CN106670464B - A kind of doubly-linked leads to the preparation method of reticular structure titanium-magnesium double metallic composite material - Google Patents
A kind of doubly-linked leads to the preparation method of reticular structure titanium-magnesium double metallic composite material Download PDFInfo
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- CN106670464B CN106670464B CN201710023783.9A CN201710023783A CN106670464B CN 106670464 B CN106670464 B CN 106670464B CN 201710023783 A CN201710023783 A CN 201710023783A CN 106670464 B CN106670464 B CN 106670464B
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- 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
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- 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
- B22F3/24—After-treatment of workpieces or articles
- B22F3/26—Impregnating
Abstract
A kind of doubly-linked leads to the preparation method of reticular structure titanium-magnesium double metallic composite material.The present invention relates to the preparation methods that a kind of doubly-linked leads to reticular structure titanium-magnesium double metallic composite material.The present invention is to solve the problems, such as that the elasticity modulus such as traditional biological medical metal material such as stainless steel, titanium alloy are high and cause " stress shielding ", bioactivity poor.Method: will have compared with after low elastic modulus and the fusing of the magnesium alloy of good osteogenic induction performance, penetrated into the POROUS TITANIUM of low elastic modulus using the method for infiltration, the cooling doubly-linked that is prepared into leads to reticular structure titanium-magnesium double metallic composite material.The present invention is used to prepare doubly-linked and leads to reticular structure titanium-magnesium double metallic composite material.
Description
Technical field
The present invention relates to the preparation methods that a kind of doubly-linked leads to reticular structure titanium-magnesium double metallic composite material.
Background technique
As biomaterial, titanium or titanium alloy is with the lower closer people's bone of its density, intensity is high, biocompatibility preferably with
And the advantages that good corrosion resistance, it is widely used in terms of bio-medical and there is vast potential for future development.However titanium
And higher (the TC4 titanium alloy: 110GPa of the elasticity modulus of titanium alloy；Pure titanium: 108GPa), it is far longer than the elasticity modulus of people's bone
(3.5~20GPa), this can cause " stress shielding effect ", so that the bone tissue around implant cannot get stress thorn appropriate
Swash and generate osteoporosis, implant fall off even autologous bone fracture etc. serious consequences.Current most effective reduction titanium and titanium close
The method of golden elasticity modulus be introduce porous structure, but the introducing of porous structure simultaneously can bring mechanical property be greatly reduced and
Mechanical property it is unstable, limit use scope and active time of the POROUS TITANIUM as implantation material.In addition, titanium is biologically inert
Material, although having good Integrated implant, its osteoinductive is poor, cannot promote the growth of bone tissue.
Magnesium alloy is also a kind of biomaterial with broad development space, and it is most to connect that elasticity modulus, which is 41~45GPa,
The metal material of person of modern times's flexible bone modulus.And magnesium is one of human body macroelement, is the indispensable element of bone uptake.Magnesium alloy
On the one hand degradability can make magnesium alloy that can voluntarily degrade after being implanted into human body, take out without second operation；Separately
On the one hand, the ion generated after magnesium alloy degradation is also beneficial to bone growth, while the degradation of magnesium also provides growth for tissue
Space, reinforce implantation material and bone tissue combination.However the corrosion resistance of magnesium is poor, in physiological electrolyte environment, contains
There is a large amount of erosion carbon dioxide, the corrosion degradation of magnesium alloy can be substantially speeded up.After the implantation, degradation speed is too fast for magnesium alloy,
It just fails before organization healing, loses and effect is fixed and supported to affected part.Too fast degradation has become magnesium alloy in human body
To limit the greatest problem that it is applied in biology and medical field.
Summary of the invention
The present invention is caused to solve the elasticity modulus such as traditional biological medical metal material such as stainless steel, titanium alloy height
The problem of " stress shielding ", bioactivity difference, and a kind of preparation of logical reticular structure titanium-magnesium double metallic composite material of doubly-linked is provided
Method.
The preparation method that a kind of doubly-linked of the present invention leads to reticular structure titanium-magnesium double metallic composite material sequentially includes the following steps:
One, cold pressing pine dress titanium valve medium temperature is pre-sintered: titanium valve being fitted into mold, the pressure for applying 8MPa~12MPa makes titanium
After powder compacting, the titanium valve of compacting is put into togerther in the closed container vacuumized together with mold and carries out vacuum-sintering, by sintering temperature
Degree is cold from room temperature to after 800 DEG C~1000 DEG C, keeping the temperature 0.5h~1.5h under conditions of temperature is 800 DEG C~1000 DEG C
But room temperature is arrived, POROUS TITANIUM pre-sintered body is obtained；
Two, POROUS TITANIUM pre-sintered body roughing: POROUS TITANIUM pre-sintered body roughing is become by the means of machining
Shape and size needed for device blank, the size for reserving later period POROUS TITANIUM pre-sintered body volume contraction and being finished
Surplus obtains part to be sintered；
Three, high temperature is finally sintered: part to be sintered is put into clean closed container and carries out vacuum high-temperature sintering, sintering temperature
Degree is 1100 DEG C~1500 DEG C, and sintering time is 2h~5h, obtains POROUS TITANIUM precast body；The compression of the POROUS TITANIUM precast body is strong
Degree is 100MPa~300MPa；
Four, magnesium alloy infiltrates: magnesium alloy being molten into liquid magnesium alloy under the protection of protection gas, is then being higher than magnesium alloy
After keeping the temperature 0.5h~1h under conditions of 50 DEG C~80 DEG C of fusing point, it is impregnated into POROUS TITANIUM prefabricated component, air-cooled or water cooling to room temperature obtains
Lead to reticular structure titanium-magnesium double metallic composite material to doubly-linked.
Beneficial effects of the present invention:
The present invention will have compared with after low elastic modulus and the fusing of the magnesium alloy of good osteogenic induction performance, utilize infiltration
Method is penetrated into the POROUS TITANIUM of low elastic modulus, and the cooling doubly-linked that is prepared into leads to reticular structure titanium-magnesium double metallic composite material.One side
Face substantially reduces the elasticity modulus of material, solves conventional metals biomaterial and asks because of " stress shielding " that elasticity modulus height generates
Topic；On the other hand, degrade in the human body magnesium ion of generation of the magnesium alloy in material can promote bone uptake, have material excellent
Different osteogenic induction performance, while the hole that magnesium alloy degradation leaves makes for the intracorporal nutrient transport of people and tissue growth
Material has excellent osseointegration character.To reach the mechanical property, biocompatibility, osteoinductive and the skeletonization that collect excellent
The integrated new bio medical composite material of conformability.
Reticular structure titanium-magnesium double metallic composite material prepared by the present invention is compared with traditional biological medical metal material, tool
Have following advantage: (1) elasticity modulus is low and controllable, solves the problems, such as " stress shielding "；(2) such as Ni, Al, Cr, Co are free of
Etc. cytotoxicities element；(3) it is provided simultaneously with Integrated implant and osteoinductive, is firmly combined after implanting with bone tissue；(4)
The magnesium alloy and POROUS TITANIUM that different performance can be selected according to different service demands carry out performance tune to the performance of composite material
Control, it is easier to for individual personalized designs.
Detailed description of the invention
Fig. 1 is the metallograph that doubly-linked leads to reticular structure titanium-magnesium double metallic composite material；
Fig. 2 is the scanning electron microscope (SEM) photograph that doubly-linked leads to reticular structure titanium-magnesium double metallic composite material.
Specific embodiment
Specific embodiment 1: a kind of doubly-linked of present embodiment leads to the system of reticular structure titanium-magnesium double metallic composite material
Preparation Method sequentially includes the following steps:
One, cold pressing pine dress titanium valve medium temperature is pre-sintered: titanium valve being fitted into mold, the pressure for applying 8MPa~12MPa makes titanium
After powder compacting, the titanium valve of compacting is put into togerther in the closed container vacuumized together with mold and carries out vacuum-sintering, by sintering temperature
Degree is cold from room temperature to after 800 DEG C~1000 DEG C, keeping the temperature 0.5h~1.5h under conditions of temperature is 800 DEG C~1000 DEG C
But room temperature is arrived, POROUS TITANIUM pre-sintered body is obtained；
Two, POROUS TITANIUM pre-sintered body roughing: POROUS TITANIUM pre-sintered body roughing is become by the means of machining
Shape and size needed for device blank, the size for reserving later period POROUS TITANIUM pre-sintered body volume contraction and being finished
Surplus obtains part to be sintered；
Three, high temperature is finally sintered: part to be sintered is put into clean closed container and carries out vacuum high-temperature sintering, sintering temperature
Degree is 1100 DEG C~1500 DEG C, and sintering time is 2h~5h, obtains POROUS TITANIUM precast body；The compression of the POROUS TITANIUM precast body is strong
Degree is 100MPa~300MPa；
Four, magnesium alloy infiltrates: magnesium alloy being molten into liquid magnesium alloy under the protection of protection gas, is then being higher than magnesium alloy
After keeping the temperature 0.5h~1h under conditions of 50 DEG C~80 DEG C of fusing point, it is impregnated into POROUS TITANIUM prefabricated component, air-cooled or water cooling to room temperature obtains
Lead to reticular structure titanium-magnesium double metallic composite material to doubly-linked.
Combination in the POROUS TITANIUM for the POROUS TITANIUM pre-sintered body that present embodiment step 1 obtains between titanium particle is weaker, machine
Processing is easier to, and will not form closed pore because of processing in process.On the one hand processing cost, another party are reduced
Face ensures the infiltration quality in later period.
Bond strength between POROUS TITANIUM precast body titanium valve obtained in present embodiment step 3 is high, the compression of POROUS TITANIUM
Intensity can achieve 100~300MPa, have reached the intensity requirement in the carrying of human body bone.
Netted titanium-magnesium double metallic composite material that present embodiment obtains utilizes the magnesium with excellent osteogenic induction performance
Porous structure in alloy fill POROUS TITANIUM compensates for POROUS TITANIUM unstable mechanical property and osteogenic induction performance is insufficient lacks
It falls into.
Heat preservation is carried out in present embodiment step 4 can allow liquid magnesium alloy temperature uniform, and mobility is preferable, more favorably
In infiltration.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: titanium valve described in step 1 is
Pure titanium, Ti-Nb alloy or Ti-Mo alloy.Other steps and parameter are same as the specific embodiment one.
Present embodiment can choose different-grain diameter titanium valve of different shapes, can obtain the porous of different aperture feature
Titanium, so as to be regulated and controled according to different service demands to its mechanical property.Titanium valve ingredient can choose pure titanium valve and
Titanium Powder without the alloying element that is harmful to the human body such as Ti-Nb, Ti-Mo alloyed powder.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: titanium described in step 1
The partial size of powder is 180 μm~220 μm.Other steps and parameter are the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: being applied in step 1
Adding the pressure of 10MPa comes into full contact with titanium valve.Other steps and parameter are identical as one of specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: will in step 1
Sintering temperature is from room temperature to 900 DEG C.Other steps and parameter are identical as one of specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: in step 1
Temperature keeps the temperature 1h under conditions of being 900 DEG C.Other steps and parameter are identical as one of specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: being burnt in step 3
Junction temperature is 1200 DEG C.Other steps and parameter are identical as one of specific embodiment one to six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: institute in step 4
Stating magnesium alloy is Mg-Zn alloy, Mg-Ca alloy or Mg-Zn-Ca alloy.Other steps and parameter and specific embodiment one to
One of seven is identical.
Present embodiment selects corrosion resistance and mechanical property preferable, and the Mg- without the alloying element that is harmful to the human body
Zn alloy, Mg-Ca alloy or Mg-Zn-Ca alloy etc. can be carried out by alloying component of the different service demands to magnesium alloy
Adjustment, to control mechanical property, biological property and the corrosion rate of magnesium alloy.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: institute in step 4
The mode for stating infiltration is ultrasonic wave auxiliary infiltration.Other steps and parameter are identical as one of specific embodiment one to eight.
Beneficial effects of the present invention are verified with following embodiment:
Embodiment one: a kind of doubly-linked lead to the preparation method of reticular structure titanium-magnesium double metallic composite material according to the following steps into
Row:
One, cold pressing pine dress titanium valve medium temperature is pre-sintered: the pure titanium valve of spherical shape that partial size is 180 μm~220 μm is fitted into mold,
Apply 10MPa pressure make titanium valve be compacted after, by the titanium valve of compacting together with mold be put into togerther in the closed container vacuumized into
Row pressureless sintering, sintering temperature keep the temperature 1h under conditions of temperature is 900 DEG C, are cooled to room from room temperature to after 900 DEG C
Temperature obtains POROUS TITANIUM pre-sintered body；
Two, POROUS TITANIUM pre-sintered body roughing: POROUS TITANIUM pre-sintered body roughing is become by the means of machining
Shape and size needed for device blank, the size for reserving later period POROUS TITANIUM pre-sintered body volume contraction and being finished
Surplus obtains part to be sintered；
Three, high temperature is finally sintered: part to be sintered is put into clean closed container and carries out vacuum high-temperature sintering, sintering temperature
Degree is 1200 DEG C, and sintering time 3h obtains POROUS TITANIUM precast body；The compressive strength of the POROUS TITANIUM precast body be 100MPa~
300MPa；
Four, magnesium alloy infiltrates: Mg-Zn-Ca alloy being molten into liquid magnesium alloy under the protection of protection gas, is then being higher than
Under conditions of 50 DEG C~80 DEG C of magnesium alloy fusing point, ultrasonic wave auxiliary is impregnated into POROUS TITANIUM prefabricated component, air-cooled or water cooling to room temperature,
It obtains doubly-linked and leads to reticular structure titanium-magnesium double metallic composite material.
The elasticity modulus that obtained doubly-linked leads to reticular structure titanium-magnesium double metallic composite material is 16.6GPa, and compression strength is
268MPa impregnates 10 days in simulated body fluid, and mass loss is about 0.9%.Not only carrying demand in human body can have been met, but also can
To eliminate " stress shielding " effect because caused by elasticity modulus is excessively high.
Embodiment two: the present embodiment and embodiment one the difference is that: by partial size be 180 μm~220 μ in step 1
The pure titanium valve of isometric irregular shape of m is fitted into mold.Other are the same as example 1.
Embodiment three: the present embodiment and embodiment one the difference is that: by partial size be 180 μm~220 μ in step 1
The spherical Ti-Nb system alloyed powder of m is fitted into mold.Other are the same as example 1.
Example IV: the present embodiment and embodiment one the difference is that: by partial size be 180 μm~220 μ in step 1
The spherical Ti-Mo system alloyed powder of m is fitted into mold.Other are the same as example 1.
Embodiment five: the present embodiment and embodiment one the difference is that: Mg-Ca alloyed powder is being protected in step 4
Liquid magnesium alloy is molten under the protection of gas.Other are the same as example 1.
Embodiment six: the present embodiment and embodiment one the difference is that: Mg-Zn alloyed powder is being protected in step 4
Liquid magnesium alloy is molten under the protection of gas.Other are the same as example 1.
Claims (1)
1. the preparation method that a kind of doubly-linked leads to reticular structure titanium-magnesium double metallic composite material, it is characterised in that doubly-linked leads to netted knot
Structure titanium-magnesium double metallic composite material preparation method sequentially includes the following steps:
One, cold pressing pine dress titanium valve medium temperature is pre-sintered: the pure titanium valve of spherical shape that partial size is 180 μm~220 μm being fitted into mold, is applied
After the pressure of 10MPa is compacted titanium valve, the titanium valve of compacting is put into togerther in the closed container vacuumized together with mold and carries out nothing
Pressure sintering, sintering temperature keep the temperature 1h under conditions of temperature is 900 DEG C, are cooled to room temperature, obtain from room temperature to after 900 DEG C
To POROUS TITANIUM pre-sintered body；
Two, POROUS TITANIUM pre-sintered body roughing POROUS TITANIUM pre-sintered body roughing: is become into device by the means of machining
Shape and size needed for blank reserve more than later period POROUS TITANIUM pre-sintered body volume contraction and the size finished
Amount, obtains part to be sintered；
Three, high temperature is finally sintered: part to be sintered being put into clean closed container and carries out vacuum high-temperature sintering, sintering temperature is
1200 DEG C, sintering time 3h obtains POROUS TITANIUM precast body；The compressive strength of the POROUS TITANIUM precast body be 100MPa~
300MPa；
Four, magnesium alloy infiltrates: Mg-Zn-Ca alloy being molten into liquid magnesium alloy under the protection of protection gas, is then being higher than magnesium conjunction
Under conditions of 50 DEG C~80 DEG C of golden fusing point, ultrasonic wave auxiliary is impregnated into POROUS TITANIUM prefabricated component, and air-cooled or water cooling to room temperature obtains
Doubly-linked leads to reticular structure titanium-magnesium double metallic composite material；Obtained doubly-linked leads to the bullet of reticular structure titanium-magnesium double metallic composite material
Property modulus be 16.6GPa, compression strength 268MPa, impregnated 10 days in simulated body fluid, mass loss is about 0.9%.
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| CN110918998B (en) * | 2019-11-24 | 2022-02-11 | 桂林理工大学 | High-damping 5083Al/Ti composite material and preparation method thereof |
| CN111266592B (en) * | 2020-03-25 | 2022-04-22 | 燕山大学 | Titanium-magnesium composite material with double-communication structure and preparation method and application thereof |
| CN111250703B (en) * | 2020-05-06 | 2020-08-14 | 季华实验室 | Magnesium-based composite material taking titanium or titanium alloy as framework reinforcement and preparation method thereof |
| CN113172224B (en) * | 2021-04-27 | 2022-03-01 | 浙江大学 | Preparation method of titanium-based composite structure material |
| CN114042898B (en) * | 2021-11-10 | 2023-02-28 | 温州医科大学附属口腔医院 | Preparation method of biomedical degradable metal skeleton reinforced Zn-based composite material with large-area galvanic corrosion structure |
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