CN103805797A - Preparation method of medical porous titanium/porous titanium alloy - Google Patents

Preparation method of medical porous titanium/porous titanium alloy Download PDF

Info

Publication number
CN103805797A
CN103805797A CN201410020662.5A CN201410020662A CN103805797A CN 103805797 A CN103805797 A CN 103805797A CN 201410020662 A CN201410020662 A CN 201410020662A CN 103805797 A CN103805797 A CN 103805797A
Authority
CN
China
Prior art keywords
titanium
porous titanium
porous
net strip
titanium alloy
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
Application number
CN201410020662.5A
Other languages
Chinese (zh)
Other versions
CN103805797B (en
Inventor
寇宏超
李金山
李福平
唐斌
徐广胜
王军
胡锐
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Northwestern Polytechnical University
Original Assignee
Northwestern Polytechnical University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Northwestern Polytechnical University filed Critical Northwestern Polytechnical University
Priority to CN201410020662.5A priority Critical patent/CN103805797B/en
Publication of CN103805797A publication Critical patent/CN103805797A/en
Application granted granted Critical
Publication of CN103805797B publication Critical patent/CN103805797B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a preparation method of medical porous titanium/porous titanium alloy. The porous titanium/porous titanium alloy with aperture S being 200-700 mu m and porosity P being 20%-70% is obtained by cutting pieces, laminating and vacuum diffusion bonding. In the preparation method disclosed by the invention, the porosity of the porous titanium/titanium alloy can be better designed, adjusted and controlled, and meanwhile as the temperature of the vacuum diffusion bonding is below a beta phase transition point, the tissue type of titanium/titanium alloy is not changed before and after the vacuum diffusion bonding, so that the tissue type of the porous titanium/titanium alloy is controllable; a pore-forming agent does not need to be added in preparation, so that the problem of pollution cannot be caused. The preparation method disclosed by the invention has the characteristics of simple process, low energy consumption, low cost, and easiness in realization of continuous industrial production.

Description

A kind of preparation method of medical porous titanium/porous titanium alloy
Technical field
The present invention relates to POROUS TITANIUM/titanium alloy technical field, specifically a kind of preparation method of medical porous titanium/titanium alloy.
Background technology
Titanium alloy of the present invention refers to type alpha+beta and β type medical titanium alloy.POROUS TITANIUM/titanium alloy combines many structures and the performance characteristics of porous material and titanium/titanium alloy, have good mechanics and chemical property, as specific tenacity is high, corrosion resistance nature is strong, also have good biocompatibility, be the medical metal material most with development prospect simultaneously.Titanium or titanium alloy porous can effectively realize the regulation and control of its Young's modulus, solves stress shielding problem, realizes the mechanical matching between implant and osseous tissue.Meanwhile, titanium or titanium alloy porous is conducive to adhering to, breed and breaking up of cell, can promote the transmission of body fluid and the growth of osseous tissue.
The performance of POROUS TITANIUM/titanium alloy and its organization type and pore texture have very large relation, and different organization types and pore texture can produce material impact to its mechanical property.Therefore,, in order to reach good biomechanics suitability, the preparation method of medical porous titanium/titanium alloy need have stronger designability and controllability to its organization type and pore texture.
At present, the preparation method of POROUS TITANIUM/titanium alloy has powder metallurgic method, pore-forming material method, speed forming method etc.POROUS TITANIUM/the titanium alloy that adopts titanium valve pressure sintering method to prepare exists porosity low, the shortcomings such as aperture is difficult to control and intensity is low, if Ik-Hyun Oh etc. is at Ik-Hyun Oh, Naoyuki Nomura, Naoya Masahashi, in Shuji Hanada.Mechanical properties of porous titanium compacts prepared by powder sintering.Scripta Materialia49 (2003) 1197 – 1202, a kind of employing titanium valve hot pressing sintering method is disclosed, the POROUS TITANIUM porosity that the method is prepared is 40% to the maximum, and porosity and aperture and distribution thereof are difficult to control.
The patent No. is in the innovation and creation of CN201310005574.3, to disclose a kind of stack of titanium net and vacuum sintering method of preparing porous titanium alloy; the method pore texture is easy to control; be suitable for large-scale production; but because sintering temperature is more than titanium alloy beta transformation temperature, sintering process has changed the original structure type of porous titanium alloy.Pore-forming material method can realize better and controlling the aperture of POROUS TITANIUM, but because the introducing meeting of pore-forming material is to bringing pollution problem, particularly considers that, as medical embedded material, the method is more inadvisable.Speed forming method is a kind of POROUS TITANIUM/titanium alloys Preparation Method growing up at present, design and the controllability of the method to pore texture is strong, but preparation technology causes the original structure type of POROUS TITANIUM/titanium alloy to change, and in POROUS TITANIUM/titanium alloy of preparing, there is unfused titanium valve, be unfavorable for implant long service in vivo, have complicated process of preparation, high in cost of production problem simultaneously.
Summary of the invention
Be difficult to design for overcoming the porosity existing in prior art, organization type changes, has pollution before and after preparation technology, and complicated process of preparation, deficiency that cost is high, the present invention proposes a kind of preparation method of medical porous titanium/porous titanium alloy.
Titanium alloy of the present invention refers to type alpha+beta and β type medical titanium alloy.
Detailed process of the present invention is:
Step 1: cut-parts.Titanium net or titanium alloy reticulated are cut into multi-disc Titanium net strip or titanium mesh; The shape of described Titanium net strip or titanium mesh is consistent with the shape of the medical porous titanium/porous titanium alloy of preparation;
Step 2: clean.
Step 3: lamination.Determine the weight in average M of described multi-disc Titanium net strip or titanium mesh, determine the lamination n of Titanium net strip or titanium mesh according to the weight in average M of Titanium net strip or titanium mesh; The unit of the weight in average M of described multi-disc Titanium net strip or titanium mesh is g;
When described Titanium net strip or titanium mesh are while being square, by formula 1) determine the lamination n of this Titanium net strip or titanium mesh,
n = ρ × ( 1 - P ) × A × B × C M × 10 - 3 - - - 1 )
Formula 1) in, the density of POROUS TITANIUM/porous titanium alloy that ρ is required preparation; P is the porosity of the POROUS TITANIUM/porous titanium alloy of required preparation; M is the weight in average of every Titanium net strip; A × B × C is the length × wide × height of POROUS TITANIUM/porous titanium alloy profile of required preparation; The unit of POROUS TITANIUM/porous titanium alloy physical dimension of required preparation is mm;
When described Titanium net strip or titanium mesh are while being circular, by formula 2) determine the lamination n of this Titanium net strip or titanium mesh,
n = ρ × ( 1 - P ) × 3.14 × ( D 2 ) 2 × C M × 10 - 3 - - - 2 )
Formula 2) in, the density of the porosity of POROUS TITANIUM/porous titanium alloy that ρ is required preparation; P is the porosity of the POROUS TITANIUM/porous titanium alloy of required preparation; M is the weight in average of every Titanium net strip.D is the diameter of the POROUS TITANIUM/porous titanium alloy of required preparation; C is the height of the POROUS TITANIUM/porous titanium alloy of required preparation; The unit of POROUS TITANIUM/porous titanium alloy physical dimension of required preparation is mm;
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N;
Repeating step one cutting titanium net or titanium alloy reticulated, makes the sum of Titanium net strip that cutting obtains or titanium mesh equal required Titanium net strip and counts N; Repeating step two, cleans the sheet Titanium net strip obtaining or titanium mesh.Titanium net strip or titanium mesh after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium alloy.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: the blank that obtains medical porous titanium alloy is placed in to vacuum diffusion and connects between the push-down head and seaming chuck of stove; The height of adjusting seaming chuck, making the vertical height between seaming chuck and push-down head is H=1.2～1.4 × C, the height of POROUS TITANIUM/porous titanium alloy that wherein C is required preparation; The unit of the height C of the POROUS TITANIUM/porous titanium alloy of vertical height H and required preparation is mm.
To vacuum, diffusion connects stove evacuation; When vacuum diffusion connects stove evacuation to≤10 -3when Pa, vacuum diffusion connection stove is heated to T-δ T ℃ with the speed of 10～15 ℃/min, wherein δ T is 120～140 ℃.When temperature arrives T ℃ of T-δ within vacuum diffusion connects stove, by the seaming chuck H-C that declines, and be incubated 1～2h.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, and obtaining aperture S is 200～700 μ m, POROUS TITANIUM/porous titanium alloy that porosity P is 20～70%.
The organization type of described titanium net or titanium alloy reticulated is bifurcation tissue or equiaxed structure or lamellar structure or basket tissue.
The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.
In the present invention, because vacuum diffusion connects temperature below beta transformation point, before and after vacuum diffusion connects, the organization type of titanium/titanium alloy does not change.Therefore, the organization type of POROUS TITANIUM/titanium alloy can be regulated and controled by the organization type of original titanium net.
While adopting the present invention to prepare POROUS TITANIUM/titanium alloy, the porosity of POROUS TITANIUM/titanium alloy can be designed and be regulated and controled by raw-material porosity and preparation technology, being simultaneously consistent of preparation technology raw-material aperture, front and back and POROUS TITANIUM/titanium alloy.Preparation technology of the present invention does not need to add pore-forming material, therefore can not produce because pore-forming material is removed the pollution problem only not causing, and the present invention to have technique simple, energy consumption is low, cost is low, is easy to realize the feature of continuity suitability for industrialized production.
For verifying effect of the present invention, the present invention adopts mercury penetration method to measure porosity and the mean pore size of POROUS TITANIUM/titanium alloy of each embodiment, adopts the organization type of metallurgical analysis POROUS TITANIUM/titanium alloy.POROUS TITANIUM/titanium alloy structure parameter of embodiment 1～12 preparation is as shown in table 1.
POROUS TITANIUM/titanium alloy structure parameter that table 1 embodiment 1～12 prepares
Figure BDA0000458057300000031
Figure BDA0000458057300000041
As shown in Table 1, deviation between its porosity measured value of POROUS TITANIUM/titanium alloy prepared by the present invention and design load is between ± 2%, deviation between mean pore size measured value and design load is between ± 10 μ m, the measured value of organization type is consistent with design load, in preparation process, do not use pore-forming material simultaneously, can production pollution problem.Therefore,, while adopting the present invention to prepare POROUS TITANIUM/titanium alloy, the porosity of POROUS TITANIUM/titanium alloy can be designed preferably and be regulated and controled, the aperture of POROUS TITANIUM/titanium alloy and organization type and raw-material being consistent.
Embodiment
Embodiment 1
The present embodiment is the preparation method of the medical porous titanium alloy of a kind of type alpha+beta.
The starting material of the present embodiment are Ti-6Al-4V titanium net, the beta transformation point T=980 ℃ of Ti-6Al-4V.The mean pore size S=200 μ m of prepared medical porous titanium alloy, porosity P=50%, organization type is equiaxed structure.Prepared medical porous titanium alloy is rectangular parallelepiped, and physical dimension is A × B × C, i.e. the length of this medical porous titanium alloy × wide × height, and in the present embodiment, the physical dimension of prepared medical porous titanium alloy is A × B × C=50 × 50 × 10mm.
The detailed process of the present embodiment is:
Step 1: cut-parts.Be that equiaxed structure, aperture are 200 μ m by organization type, the Ti-6Al-4V titanium net that porosity is 75% is cut into the Titanium net strip that 20 chip sizes are 50 × 50mm.
Step 2: clean.The Titanium net strip obtaining is soaked to 0.5min in mix acid liquor.The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.Titanium net strip after pickling is adopted to deionized water ultrasonic cleaning 15min.Cleaning is dried after completing.
Step 3: lamination.Adopt electronic balance to weigh respectively the weight of 20 Titanium net strips that obtain in step 2, and calculate the weight in average M=0.35g of every Titanium net strip.Determine the lamination n of Titanium net strip according to formula (1),
n = ρ × ( 1 - P ) × A × B × C M × 10 - 3 - - - ( 1 )
In formula, ρ is the density of entity Ti-6Al-4V, ρ=4.51g/cm 3;
P is the porosity of the porous Ti-6Al-4V of required preparation, P=50%;
M is the weight in average of every Titanium net strip, in the present embodiment, and the weight in average=0.35g of every Titanium net strip.
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N=161.Repeating step one cutting Ti-6Al-4V titanium net, makes the sum of the Titanium net strip that cutting obtains equal 161.Repeating step two, cleans obtain 161 Titanium net strips.161 titanium nets after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium alloy.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: vacuum diffusion connects.The blank that obtains medical porous titanium alloy is placed in to the push-down head upper surface that vacuum diffusion connects stove, and seaming chuck is declined, make height H=C × 1.2～1.4 between described seaming chuck lower surface and push-down head upper surface.In the present embodiment, C=10mm, height coefficient gets 1.2, therefore the height H=12mm between seaming chuck lower surface and push-down head upper surface.Vacuum diffusion is connected to stove evacuation to≤10 -3when Pa, start vacuum diffusion connection stove to be heated to 850 ℃ with the speed of 10 ℃/min.In the time that temperature in stove reaches 850 ℃, seaming chuck is declined, the height of decline is H-C, in the present embodiment, 12mm-10mm=2mm, and be incubated 1h under this state.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, obtains required porous Ti-6Al-4V.
Embodiment 2
The present embodiment is the preparation method of the medical porous titanium alloy of a kind of type alpha+beta.
The starting material of the present embodiment are Ti-6Al-4V titanium net, the beta transformation point T=980 ℃ of Ti-6Al-4V.The mean pore size S=700 μ m of prepared medical porous titanium alloy, porosity P=20%, organization type is bifurcation tissue.Prepared medical porous titanium alloy is rectangular parallelepiped, and physical dimension is A × B × C, i.e. the length of this medical porous titanium alloy × wide × height, and in the present embodiment, the physical dimension of prepared medical porous titanium alloy is A × B × C=60 × 80 × 20mm.
The detailed process of the present embodiment is:
Step 1: cut-parts.Be that bifurcation tissue, aperture are 700 μ m by organization type, the Ti-6Al-4V titanium net that porosity is 75% is cut into the Titanium net strip that 25 chip sizes are 60 × 80mm.
Step 2: clean.The Titanium net strip obtaining is soaked to 1min in mix acid liquor.The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.Titanium net strip after pickling is adopted to deionized water ultrasonic cleaning 15min.Cleaning is dried after completing.
Step 3: lamination.Adopt electronic balance to weigh respectively the weight of 25 Titanium net strips that obtain in step 2, and calculate the weight in average M=3.1g of every Titanium net strip.Determine the lamination n of Titanium net strip according to formula (1),
n = ρ × ( 1 - P ) × A × B × C M × 10 - 3 - - - ( 1 )
In formula, ρ is the density of entity Ti-6Al-4V, ρ=4.51g/cm 3;
P is the porosity of the porous Ti-6Al-4V of required preparation, P=20%;
M is the weight in average of every Titanium net strip, in the present embodiment, and the weight in average=3.1g of every Titanium net strip.
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N=112.Repeating step one cutting Ti-6Al-4V titanium net, makes the sum of the Titanium net strip that cutting obtains equal 112.Repeating step two, cleans obtain 112 Titanium net strips.112 titanium nets after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium alloy.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: vacuum diffusion connects.The blank that obtains medical porous titanium alloy is placed in to the push-down head upper surface that vacuum diffusion connects stove, and seaming chuck is declined, make height H=C × 1.2～1.4 between described seaming chuck lower surface and push-down head upper surface.In the present embodiment, C=20mm, height coefficient gets 1.3, therefore the height H=26mm between seaming chuck lower surface and push-down head upper surface.Vacuum diffusion is connected to stove evacuation to≤10 -3when Pa, start vacuum diffusion connection stove to be heated to 860 ℃ with the speed of 12 ℃/min.In the time that temperature in stove reaches 860 ℃, seaming chuck is declined, the height of decline is H-C, in the present embodiment, 26mm-20mm=6mm, and be incubated 1.5h under this state.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, obtains required porous Ti-6Al-4V.
Embodiment 3
The present embodiment is the preparation method of the medical porous titanium alloy of a kind of type alpha+beta.
The starting material of the present embodiment are Ti-6Al-4V titanium net, the beta transformation point T=980 ℃ of Ti-6Al-4V.The mean pore size S=500 μ m of prepared medical porous titanium alloy, porosity P=40%, organization type is lamellar structure.Prepared medical porous titanium alloy is rectangular parallelepiped, and physical dimension is A × B × C, i.e. the length of this medical porous titanium alloy × wide × height, and in the present embodiment, the physical dimension of prepared medical porous titanium alloy is A × B × C=100 × 50 × 30mm.
The detailed process of the present embodiment is:
Step 1: cut-parts.Be that lamellar structure, aperture are 500 μ m by organization type, the Ti-6Al-4V titanium net that porosity is 75% is cut into the Titanium net strip that 30 chip sizes are 100 × 50mm.
Step 2: clean.The Titanium net strip obtaining is soaked to 1min in mix acid liquor.The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.Titanium net strip after pickling is adopted to deionized water ultrasonic cleaning 20min.Cleaning is dried after completing.
Step 3: lamination.Adopt electronic balance to weigh respectively the weight of 30 Titanium net strips that obtain in step 2, and calculate the weight in average M=2.2g of every Titanium net strip.Determine the lamination n of Titanium net strip according to formula (1),
n = ρ × ( 1 - P ) × A × B × C M × 10 - 3 - - - ( 1 )
In formula, ρ is the density of entity Ti-6Al-4V, ρ=4.51g/cm 3;
P is the porosity of the porous Ti-6Al-4V of required preparation, P=40%;
M is the weight in average of every Titanium net strip, in the present embodiment, and the weight in average=2.2g of every Titanium net strip.
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N=185.Repeating step one cutting Ti-6Al-4V titanium net, makes the sum of the Titanium net strip that cutting obtains equal 185.Repeating step two, cleans obtain 185 Titanium net strips.185 titanium nets after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium alloy.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: vacuum diffusion connects.The blank that obtains medical porous titanium alloy is placed in to the push-down head upper surface that vacuum diffusion connects stove, and seaming chuck is declined, make height H=C × 1.2～1.4 between described seaming chuck lower surface and push-down head upper surface.In the present embodiment, C=30mm, height coefficient gets 1.4, therefore the height H=42mm between seaming chuck lower surface and push-down head upper surface.Vacuum diffusion is connected to stove evacuation to≤10 -3when Pa, start vacuum diffusion connection stove to be heated to 855 ℃ with the speed of 12 ℃/min.In the time that temperature in stove reaches 855 ℃, seaming chuck is declined, the height of decline is H-C, in the present embodiment, 42mm-30mm=12mm, and be incubated 1.5h under this state.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, obtains required porous Ti-6Al-4V.
Embodiment 4
The present embodiment is a kind of preparation method of medical porous titanium.
The starting material of the present embodiment are pure titanium net, the beta transformation point T=885 ℃ of pure titanium.The mean pore size S=400 μ m of prepared medical porous titanium, porosity P=70%, organization type is equiaxed structure.Prepared medical porous titanium is rectangular parallelepiped, and physical dimension is A × B × C, i.e. the length of this medical porous titanium × wide × height, and in the present embodiment, the physical dimension of prepared medical porous titanium is A × B × C=50 × 50 × 50mm.
The detailed process of the present embodiment is:
Step 1: cut-parts.Be that equiaxed structure, aperture are 400 μ m by organization type, the pure titanium net that porosity is 75% is cut into the Titanium net strip that 30 chip sizes are 50 × 50mm.
Step 2: clean.The Titanium net strip obtaining is soaked to 0.8min in mix acid liquor.The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.Titanium net strip after pickling is adopted to deionized water ultrasonic cleaning 16min.Cleaning is dried after completing.
Step 3: lamination.Adopt electronic balance to weigh respectively the weight of 30 Titanium net strips that obtain in step 2, and calculate the weight in average M=0.85g of every Titanium net strip.Determine the lamination n of Titanium net strip according to formula (1),
n = ρ × ( 1 - P ) × A × B × C M × 10 - 3 - - - ( 1 )
In formula, ρ is the density of the pure titanium of entity, ρ=4.51g/cm 3;
P is the porosity of the POROUS TITANIUM of required preparation, P=70%;
M is the weight in average of every Titanium net strip, in the present embodiment, and the weight in average=0.85g of every Titanium net strip.
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N=199.The pure titanium net of repeating step one cutting, makes the sum of the Titanium net strip that cutting obtains equal 199.Repeating step two, cleans obtain 199 Titanium net strips.199 titanium nets after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: vacuum diffusion connects.The blank that obtains medical porous titanium is placed in to the push-down head upper surface that vacuum diffusion connects stove, and seaming chuck is declined, make height H=C × 1.2～1.4 between described seaming chuck lower surface and push-down head upper surface.In the present embodiment, C=50mm, height coefficient gets 1.2, therefore the height H=60mm between seaming chuck lower surface and push-down head upper surface.Vacuum diffusion is connected to stove evacuation to≤10 -3when Pa, start vacuum diffusion connection stove to be heated to 765 ℃ with the speed of 15 ℃/min.In the time that temperature in stove reaches 765 ℃, seaming chuck is declined, the height of decline is H-C, in the present embodiment, 60mm-50mm=10mm, and be incubated 1h under this state.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, obtains required POROUS TITANIUM.
Embodiment 5
The present embodiment is the preparation method of the medical porous titanium alloy of a kind of β type.
The starting material of the present embodiment are Ti-13Nb-13Zr titanium net, the beta transformation point T=735 ℃ of Ti-13Nb-13Zr.The mean pore size S=700 μ m of prepared medical porous titanium alloy, porosity P=70%, organization type is lamellar structure.Prepared medical porous titanium alloy is rectangular parallelepiped, and physical dimension is A × B × C, i.e. the length of this medical porous titanium alloy × wide × height, and in the present embodiment, the physical dimension of prepared medical porous titanium alloy is A × B × C=100 × 100 × 50mm
The detailed process of the present embodiment is:
Step 1: cut-parts.Be that lamellar structure, aperture are 700 μ m by organization type, the Ti-13Nb-13Zr titanium net that porosity is 75% is cut into the Titanium net strip that 20 chip sizes are 100 × 100mm.
Step 2: clean.The Titanium net strip obtaining is soaked to 0.5min in mix acid liquor.The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.Titanium net strip after pickling is adopted to deionized water ultrasonic cleaning 15min.Cleaning is dried after completing.
Step 3: lamination.Adopt electronic balance to weigh respectively the weight of 20 Titanium net strips that obtain in step 2, and calculate the weight in average M=6.4g of every Titanium net strip.Determine the lamination n of Titanium net strip according to formula (1),
n = ρ × ( 1 - P ) × A × B × C M × 10 - 3 - - - ( 1 )
In formula, ρ is the density of entity Ti-13Nb-13Zr, ρ=4.51g/cm 3;
P is the porosity of the porous Ti-13Nb-13Zr of required preparation, P=70%;
M is the weight in average of every Titanium net strip, in the present embodiment, and the weight in average=6.4g of every Titanium net strip.
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N=106.Repeating step one cutting Ti-13Nb-13Zr titanium net, makes the sum of the Titanium net strip that cutting obtains equal 106.Repeating step two, cleans obtain 106 Titanium net strips.106 titanium nets after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium alloy.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: vacuum diffusion connects.The blank that obtains medical porous titanium alloy is placed in to the push-down head upper surface that vacuum diffusion connects stove, and seaming chuck is declined, make height H=C × 1.2～1.4 between described seaming chuck lower surface and push-down head upper surface.In the present embodiment, C=50mm, height coefficient gets 1.2, therefore the height H=60mm between seaming chuck lower surface and push-down head upper surface.Vacuum diffusion is connected to stove evacuation to≤10 -3when Pa, start vacuum diffusion connection stove to be heated to 615 ℃ with the speed of 10 ℃/min.In the time that temperature in stove reaches 615 ℃, seaming chuck is declined, the height of decline is H-C, in the present embodiment, 60mm-50mm=10mm, and be incubated 1h under this state.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, obtains required porous Ti-13Nb-13Zr.
Embodiment 6
The present embodiment is the preparation method of the medical porous titanium alloy of a kind of β type.
The starting material of the present embodiment are Ti-13Nb-13Zr titanium net, the beta transformation point T=735 ℃ of Ti-13Nb-13Zr.The mean pore size S=500 μ m of prepared medical porous titanium alloy, porosity P=50%, organization type is basket tissue.Prepared medical porous titanium alloy is rectangular parallelepiped, and physical dimension is A × B × C, i.e. the length of this medical porous titanium alloy × wide × height, and in the present embodiment, the physical dimension of prepared medical porous titanium alloy is A × B × C=40 × 80 × 60mm
The detailed process of the present embodiment is:
Step 1: cut-parts.Be that basket tissue, aperture are 500 μ m by organization type, the Ti-13Nb-13Zr titanium net that porosity is 75% is cut into the Titanium net strip that 30 chip sizes are 40 × 80mm.
Step 2: clean.The Titanium net strip obtaining is soaked to 1min in mix acid liquor.The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.Titanium net strip after pickling is adopted to deionized water ultrasonic cleaning 20min.Cleaning is dried after completing.
Step 3: lamination.Adopt electronic balance to weigh respectively the weight of 30 Titanium net strips that obtain in step 2, and calculate the weight in average M=1.41g of every Titanium net strip.Determine the lamination n of Titanium net strip according to formula (1),
n = ρ × ( 1 - P ) × A × B × C M × 10 - 3 - - - ( 1 )
In formula, ρ is the density of entity Ti-13Nb-13Zr, ρ=4.51g/cm 3;
P is the porosity of the porous Ti-13Nb-13Zr of required preparation, P=50%;
M is the weight in average of every Titanium net strip, in the present embodiment, and the weight in average=1.41g of every Titanium net strip.
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N=307.Repeating step one cutting Ti-13Nb-13Zr titanium net, makes the sum of the Titanium net strip that cutting obtains equal 307.Repeating step two, cleans obtain 307 Titanium net strips.307 titanium nets after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium alloy.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: vacuum diffusion connects.The blank that obtains medical porous titanium alloy is placed in to the push-down head upper surface that vacuum diffusion connects stove, and seaming chuck is declined, make height H=C × 1.2～1.4 between described seaming chuck lower surface and push-down head upper surface.In the present embodiment, C=60mm, height coefficient gets 1.4, therefore the height H=84mm between seaming chuck lower surface and push-down head upper surface.Vacuum diffusion is connected to stove evacuation to≤10 -3when Pa, start vacuum diffusion connection stove to be heated to 595 ℃ with the speed of 15 ℃/min.In the time that temperature in stove reaches 595 ℃, seaming chuck is declined, the height of decline is H-C, in the present embodiment, 84mm-60mm=24mm, and be incubated 2h under this state.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, obtains required porous Ti-13Nb-13Zr.
Embodiment 7
The present embodiment is the preparation method of the medical porous titanium alloy of a kind of β type.
The starting material of the present embodiment are Ti-13Nb-13Zr titanium net, the beta transformation point T=735 ℃ of Ti-13Nb-13Zr.The mean pore size S=300 μ m of prepared medical porous titanium alloy, porosity P=30%, organization type is bifurcation tissue.Prepared medical porous titanium alloy is cylindrical, diameter D=100mm, height C=30mm.
The detailed process of the present embodiment is:
Step 1: cut-parts.Be that lamellar structure, aperture are 300 μ m by organization type, the Ti-13Nb-13Zr titanium net that porosity is 75% is cut into the Titanium net strip that 25 diameters are 100mm.
Step 2: clean.The Titanium net strip obtaining is soaked to 0.8min in mix acid liquor.The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.Titanium net strip after pickling is adopted to deionized water ultrasonic cleaning 18min.Cleaning is dried after completing.
Step 3: lamination.Adopt electronic balance to weigh respectively the weight of 25 Titanium net strips that obtain in step 2, and count
Calculate the weight in average M=1.88g of every Titanium net strip.Determine the lamination n of Titanium net strip according to formula (2),
n = ρ × ( 1 - P ) × 3.14 × ( D 2 ) 2 × C M × 10 - 3 Formula (2)
In formula, ρ is the density of entity Ti-13Nb-13Zr, ρ=4.51g/cm 3;
P is the porosity of the porous Ti-13Nb-13Zr of required preparation, P=30%;
M is the weight in average of every Titanium net strip, in the present embodiment, and the weight in average=1.88g of every Titanium net strip.
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N=395.Repeating step one cutting Ti-13Nb-13Zr titanium net, makes the sum of the Titanium net strip that cutting obtains equal 395.Repeating step two, cleans obtain 395 Titanium net strips.395 titanium nets after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium alloy.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: vacuum diffusion connects.The blank that obtains medical porous titanium alloy is placed in to the push-down head upper surface that vacuum diffusion connects stove, and seaming chuck is declined, make height H=C × 1.2～1.4 between described seaming chuck lower surface and push-down head upper surface.In the present embodiment, C=30mm, height coefficient gets 1.3, therefore the height H=39mm between seaming chuck lower surface and push-down head upper surface.Vacuum diffusion is connected to stove evacuation to≤10 -3when Pa, start vacuum diffusion connection stove to be heated to 605 ℃ with the speed of 12 ℃/min.In the time that temperature in stove reaches 605 ℃, seaming chuck is declined, the height of decline is H-C, in the present embodiment, 39mm-30mm=9mm, and be incubated 1.5h under this state.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, obtains required porous Ti-13Nb-13Zr.
Embodiment 8
The present embodiment is the preparation method of the medical porous titanium alloy of a kind of β type.
The starting material of the present embodiment are Ti-13Nb-13Zr titanium net, the beta transformation point T=735 ℃ of Ti-13Nb-13Zr.The mean pore size S=200 μ m of prepared medical porous titanium alloy, porosity P=20%, organization type is equiaxed structure.Prepared medical porous titanium alloy is cylindrical, diameter D=50mm, height C=20mm.
The detailed process of the present embodiment is:
Step 1: cut-parts.Be that equiaxed structure, aperture are 200 μ m by organization type, the Ti-13Nb-13Zr titanium net that porosity is 75% is cut into the Titanium net strip that 28 diameters are 100mm.
Step 2: clean.The Titanium net strip obtaining is soaked to 0.5min in mix acid liquor.The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.Titanium net strip after pickling is adopted to deionized water ultrasonic cleaning 16min.Cleaning is dried after completing.
Step 3: lamination.Adopt electronic balance to weigh respectively the weight of 28 Titanium net strips that obtain in step 2, and count
Calculate the weight in average M=0.27g of every Titanium net strip.Determine the lamination n of Titanium net strip according to formula (2),
n = ρ × ( 1 - P ) × 3.14 × ( D 2 ) 2 × C M × 10 - 3 - - - ( 2 )
In formula, ρ is the density of entity Ti-13Nb-13Zr, ρ=4.51g/cm 3;
P is the porosity of the porous Ti-13Nb-13Zr of required preparation, P=20%;
M is the weight in average of every Titanium net strip, in the present embodiment, and the weight in average=0.27g of every Titanium net strip.
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N=524.Repeating step one cutting Ti-13Nb-13Zr titanium net, makes the sum of the Titanium net strip that cutting obtains equal 524.Repeating step two, cleans obtain 524 Titanium net strips.524 titanium nets after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium alloy.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: vacuum diffusion connects.The blank that obtains medical porous titanium alloy is placed in to the push-down head upper surface that vacuum diffusion connects stove, and seaming chuck is declined, make height H=C × 1.2～1.4 between described seaming chuck lower surface and push-down head upper surface.In the present embodiment, C=20mm, height coefficient gets 1.4, therefore the height H=28mm between seaming chuck lower surface and push-down head upper surface.Vacuum diffusion is connected to stove evacuation to≤10 -3when Pa, start vacuum diffusion connection stove to be heated to 610 ℃ with the speed of 14 ℃/min.In the time that temperature in stove reaches 610 ℃, seaming chuck is declined, the height of decline is H-C, in the present embodiment, 28mm-20mm=8mm, and be incubated 1.8h under this state.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, obtains required porous Ti-13Nb-13Zr.
Embodiment 9
The present embodiment is the preparation method of the medical porous titanium alloy of a kind of type alpha+beta.
The starting material of the present embodiment are Ti-6Al-4V titanium net, the beta transformation point T=980 ℃ of Ti-6Al-4V.The mean pore size S=400 μ m of prepared medical porous titanium alloy, porosity P=70%, organization type is basket tissue.Prepared medical porous titanium alloy is cylindrical, diameter D=80mm, height C=100mm.
The detailed process of the present embodiment is:
Step 1: cut-parts.Be that basket tissue, aperture are 400 μ m by organization type, the Ti-6Al-4V titanium net that porosity is 75% is cut into the Titanium net strip that 22 diameters are 80mm.
Step 2: clean.The Titanium net strip obtaining is soaked to 0.6min in mix acid liquor.The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.Titanium net strip after pickling is adopted to deionized water ultrasonic cleaning 16min.Cleaning is dried after completing.
Step 3: lamination.Adopt electronic balance to weigh respectively the weight of 22 Titanium net strips that obtain in step 2, and calculate the weight in average M=1.71g of every Titanium net strip.Determine the lamination n of Titanium net strip according to formula (2),
n = ρ × ( 1 - P ) × 3.14 × ( D 2 ) 2 × C M × 10 - 3 - - - ( 2 )
In formula, ρ is the density of entity Ti-6Al-4V, ρ=4.51g/cm 3;
P is the porosity of the porous Ti-6Al-4V of required preparation, P=70%;
M is the weight in average of every Titanium net strip, in the present embodiment, and the weight in average=1.71g of every Titanium net strip.
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N=398.Repeating step one cutting Ti-6Al-4V titanium net, makes the sum of the Titanium net strip that cutting obtains equal 398.Repeating step two, cleans obtain 398 Titanium net strips.398 titanium nets after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium alloy.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: vacuum diffusion connects.The blank that obtains medical porous titanium alloy is placed in to the push-down head upper surface that vacuum diffusion connects stove, and seaming chuck is declined, make height H=C × 1.2～1.4 between described seaming chuck lower surface and push-down head upper surface.In the present embodiment, C=100mm, height coefficient gets 1.2, therefore the height H=120mm between seaming chuck lower surface and push-down head upper surface.Vacuum diffusion is connected to stove evacuation to≤10 -3when Pa, start vacuum diffusion connection stove to be heated to 840 ℃ with the speed of 15 ℃/min.In the time that temperature in stove reaches 840 ℃, seaming chuck is declined, the height of decline is H-C, in the present embodiment, 120mm-100mm=20mm, and be incubated 2h under this state.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, obtains required porous Ti-6Al-4V.
Embodiment 10
The present embodiment is a kind of preparation method of medical porous titanium.
The starting material of the present embodiment are pure titanium net, the beta transformation point T=885 ℃ of pure titanium.The mean pore size S=700 μ m of prepared medical porous titanium, porosity P=60%, organization type is basket tissue.Prepared medical porous titanium is cylindrical, diameter D=50mm, height C=20mm.
The detailed process of the present embodiment is:
Step 1: cut-parts.Be that basket tissue, aperture are 700 μ m by organization type, the pure titanium net that porosity is 75% is cut into the Titanium net strip that 20 diameters are 50mm.
Step 2: clean.The Titanium net strip obtaining is soaked to 0.5min in mix acid liquor.The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.Titanium net strip after pickling is adopted to deionized water ultrasonic cleaning 15min.Cleaning is dried after completing.
Step 3: lamination.Adopt electronic balance to weigh respectively the weight of 20 Titanium net strips that obtain in step 2, and calculate the weight in average M=1.26g of every Titanium net strip.Determine the lamination n of Titanium net strip according to formula (2),
n = ρ × ( 1 - P ) × 3.14 × ( D 2 ) 2 × C M × 10 - 3 - - - ( 2 )
In formula, ρ is the density of the pure titanium of entity, ρ=4.51g/cm 3;
P is the porosity of the POROUS TITANIUM of required preparation, P=60%;
M is the weight in average of every Titanium net strip, in the present embodiment, and the weight in average=1.26g of every Titanium net strip.
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N=56.The pure titanium net of repeating step one cutting, makes the sum of the Titanium net strip that cutting obtains equal 56.Repeating step two, cleans obtain 56 Titanium net strips.56 titanium nets after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: vacuum diffusion connects.The blank that obtains medical porous titanium is placed in to the push-down head upper surface that vacuum diffusion connects stove, and seaming chuck is declined, make height H=C × 1.2～1.4 between described seaming chuck lower surface and push-down head upper surface.In the present embodiment, C=20mm, height coefficient gets 1.4, therefore the height H=28mm between seaming chuck lower surface and push-down head upper surface.Vacuum diffusion is connected to stove evacuation to≤10 -3when Pa, start vacuum diffusion connection stove to be heated to 745 ℃ with the speed of 10 ℃/min.In the time that temperature in stove reaches 745 ℃, seaming chuck is declined, the height of decline is H-C, in the present embodiment, 28mm-20mm=8mm, and be incubated 2h under this state.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, obtains required POROUS TITANIUM.
Embodiment 11
The present embodiment is a kind of preparation method of medical porous titanium.
The starting material of the present embodiment are pure titanium net, the beta transformation point T=885 ℃ of pure titanium.The mean pore size S=500 μ m of prepared medical porous titanium, porosity P=40%, organization type is lamellar structure.Prepared medical porous titanium is cylindrical, diameter D=20mm, height C=40mm.
The detailed process of the present embodiment is:
Step 1: cut-parts.Be that lamellar structure, aperture are 500 μ m by organization type, the pure titanium net that porosity is 75% is cut into the Titanium net strip that 25 diameters are 20mm.
Step 2: clean.The Titanium net strip obtaining is soaked to 1min in mix acid liquor.The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.Titanium net strip after pickling is adopted to deionized water ultrasonic cleaning 20min.Cleaning is dried after completing.
Step 3: lamination.Adopt electronic balance to weigh respectively the weight of 25 Titanium net strips that obtain in step 2, and calculate the weight in average M=0.14g of every Titanium net strip.Determine the lamination n of Titanium net strip according to formula (2),
n = ρ × ( 1 - P ) × 3.14 × ( D 2 ) 2 × C M × 10 - 3 - - - ( 2 )
In formula, ρ is the density of the pure titanium of entity, ρ=4.51g/cm 3;
P is the porosity of the POROUS TITANIUM of required preparation, P=40%;
M is the weight in average of every Titanium net strip, in the present embodiment, and the weight in average=0.14g of every Titanium net strip.
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N=243.The pure titanium net of repeating step one cutting, makes the sum of the Titanium net strip that cutting obtains equal 243.Repeating step two, cleans obtain 243 Titanium net strips.243 titanium nets after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: vacuum diffusion connects.The blank that obtains medical porous titanium is placed in to the push-down head upper surface that vacuum diffusion connects stove, and seaming chuck is declined, make height H=C × 1.2～1.4 between described seaming chuck lower surface and push-down head upper surface.In the present embodiment, C=40mm, height coefficient gets 1.3, therefore the height H=52mm between seaming chuck lower surface and push-down head upper surface.Vacuum diffusion is connected to stove evacuation to≤10 -3when Pa, start vacuum diffusion connection stove to be heated to 755 ℃ with the speed of 12 ℃/min.In the time that temperature in stove reaches 755 ℃, seaming chuck is declined, the height of decline is H-C, in the present embodiment, 52mm-40mm=12mm, and be incubated 1.5h under this state.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, obtains required POROUS TITANIUM.
Embodiment 12
The present embodiment is a kind of preparation method of medical porous titanium.
The starting material of the present embodiment are pure titanium net, the beta transformation point T=885 ℃ of pure titanium.The mean pore size S=200 μ m of prepared medical porous titanium, porosity P=20%, organization type is bifurcation tissue.Prepared medical porous titanium is cylindrical, diameter D=50mm, height C=25mm.
The detailed process of the present embodiment is:
Step 1: cut-parts.Be that bifurcation tissue, aperture are 200 μ m by organization type, the pure titanium net that porosity is 75% is cut into the Titanium net strip that 28 diameters are 50mm.
Step 2: clean.The Titanium net strip obtaining is soaked to 1min in mix acid liquor.The hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.Titanium net strip after pickling is adopted to deionized water ultrasonic cleaning 20min.Cleaning is dried after completing.
Step 3: lamination.Adopt electronic balance to weigh respectively the weight of 28 Titanium net strips that obtain in step 2, and calculate the weight in average M=0.27g of every Titanium net strip.Determine the lamination n of Titanium net strip according to formula (2),
n = ρ × ( 1 - P ) × 3.14 × ( D 2 ) 2 × C M × 10 - 3 - - - ( 2 )
In formula, ρ is the density of the pure titanium of entity, ρ=4.51g/cm 3;
P is the porosity of the POROUS TITANIUM of required preparation, P=20%;
M is the weight in average of every Titanium net strip, in the present embodiment, and the weight in average=0.27g of every Titanium net strip.
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N=656.The pure titanium net of repeating step one cutting, makes the sum of the Titanium net strip that cutting obtains equal 656.Repeating step two, cleans obtain 656 Titanium net strips.656 titanium nets after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium.In stacking, the grid of each Titanium net strip is overlapped.
Step 4: vacuum diffusion connects.The blank that obtains medical porous titanium is placed in to the push-down head upper surface that vacuum diffusion connects stove, and seaming chuck is declined, make height H=C × 1.2～1.4 between described seaming chuck lower surface and push-down head upper surface.In the present embodiment, C=25mm, height coefficient gets 1.4, therefore the height H=35mm between seaming chuck lower surface and push-down head upper surface.Vacuum diffusion is connected to stove evacuation to≤10 -3when Pa, start vacuum diffusion connection stove to be heated to 750 ℃ with the speed of 15 ℃/min.In the time that temperature in stove reaches 750 ℃, seaming chuck is declined, the height of decline is H-C, in the present embodiment, 35mm-25mm=10mm, and be incubated 1.5h under this state.After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, obtains required POROUS TITANIUM.

Claims (3)

1. a preparation method for medical porous titanium/porous titanium alloy, is characterized in that, detailed process is:
Step 1: cut-parts; Titanium net or titanium alloy reticulated are cut into multi-disc Titanium net strip or titanium mesh; The shape of described Titanium net strip or titanium mesh is consistent with the shape of the medical porous titanium/porous titanium alloy of preparation;
Step 2: clean;
Step 3: lamination; Determine the weight in average M of described multi-disc Titanium net strip or titanium mesh, determine the lamination n of Titanium net strip or titanium mesh according to the weight in average M of Titanium net strip or titanium mesh; The unit of the weight in average M of described multi-disc Titanium net strip or titanium mesh is g;
When described Titanium net strip or titanium mesh are while being square, by formula 1) determine the lamination n of this Titanium net strip or titanium mesh,
n = ρ × ( 1 - P ) × A × B × C M × 10 - 3 - - - 1 )
Formula 1) in, the density of POROUS TITANIUM/porous titanium alloy that ρ is required preparation; P is the porosity of the POROUS TITANIUM/porous titanium alloy of required preparation; M is the weight in average of every Titanium net strip; A × B × C is the length × wide × height of POROUS TITANIUM/porous titanium alloy profile of required preparation; The unit of POROUS TITANIUM/porous titanium alloy physical dimension of required preparation is mm;
When described Titanium net strip or titanium mesh are while being circular, by formula 2) determine the lamination n of this Titanium net strip or titanium mesh,
n = ρ × ( 1 - P ) × 3.14 × ( D 2 ) 2 × C M × 10 - 3 - - - 2 )
Formula 2) in, the density of the porosity of POROUS TITANIUM/porous titanium alloy that ρ is required preparation; P is the porosity of the POROUS TITANIUM/porous titanium alloy of required preparation; M is the weight in average of every Titanium net strip; D is the diameter of the POROUS TITANIUM/porous titanium alloy of required preparation; C is the height of the POROUS TITANIUM/porous titanium alloy of required preparation; The unit of POROUS TITANIUM/porous titanium alloy physical dimension of required preparation is mm;
Lamination n to the Titanium net strip obtaining rounds, and determines that required Titanium net strip counts N;
Repeating step one cutting titanium net or titanium alloy reticulated, makes the sum of Titanium net strip that cutting obtains or titanium mesh equal required Titanium net strip and counts N; Repeating step two, cleans the sheet Titanium net strip obtaining or titanium mesh; Titanium net strip or titanium mesh after cleaning are stacked neatly piecewise, obtain the blank of medical porous titanium alloy; In stacking, the grid of each Titanium net strip is overlapped;
Step 4: the blank that obtains medical porous titanium alloy is placed in to vacuum diffusion and connects between the push-down head and seaming chuck of stove; The height of adjusting seaming chuck, making the vertical height between seaming chuck and push-down head is H=1.2～1.4 × C, the height of POROUS TITANIUM/porous titanium alloy that wherein C is required preparation; The unit of the height C of the POROUS TITANIUM/porous titanium alloy of vertical height H and required preparation is mm;
To vacuum, diffusion connects stove evacuation; When vacuum diffusion connects stove evacuation to≤10 -3when Pa, vacuum diffusion connection stove is heated to T-δ T ℃ with the speed of 10～15 ℃/min, wherein δ T is 120～140 ℃; When temperature arrives T ℃ of T-δ within vacuum diffusion connects stove, by the seaming chuck H-C that declines, and be incubated 1～2h; After insulation finishes, vacuum diffusion connects stove and naturally cools to room temperature, and obtaining aperture S is 200～700 μ m, POROUS TITANIUM/porous titanium alloy that porosity P is 20～70%.
2. the preparation method of medical porous titanium/porous titanium alloy as claimed in claim 1, is characterized in that, the organization type of described titanium net or titanium alloy reticulated is bifurcation tissue or equiaxed structure or lamellar structure or basket tissue.
3. the preparation method of medical porous titanium/porous titanium alloy as claimed in claim 1, it is characterized in that, the hydrofluoric acid that described mix acid liquor is 5% by volume fraction, the nitric acid that volume fraction is 10% and deionized water mix and form, and hydrofluoric acid: nitric acid: the weight ratio of deionized water is 1:3:10.
CN201410020662.5A 2014-01-17 2014-01-17 A kind of preparation method of medical porous titanium/porous titanium alloy Active CN103805797B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410020662.5A CN103805797B (en) 2014-01-17 2014-01-17 A kind of preparation method of medical porous titanium/porous titanium alloy

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410020662.5A CN103805797B (en) 2014-01-17 2014-01-17 A kind of preparation method of medical porous titanium/porous titanium alloy

Publications (2)

Publication Number Publication Date
CN103805797A true CN103805797A (en) 2014-05-21
CN103805797B CN103805797B (en) 2016-02-10

Family

ID=50703178

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410020662.5A Active CN103805797B (en) 2014-01-17 2014-01-17 A kind of preparation method of medical porous titanium/porous titanium alloy

Country Status (1)

Country Link
CN (1) CN103805797B (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106222467A (en) * 2016-07-19 2016-12-14 中南大学 A kind of titanium material with high-orientation stratiform orientation interconnected pore and preparation method thereof
CN108213683A (en) * 2017-12-29 2018-06-29 有研医疗器械（北京）有限公司 A kind of preparation method of porous nickel titanium plate
US20180258512A1 (en) * 2015-09-17 2018-09-13 Nanyang Technological University Titanium-tantalum alloy and method of forming thereof
CN108580902A (en) * 2018-05-02 2018-09-28 东北大学 A kind of electrochemistry adjuvant powders metallurgy prepares POROUS TITANIUM or the method for titanium alloy
CN108714238A (en) * 2018-06-16 2018-10-30 东莞市联洲知识产权运营管理有限公司 A kind of porous based composite dressing for medical use of fibroin/titanium and preparation method thereof of load Anti-radiation Microbes
CN113967746A (en) * 2021-09-30 2022-01-25 长沙理工大学 3D printing method of high-corrosion-resistance high-strength low-elasticity-modulus titanium alloy powder and titanium alloy

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08218103A (en) * 1994-12-12 1996-08-27 Kubota Corp Production of metallic porous body
CN101053672A (en) * 2007-03-22 2007-10-17 上海交通大学 Method for preparing hollow fiber multiporous biological titanium material
CN101967578A (en) * 2010-11-02 2011-02-09 北京科技大学 Preparation method of gradient pore porous high-niobium titanium-aluminum alloy
CN102242288A (en) * 2011-06-20 2011-11-16 烟台工程职业技术学院 Preparation method of porous titanium
CN103060590A (en) * 2013-01-08 2013-04-24 西北工业大学 Preparation method of gradient porous titanium alloy
CN103317225A (en) * 2013-05-28 2013-09-25 西北工业大学 Vacuum diffusion bonding method for TC18 titanium alloys

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08218103A (en) * 1994-12-12 1996-08-27 Kubota Corp Production of metallic porous body
CN101053672A (en) * 2007-03-22 2007-10-17 上海交通大学 Method for preparing hollow fiber multiporous biological titanium material
CN101967578A (en) * 2010-11-02 2011-02-09 北京科技大学 Preparation method of gradient pore porous high-niobium titanium-aluminum alloy
CN102242288A (en) * 2011-06-20 2011-11-16 烟台工程职业技术学院 Preparation method of porous titanium
CN103060590A (en) * 2013-01-08 2013-04-24 西北工业大学 Preparation method of gradient porous titanium alloy
CN103317225A (en) * 2013-05-28 2013-09-25 西北工业大学 Vacuum diffusion bonding method for TC18 titanium alloys

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180258512A1 (en) * 2015-09-17 2018-09-13 Nanyang Technological University Titanium-tantalum alloy and method of forming thereof
CN106222467A (en) * 2016-07-19 2016-12-14 中南大学 A kind of titanium material with high-orientation stratiform orientation interconnected pore and preparation method thereof
CN108213683A (en) * 2017-12-29 2018-06-29 有研医疗器械（北京）有限公司 A kind of preparation method of porous nickel titanium plate
CN108580902A (en) * 2018-05-02 2018-09-28 东北大学 A kind of electrochemistry adjuvant powders metallurgy prepares POROUS TITANIUM or the method for titanium alloy
CN108580902B (en) * 2018-05-02 2019-06-04 东北大学 A kind of method that electrochemistry adjuvant powders metallurgy prepares POROUS TITANIUM or titanium alloy
CN108714238A (en) * 2018-06-16 2018-10-30 东莞市联洲知识产权运营管理有限公司 A kind of porous based composite dressing for medical use of fibroin/titanium and preparation method thereof of load Anti-radiation Microbes
CN113967746A (en) * 2021-09-30 2022-01-25 长沙理工大学 3D printing method of high-corrosion-resistance high-strength low-elasticity-modulus titanium alloy powder and titanium alloy
CN113967746B (en) * 2021-09-30 2024-04-16 长沙理工大学 3D printing method of high-corrosion-resistance high-strength low-elastic modulus titanium alloy powder and titanium alloy

Also Published As

Publication number Publication date
CN103805797B (en) 2016-02-10

Similar Documents

Publication Publication Date Title
CN103805797B (en) A kind of preparation method of medical porous titanium/porous titanium alloy
CN106041084B (en) Three-dimensional lattice material and preparation method thereof based on electron beam selective melting technology
Diao et al. Specific surface areas of porous Cu manufactured by Lost Carbonate Sintering: Measurements by quantitative stereology and cyclic voltammetry
Lee et al. Space-holder effect on designing pore structure and determining mechanical properties in porous titanium
PL2356713T3 (en) Substrate made of a porous metal or metal alloy, its method of production and hte or sofc cells having a support metal comprising this substrate
WO2008099014A8 (en) Porous metal article and method of producing a porous metallic article
CN106148749B (en) One kind has both high intensity and the gradient porous Ti-6Al-4V block materials of high-selenium corn energy and preparation method thereof
EP2424010A4 (en) Method for producing electrode for battery and coating die used in the method
CN106693069A (en) Method for preparing medical porous titanium-tantalum artificial bone and artificial joint, and products thereof
CN103805798A (en) Porous tantalum-niobium alloy and preparation method thereof
WO2006130935A3 (en) TITANIUM, TITANIUM ALLOY AND NiTi FOAMS WITH HIGH DUCTILITY
GB201308792D0 (en) Porous implant material
CN105884390B (en) A kind of regulation and control method of layered porous aluminium oxide ceramics pore structure
CN106801159A (en) A kind of preparation method of nickel foam or foam nickel-base alloy
PL2440688T3 (en) Cathode bottom, method for producing a cathode bottom, and use of the same in an electrolytic cell for producing aluminum
CN105274483B (en) A kind of negative thermal expansion material Sc2W3O12The preparation method of film
CN101292837B (en) Method for determining optimum cooking and boiling power of electric cooker
CN104999085B (en) Preparation method of nanosheet layer phase reinforced TiNi-based alloy composite plate
CN110735093A (en) porous titanium-based metal glass biomedical material and preparation method thereof
CN106734715A (en) 904L+Q345R pressure container of composite board end socket thermoforming process
CN103862049A (en) Ni-Ti porous material mini-sized part and sintering method thereof
CN108213683A (en) A kind of preparation method of porous nickel titanium plate
CN114472919A (en) Forming process of porous metal thin net structure
CN107397422B (en) Preparation method of double-layer soaking pot
CN102475902B (en) Preparation method of medical porous metal implant material

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant