotating speed of the ball mill is 300r/min, and the ball milling time is 30 h.
Step 3, freezing;
and (3) carrying out ultrasonic treatment on the slurry obtained in the step (2) to remove air bubbles in the slurry, and carrying out freezing treatment, wherein directional freezing is adopted for freezing, the freezing temperature is-10 ℃, a freezing mold is adopted for freezing, the side wall of the freezing mold is made of a tubular heat-insulating material, the bottom surface of the freezing mold is made of a heat-conducting metal, and the freezing direction is vertical to the ground and is upward. The freezing molds n are 3 groups, and are respectively marked as M1、M2、M3The composite frozen bodies obtained after each freezing are respectively marked as F1、F2、F3(ii) a The directional freezing temperature is-15 ℃; the freezing mould is cylindrical polyvinyl chloride with the inner diameter of 21.5mm and the height of 45mm(PVC) pipe, freezing time t is 10 h; the cold source at the bottom of the cooling mould is a heat-conducting copper plate.
Step 4, vacuum freeze drying
Subjecting the cylindrical composite frozen body F obtained in the step 3 to1、F2Freeze-drying under vacuum for 40 min to obtain cylindrical composite frozen body F1、F2Sublimating the solvent crystal to obtain a porous blank;
step 5, sintering
Maintaining the porous blank obtained in the step 4 at 1200 ℃ and the vacuum degree of 1 multiplied by 10-2Sintering in a vacuum furnace below Pa for 2h to obtain the inorganic fiber reinforced layered titanium alloy porous material.
Example 3
The embodiment of the invention provides a method for improving the strength of high-porosity layered porous titanium and titanium alloy, which specifically comprises the following steps:
step 1, preparing slurry;
adding 2 wt.% of dispersant into 50ML solvent, fully stirring for 30min at 70 ℃, uniformly mixing, then adding 0.2 wt.% of binder, fully stirring for 2h, uniformly mixing, then adding inorganic fiber, performing ultrasonic dispersion for 1h, finally adding metal particles, and mixing to obtain slurry; the solvent is deionized water; the dispersant is polyvinylpyrrolidone; the binder is xanthan gum; the (metal particle) matrix is Ti6Al4V alloy; the inorganic fiber is silicon carbide fiber; the overall solid content of the porous material was 20 vol.%, and the amount of the inorganic fibers added was 10 vol.%.
Step 2, ball milling
And (3) transferring the slurry obtained in the step (1) to a ball milling tank, and carrying out ball milling treatment in a roller ball mill to obtain stable mixed slurry. The rotating speed of the ball mill is 300r/min, and the ball milling time is 48 h.
Step 3, freezing;
carrying out ultrasonic treatment on the slurry obtained in the step 2 to remove air bubbles in the slurry, and carrying out freezing treatment, wherein directional freezing is adopted for freezing, the freezing temperature is-10 ℃, freezing mould freezing is adopted, the side wall of the freezing mould is a tubular heat-insulating material, the bottom surface of the freezing mould is a heat-conducting metal, and the freezing direction isIs directed vertically upwards. The freezing molds are n in 4 groups and are respectively marked as M1、M2、M3、M4The composite frozen bodies obtained after each freezing are respectively marked as F1、F2、F3、F4The directional freezing temperature is-10 ℃; the freezing mould is a cylindrical polyvinyl chloride (PVC) pipe with the inner diameter of 21.5mm and the height of 45 mm. The freezing time t is 10 h; the cold source at the bottom of the cooling mould is a heat-conducting copper plate.
Step 4, vacuum freeze drying;
subjecting the cylindrical composite frozen body F obtained in the step 3 to1、F2、F3、F4Freeze-drying under vacuum for 1 hr to obtain cylindrical composite frozen body F1、F2、F3、F4Sublimating the solvent crystal to obtain a porous blank;
step 5, sintering;
maintaining the porous blank obtained in the step 4 at 1200 ℃ and the vacuum degree of 1 multiplied by 10-2Sintering in a vacuum furnace below Pa for 2h to obtain the inorganic fiber reinforced layered titanium alloy porous material.
Claims (6)
1. A method for improving the strength of high-porosity layered porous titanium and titanium alloy is characterized by comprising the following steps:
step 1, preparing slurry;
step 2, performing ball milling treatment on the slurry obtained in the step 1;
step 3, freezing the slurry obtained in the step 2 to obtain a cylindrical composite frozen body;
step 4, freezing and drying the cylindrical composite frozen body obtained in the step 3 in a vacuum environment to sublimate solvent crystals in the cylindrical composite frozen body to obtain a porous blank body;
and 5, sintering the porous blank obtained in the step 4 in vacuum to obtain the inorganic fiber reinforced layered titanium alloy porous material.
2. The method for improving the strength of the high-porosity layered porous titanium and the titanium alloy according to claim 1, wherein the specific process of the step 1 is as follows:
sequentially adding a dispersing agent and a binder into a solvent, then adding inorganic fibers and metal particles, mixing to obtain slurry, and preparing ceramic slurry with n being more than or equal to 2 groups, wherein the mark is T1,T2,T3,…,Tn-1,TnWherein the volume ratio of the inorganic fibers in the n-th group of pulps is larger than the volume ratio of the solvent in the n-1 th group of pulps.
3. The method for improving the strength of the high-porosity layered porous titanium and the titanium alloy according to claim 2, wherein the solvent in the step 1 is deionized water;
the dispersing agent is any one of polyacrylate, polyvinylpyrrolidone, polyvinyl butyral and citric acid;
the inorganic fiber is any one of silicon carbide fiber, alumina fiber, silicon oxide fiber and carbon fiber.
4. The method for improving the strength of the high-porosity layered porous titanium and the titanium alloy according to claim 2, wherein the dispersant is added in an amount of 2 wt.%, the binder is added in an amount of 0.2 wt.%, and the inorganic fiber is added in an amount of 1 to 10 vol.% in step 1.
5. The method for improving the strength of the high-porosity layered porous titanium and the titanium alloy according to claim 2, wherein the specific process of the step 2 is as follows:
and (3) transferring the slurry obtained in the step (1) into a ball milling tank, and carrying out ball milling treatment in a roller ball mill to obtain stable mixed slurry, wherein the rotating speed of the ball mill is 300r/min, and the ball milling time is 24-48 h.
6. The method for improving the strength of the high-porosity layered porous titanium and the titanium alloy according to claim 5, wherein the specific process of the step 3 is as follows:
carrying out ultrasonic treatment on the slurry obtained in the step 2 to remove air bubbles in the slurry, and then carrying out freezing treatment, wherein directional freezing is adopted for freezing, a freezing mold is adopted for freezing, the side wall of the freezing mold is made of a tubular heat-insulating material, the bottom surface of the freezing mold is made of a heat-conducting metal, and the freezing direction is vertical to the ground and upward;
the total n of the freezing molds is more than or equal to 2 groups and respectively marked as M1,M2,M3,…,Mn-1,MnThe composite frozen bodies obtained after each freezing are respectively marked as F1,F2,F3,…,Fn-1,Fn(ii) a The directional freezing temperature is-20 to-10 ℃; the freezing mould is a cylindrical polyvinyl chloride pipe, and the freezing time t is more than or equal to 7 h.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011272103.5A CN112517910A (en) | 2020-11-13 | 2020-11-13 | Method for improving strength of high-porosity layered porous titanium and titanium alloy |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202011272103.5A CN112517910A (en) | 2020-11-13 | 2020-11-13 | Method for improving strength of high-porosity layered porous titanium and titanium alloy |
Publications (1)
Publication Number | Publication Date |
---|---|
CN112517910A true CN112517910A (en) | 2021-03-19 |
Family
ID=74982620
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202011272103.5A Pending CN112517910A (en) | 2020-11-13 | 2020-11-13 | Method for improving strength of high-porosity layered porous titanium and titanium alloy |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN112517910A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113185312A (en) * | 2021-04-09 | 2021-07-30 | 西安理工大学 | Porous SiC ceramic with high porosity, high strength and low thermal conductivity and preparation method thereof |
CN113477923A (en) * | 2021-06-29 | 2021-10-08 | 吉林大学重庆研究院 | Preparation and sintering method of titanium alloy slurry for 3D printing |
CN114000069A (en) * | 2021-10-09 | 2022-02-01 | 中国航发北京航空材料研究院 | Preparation method of continuous SiC fiber reinforced metal matrix composite lattice structure |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006299405A (en) * | 2005-03-24 | 2006-11-02 | Mitsubishi Materials Corp | Method for producing porous metal or porous ceramics |
JP2013189676A (en) * | 2012-03-13 | 2013-09-26 | National Institute Of Advanced Industrial Science & Technology | Metallic porous body and method for producing metallic porous body |
CN108638590A (en) * | 2018-05-15 | 2018-10-12 | 西安交通大学 | Fibre reinforced foamed aluminium-pyramid sandwich plate composite construction and preparation method thereof |
CN109940162A (en) * | 2019-04-30 | 2019-06-28 | 西安理工大学 | A kind of preparation method of carbide In-sltu reinforcement titanium and its alloy porous bracket |
CN110385437A (en) * | 2019-07-03 | 2019-10-29 | 西安理工大学 | A kind of preparation method of directional fiber In-sltu reinforcement titanium and its alloy bracket |
CN110629072A (en) * | 2019-10-10 | 2019-12-31 | 太原理工大学 | Method for preparing porous titanium-aluminum alloy with lamellar structure based on freezing molding process |
CN110732672A (en) * | 2019-12-11 | 2020-01-31 | 中南大学 | gradient metal-based porous material and preparation method and application thereof |
-
2020
- 2020-11-13 CN CN202011272103.5A patent/CN112517910A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006299405A (en) * | 2005-03-24 | 2006-11-02 | Mitsubishi Materials Corp | Method for producing porous metal or porous ceramics |
JP2013189676A (en) * | 2012-03-13 | 2013-09-26 | National Institute Of Advanced Industrial Science & Technology | Metallic porous body and method for producing metallic porous body |
CN108638590A (en) * | 2018-05-15 | 2018-10-12 | 西安交通大学 | Fibre reinforced foamed aluminium-pyramid sandwich plate composite construction and preparation method thereof |
CN109940162A (en) * | 2019-04-30 | 2019-06-28 | 西安理工大学 | A kind of preparation method of carbide In-sltu reinforcement titanium and its alloy porous bracket |
CN110385437A (en) * | 2019-07-03 | 2019-10-29 | 西安理工大学 | A kind of preparation method of directional fiber In-sltu reinforcement titanium and its alloy bracket |
CN110629072A (en) * | 2019-10-10 | 2019-12-31 | 太原理工大学 | Method for preparing porous titanium-aluminum alloy with lamellar structure based on freezing molding process |
CN110732672A (en) * | 2019-12-11 | 2020-01-31 | 中南大学 | gradient metal-based porous material and preparation method and application thereof |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113185312A (en) * | 2021-04-09 | 2021-07-30 | 西安理工大学 | Porous SiC ceramic with high porosity, high strength and low thermal conductivity and preparation method thereof |
CN113477923A (en) * | 2021-06-29 | 2021-10-08 | 吉林大学重庆研究院 | Preparation and sintering method of titanium alloy slurry for 3D printing |
CN114000069A (en) * | 2021-10-09 | 2022-02-01 | 中国航发北京航空材料研究院 | Preparation method of continuous SiC fiber reinforced metal matrix composite lattice structure |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN112517910A (en) | Method for improving strength of high-porosity layered porous titanium and titanium alloy | |
CN111644615B (en) | Preparation method for realizing high strength and toughness of TC4 titanium alloy by co-strengthening method | |
CN109097657B (en) | Mo nanoparticle reinforced CoCrNi intermediate entropy alloy composite material and preparation method thereof | |
CN106521219B (en) | A kind of preparation method of TiC granule intensified titaniums based porous materials | |
WO2012142952A1 (en) | Porous tantalum rod | |
CN105169471A (en) | Implant porous niobium-titanium alloy material for medical use and preparation method of alloy material | |
Gülsoy et al. | Particle morphology influence on mechanical and biocompatibility properties of injection molded Ti alloy powder | |
CN111410517B (en) | Carbon nanotube and graphene synergistically enhanced aluminum oxide-based composite material and preparation method thereof | |
CN107602111B (en) | Preparation method of porous biological ceramic | |
Eqtesadi et al. | Reinforcement with reduced graphene oxide of bioactive glass scaffolds fabricated by robocasting | |
CN113304323B (en) | Porous polyether-ether-ketone-hydroxyapatite composite material and preparation method and application thereof | |
Han et al. | Ti/SiO2 composite fabricated by powder metallurgy for orthopedic implant | |
Zhang et al. | Fabrication and properties of porous β-tricalcium phosphate ceramics prepared using a double slip-casting method using slips with different viscosities | |
CN111254304B (en) | Preparation method of in-situ synthesized titanium-nickel alloy framework reinforced titanium-based composite material | |
CN109332700B (en) | Preparation method of TiB-reinforced medical porous titanium | |
Wang et al. | Preparation of porous titanium materials by powder sintering process and use of space holder technique | |
Kang et al. | Advanced composite material: effect of composite SiC on compressive strength and hardness of porous titanium | |
WO2011147139A1 (en) | Porous niobium used as metal medical implant material and preparation method thereof | |
CN113210627A (en) | Preparation method of carbide-reinforced TiAl-based nanocomposite | |
CN110423911B (en) | Mesh-shaped particle reinforced degradable zinc-based cermet and preparation method thereof | |
CN107601902B (en) | Rubidium-containing bioglass ceramic and preparation method thereof | |
Hu et al. | In situ formation of nano-hydroxyapatite whisker reinfoced porous β-TCP scaffolds | |
CN112957522B (en) | Rigidity-adjustable porous liquid metal bone tissue engineering scaffold and preparation method thereof | |
CN110408810B (en) | Method for preparing porous titanium by calcium thermal reduction of porous TiO | |
CN110697725B (en) | Preparation method of lithium disilicate whisker |
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 | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210319 |
|
RJ01 | Rejection of invention patent application after publication |