CN109550077A - A kind of preparation method of medical Ti 6Al4V artificial implantation - Google Patents
A kind of preparation method of medical Ti 6Al4V artificial implantation Download PDFInfo
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- CN109550077A CN109550077A CN201811294899.7A CN201811294899A CN109550077A CN 109550077 A CN109550077 A CN 109550077A CN 201811294899 A CN201811294899 A CN 201811294899A CN 109550077 A CN109550077 A CN 109550077A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y80/00—Products made by additive manufacturing
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/24—Materials or treatment for tissue regeneration for joint reconstruction
Abstract
The present invention relates to a kind of preparation methods of medical Ti 6Al4V artificial implantation, comprising: using Ti6Al4 alloy powder as raw material, the raw material is prepared into the Ti6Al4V alloy of block by electron beam melting sedimentation；The Ti6Al4V alloy of block is heat-treated later, obtains the implantation material.Tensile strength of the invention reaches 960~990MPa, and yield strength reaches 940~970MPa, and elasticity modulus is 30~40GPa, close to human body bone modulus, reduces stress shielding and stress shielding.
Description
Technical field
The invention belongs to medical titanium alloy material increasing fields, specifically, being related to a kind of electron beam melting deposition doctor
With the preparation method of Ti6Al4V artificial implantation.
Background technique
With the rapid development of our national economy, prosthetic replacement's amount for surgical increases year by year.And China is made at present
Titanium alloy artificial joint is generally processed through numerically-controlled machine tool by forging titanium alloy and is obtained.This tradition subtracts the people of material method manufacture
Work joint, elasticity modulus is generally in 100~110GPa, and the bone modulus of human body is generally 10~30GPa, is easy after being implanted into human body
Stress shielding and stress shielding are caused, big skelagia and bone resorption are caused.Meanwhile traditional titanium alloy artificial for subtracting the manufacture of material method closes
Section can not be exactly matched with ossis, to generate fretting wear, eventually lead to material failure.If wanting further satisfaction patient
Individual demand exactly matches joint prosthesis and ossis, it is necessary to carry out personalized designs, but tradition according to patient bone pulp cavity
Individuation handle rely on cnc machine tool technology, to Machining Free-Form Surfaces do not have outstanding advantage.And to reduce material
Elasticity modulus to reduce stress shielding and stress shielding, there are two types of conventional methods: (1) use reticular structure；(2) building is new
Alloy system.But the fatigue life of first method material is unable to get guarantee.Second method can introduce new alloy member
Element, it is possible to cytotoxicity can be generated.And the increase with the country to joint prosthesis demand, and " made in China 2025 " to height
The requirement of performance medical instrument, more stringent requirements are proposed for manufacture and processing to joint prosthesis.
Summary of the invention
The present invention In view of the above shortcomings of the prior art, proposes a kind of system of medical Ti 6Al4V artificial implantation
Preparation Method, this method are formed using electron beam melting sedimentation, are cooperated Post isothermal treatment, can be made TTi6Al4V alloy tensile strength
Reach 960~990MPa, yield strength reaches 940~970MPa, while modulus being made to drop to 35~40GPa, close to human body
Bone modulus reduces stress shielding and stress shielding.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of medical Ti 6Al4V artificial implantation, which comprises
Using Ti6Al4 alloy powder as raw material, the raw material is prepared into block by electron beam melting sedimentation
Ti6Al4V alloy；
The Ti6Al4V alloy of block is heat-treated, the implantation material is obtained.
Optionally, the Ti6Al4V alloy of block is heat-treated, in which: by the Ti6Al4V alloy of block
It is put into quartz glass tube and vacuumizes or seal, or used in heat-treatment furnace using Ti6Al4V alloy described in inert gas shielding
In preventing from being oxidized under titanium alloy high-temperature.
Optionally, the Ti6Al4V alloy of block is heat-treated, is referred to: by sectional heating method, first by temperature from
Room temperature is increased to 450~650 DEG C, is kept the temperature, and then raises the temperature to 900~1300 DEG C again, is kept the temperature, then empty
It is cold.
Further, the preparation method is according to performed below:
S1: it using Ti6Al4V alloy powder as raw material, is prepared described in block by electron beam melting sedimentation
Ti6Al4V alloy；
S2: the Ti6Al4V alloy of the block of preparation is put into quartz glass tube and is vacuumized or sealed shape
At sample；
S3: the sample being put into heat-treatment furnace and is heated, using sectional heating method, 450 are increased to from room temperature first~
650 DEG C, 5~20 minutes are kept the temperature later, then temperature is increased to 900~1300 DEG C again, heating rate is 5~15 DEG C/min,
0.5~3 hour is kept the temperature later, it is then air-cooled, obtain the implantation material.
Optionally, the electron beam melting sedimentation prepares the Ti6Al4V alloy of block, in which: the electron beam
Power is 80~120kW/cm2, and for powdering with a thickness of 30~70 μm, scanning speed is 900~1200mm/sec, in printer housing
Temperature is maintained at 650~750 DEG C.
Optionally, the Ti6Al4V alloy powder is made of the element of following weight percentage: Al be 5.5~
6.8%, V are that 3.5~4.5%, Fe is less than less than 0.05%, H less than 0.015%, O less than 0.3%, C less than 0.1%, N
0.2%, remaining is titanium.Further, be made of the element of following weight percents: Al is that 6~6.8%, V is 4~4.5%,
Fe is less than 0.2% less than 0.013%, O less than 0.007%, H less than 0.02%, N less than 0.2%, C, remaining is titanium.
Optionally, the tensile strength for the implantation material being prepared is 960~990MPa, and yield strength is 940~970MPa.
Optionally, the elasticity modulus for the implantation material being prepared is 30~40GPa.
Optionally, the hardness for the implantation material being prepared is 370~400HV, much higher than general forging and cast titanium alloy.
Compared with prior art, the present invention has the following beneficial effects:
1, the tensile strength for the implantation material that the above method of the present invention is prepared reaches 960~990MPa, and yield strength reaches
To 940~970MPa, it is much higher than medical titanium alloy standard；Hardness reaches 370~400HV, and it is hard to be higher than medical titanium alloy at this stage
It spends (about 330~350HV)；
2, the elasticity modulus of implantation material of the invention after Overheating Treatment is 30~40GPa, and existing titanium alloy artificial closes
Section modulus is 100~110GPa；
3, it by heat treatment regulation modulus, does not need to reduce modulus by complicated structure design, while improving component
Structural stability and reliability；
4, the biological reliability of Ti6Al4V has been subjected to market and examines for a long time, is to have obtained food and medicine Surveillance Authority batch
Quasi- medical titanium alloy, the present invention can rapidly enter clinical test by above-mentioned alloying component, while reduce rare earth element
Usage amount, economize on resources, protect environment.
5, in the above method of the present invention, the three dimensional design of joint prosthesis can be realized based on CT data, and pass through 3D printing
Technology prepares individuation joint prosthesis, so as to make implantation material and ossis reach perfect matching, reduces fretting wear.And
And by heat treatment process the modulus of material is significantly reduced, close to human body bone modulus, reduces stress shielding and stress hides
Gear.
Specific embodiment
This bright feature and other correlated characteristics are described in further detail by embodiment, in order to technology people of the same trade
The understanding of member；But the invention is not limited in any way, it is noted that those skilled in the art,
Under the premise of not departing from present inventive concept, various modifications and improvements can be made, and these are all within the scope of protection of the present invention.
Embodiment 1:
The Arcam A2XX3D printer that xuanAcram company can be used in the present embodiment carries out electron beam melting sedimentation
It is prepared into the Ti6Al4V alloy of block, prepares block Ti6Al4V alloy by raw material of Arcam Ti6Al4V powder P1034,
Middle Ti6Al4V alloy powder ingredient are as follows: aluminium Al5.6%, vanadium V 3.6%, iron Fe0.2%, carbon C 0.01%, nitrogen N 0.006%,
Hydrogen H0.012%, oxygen O 0.19%, remaining is titanium.The printing technology parameter of use are as follows: beam power 90kW/cm2, powdering
With a thickness of 40 μm, scanning speed 950mm/sec, the temperature in chassis of printer is maintained at 650 DEG C in whole process.It will preparation
The Ti6Al4V alloy of good block is put into quartz glass tube and vacuumizes sealing as sample.Then sample is put into hot place
It is heated in reason furnace, temperature is increased to 500 DEG C from room temperature first, keeps the temperature 10 minutes, then raises the temperature to 1000 DEG C again, heating
Speed is 10 DEG C/min, keeps the temperature 1 hour, then air-cooled.Tensile sample, tensile sample surface warp are prepared using wire cutting mode
The polishing of 800# sand paper.
After tested, implant material tensile strength manufactured in the present embodiment is 983.3 ± 12.7MPa, and yield strength reaches
967.8 ± 13.4MPa, elasticity modulus are 36.7 ± 2.3GPa, and hardness reaches 380.5 ± 7.8HV.
The present embodiment realizes the three dimensional design of joint prosthesis based on CT data, and prepares individuation people by 3D printing technique
Work joint reduces fretting wear so as to make implantation material and ossis reach perfect matching.And pass through heat treatment process
So that the modulus of material significantly reduces, close to human body bone modulus, reduce stress shielding and stress shielding.In addition, using this reality
The titanium alloy member of example preparation is applied, vickers microhardness is much higher than general forging and cast titanium alloy (about 330~350HV), material
The wearability of material is greatly improved, and reduces the abrasion generated when metal artificial's joint ball head and acetabular bone friction.
Embodiment 2:
The Arcam A2XX3D printer that Acram company can be used in the present embodiment carries out the preparation of electron beam melting sedimentation
At the Ti6Al4V alloy of block, block Ti6Al4V alloy is prepared by raw material of Arcam Ti6Al4V powder P1034, wherein
Ti6Al4V alloy powder ingredient are as follows: aluminium Al 6.26%, vanadium V 4.18%, iron Fe0.2%, carbon C0.01%, nitrogen N 0.006%,
Hydrogen H0.012%, oxygen O 0.13%, remaining is titanium.The printing technology parameter of use are as follows: beam power 100kW/cm2, paving
Powder is with a thickness of 50 μm, scanning speed 1000mm/sec, and the temperature in chassis of printer is maintained at 700 DEG C in whole process.It will
The block Ti6Al4V alloy prepared is put into quartz glass tube and vacuumizes sealing.Then sample is put into heat-treatment furnace
Heating, first temperature are increased to 550 DEG C from room temperature, keep the temperature 5 minutes, then raise the temperature to 1100 DEG C again, heating rate is
15 DEG C/min, 1.5 hours are kept the temperature, it is then air-cooled.Then tensile sample, tensile sample surface warp are prepared using wire cutting mode
The polishing of 800# sand paper.
After tested, the implant material tensile strength that the present embodiment states preparation is 974.9 ± 4.1MPa, and yield strength reaches
945.3 ± 17.8MPa, elasticity modulus are 38 ± 0.5GPa, and hardness reaches 386.1 ± 11.2HV.
The present embodiment realizes the three dimensional design of joint prosthesis based on CT data, and prepares individuation people by 3D printing technique
Work joint reduces fretting wear so as to make implantation material and ossis reach perfect matching.And pass through heat treatment process
So that the modulus of material significantly reduces, close to human body bone modulus, reduce stress shielding and stress shielding.In addition, using this reality
The titanium alloy member of example preparation is applied, vickers microhardness is much higher than general forging and cast titanium alloy (about 330~350HV), material
The wearability of material is greatly improved, and reduces the abrasion generated when metal artificial's joint ball head and acetabular bone friction.
Embodiment 3:
The Arcam A2XX3D printer that Acram company can be used in the present embodiment carries out the preparation of electron beam melting sedimentation
At the Ti6Al4V alloy of block, block Ti6Al4V alloy is prepared by raw material of Arcam Ti6Al4V powder P1034, wherein
Ti6Al4V alloy powder ingredient are as follows: aluminium Al 6.5%, vanadium V 4%, iron Fe0.1%, carbon C0.01%, nitrogen N 0.006%, hydrogen
H0.012%, oxygen O 0.16%, remaining is titanium.The printing technology parameter of use are as follows: beam power 110kW/cm2, powdering
With a thickness of 60 μm, scanning speed 1100mm/sec, the temperature in chassis of printer is maintained at 725 DEG C in whole process.It will system
The block Ti6Al4V alloy got ready is put into heat-treatment furnace, and is protected using argon gas.Block Ti6Al4V alloy is heated,
Temperature is increased to 650 DEG C from room temperature first, keeps the temperature 15 minutes, then raises the temperature to 1200 DEG C again, and heating rate is 15 DEG C/
Min keeps the temperature 2 hours, then air-cooled.Then tensile sample is prepared using wire cutting mode, tensile sample surface is through 800# sand paper
Polishing.
After tested, the tensile strength of implant material manufactured in the present embodiment is 970.1 ± 15.2MPa, and yield strength reaches
To 947.3 ± 5.6MPa, elasticity modulus is 35.8 ± 1.5GPa, and hardness reaches 386.1 ± 11.2HV.
The present embodiment realizes the three dimensional design of joint prosthesis based on CT data, and prepares individuation people by 3D printing technique
Work joint reduces fretting wear so as to make implantation material and ossis reach perfect matching.And pass through heat treatment process
So that the modulus of material significantly reduces, close to human body bone modulus, reduce stress shielding and stress shielding.In addition, using this reality
The titanium alloy member of example preparation is applied, vickers microhardness is much higher than general forging and cast titanium alloy (about 330~350HV), material
The wearability of material is greatly improved, and reduces the abrasion generated when metal artificial's joint ball head and acetabular bone friction.
The selection of the parameter selection of above-described embodiment and specific component is not uniquely, in other embodiments, originally
Field technical staff can also select other parameters and specific component according to actual application.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or modify within the scope of the claims, this not shadow
Ring substantive content of the invention.In the absence of conflict, the feature in embodiments herein and embodiment can any phase
Mutually combination.
Claims (10)
1. a kind of preparation method of medical Ti 6Al4V artificial implantation, it is characterised in that: include:
Using Ti6Al4V alloy powder as raw material, the raw material is prepared into block by electron beam melting sedimentation
Ti6Al4V alloy；
The Ti6Al4V alloy of block is heat-treated, the implantation material is obtained.
2. a kind of preparation method of medical Ti 6Al4V artificial implantation according to claim 1, it is characterised in that: described
The Ti6Al4V alloy of block is heat-treated, in which: the Ti6Al4V alloy of block is put into quartz glass tube
In vacuumize or seal, or using Ti6Al4V alloy described in inert gas shielding in heat-treatment furnace, for preventing titanium alloy height
It is oxidized under temperature.
3. a kind of preparation method of medical Ti 6Al4V artificial implantation according to claim 1, it is characterised in that: to institute
The Ti6Al4V alloy for stating block is heat-treated, wherein heat treatment uses sectional heating method: first by temperature from room temperature liter
It up to 450~600 DEG C, is kept the temperature, then raises the temperature to 900~1300 DEG C again, kept the temperature, it is then air-cooled.
4. a kind of preparation method of medical Ti 6Al4V artificial implantation according to claim 1, it is characterised in that: by with
Lower execution:
S1: it using Ti6Al4V alloy powder as raw material, is closed by the Ti6Al4V that electron beam melting sedimentation prepares block
Gold；
S2: it is put into quartz glass tube and is vacuumized or sealed the Ti6Al4V alloy of the block of preparation to form examination
Sample；
S3: the sample being put into heat-treatment furnace and is heated, and using sectional heating method, is increased to 450~650 from room temperature first
DEG C, 5~20 minutes are kept the temperature, then raises the temperature to 900~1300 DEG C, heating rate is 5~15 DEG C/min, heat preservation 0.5~3
Hour, it is then air-cooled, obtain the implantation material.
5. a kind of preparation method of medical Ti 6Al4V artificial implantation according to claim 4, it is characterised in that: described
The Ti6Al4V alloy of block is prepared by electron beam melting sedimentation, in which: the beam power is 80~120kW/
cm2, for powdering with a thickness of 30~70 μm, scanning speed is 900~1200mm/sec, in printer housing temperature be maintained at 650~
750℃。
6. a kind of preparation method of medical Ti 6Al4V artificial implantation according to claim 1-5, feature exist
In: the Ti6Al4V alloy powder is made of the element of following weight percentage: Al be 5.5~6.8%, V be 3.5~
4.5%, Fe are less than 0.2% less than 0.015%, O less than 0.05%, H less than 0.1%, N less than 0.3%, C, remaining is titanium.
7. a kind of preparation method of medical Ti 6Al4V artificial implantation according to claim 6, it is characterised in that: described
Ti6Al4V alloy powder is made of the element of following weight percents: Al is that 6~6.8%, V is that 4~4.5%, Fe is less than
0.2%, C are less than 0.2% less than 0.013%, O less than 0.007%, H less than 0.02%, N, remaining is titanium.
8. a kind of preparation method of medical Ti 6Al4V artificial implantation according to claim 1-5, feature exist
In: the tensile strength for the implantation material being prepared is 960~990MPa, and yield strength is 940~970MPa.
9. a kind of preparation method of medical Ti 6Al4V artificial implantation according to claim 1-5, feature exist
In: the elasticity modulus for the implantation material being prepared is 30~40GPa.
10. a kind of preparation method of medical Ti 6Al4V artificial implantation according to claim 1-5, feature
Be: the hardness for the implantation material being prepared is 370~400HV.
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