CN108165811A - A kind of preparation method of high-strength degradable nanometer medical porous titanium magnesium base composite material - Google Patents
A kind of preparation method of high-strength degradable nanometer medical porous titanium magnesium base composite material Download PDFInfo
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- CN108165811A CN108165811A CN201810093337.XA CN201810093337A CN108165811A CN 108165811 A CN108165811 A CN 108165811A CN 201810093337 A CN201810093337 A CN 201810093337A CN 108165811 A CN108165811 A CN 108165811A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C3/00—Removing material from alloys to produce alloys of different constitution separation of the constituents of alloys
-
- 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
-
- 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
- B22F3/02—Compacting only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/08—Alloys with open or closed pores
-
- 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
Abstract
The present invention relates to it is a kind of it is degradable with human body compatibility and mechanical property close to the preparation method of the nano-titanium magnesium base composite material of people's bone, specifically a kind of novel porous titanium magnesium base composite material, applied to medical implantation field.The present invention provides the POROUS TITANIUM magnesium base composite material with nanocrystal tissue with titanium, magnesium, silicon, vanadium, silver as initial constituent element, and composition can use aTi bMg cSi dV eAg f（TiC‑SiC‑VC）It represents, wherein a=40, b=10, c=45, d=3, e=1.5, f=0.5 and a+b+c+d+e+f=100, high-strength medical nanoporous titanium magnesium base composite material TiMg 3V 1.5Ag 0.5 is obtained eventually by chemical removal method（TiC‑SiC‑VC）Titanium magnesium is composite porous.Form the nano material of the porous structure with high opening, material is made to have and mechanical property similar in human body, and magnesium slowly can voluntarily be degraded after human body is implanted into, and is provided possibility for the original bone tissue in-growth of body, is promoted the healing of implantation material and the original bone tissue of body.
Description
Technical field
The present invention relates to it is a kind of it is degradable with human body compatibility and mechanical property close to the nano-titanium magnesium composite wood of people's bone
The preparation method of material, specifically a kind of novel porous titanium magnesium base composite material, applied to medical implantation field.
Background technology
Metal and alloy currently used for medicine mainly have medical stainless steel, Medical Cobalt-Based Alloys, medical titanium and its conjunction
There are perishable, released ions may induce disease for the metals such as gold, medical magnesium alloy and alloy, traditional medical metal and alloy
Disease causes cell and tissue necrosis, poor mechanical property, inactive, wear no resistance, fatigue and fracture toughness are not satisfactory etc.
Shortcoming.And conventional implant rigidity is excessively high, and due to this stress shielding, big and rigid femoral prosthesis, it is not recommended that bone density is low
Patient uses, this is related to bone absorption and bone loss caused by a stress shielding.In clinical test, in implantation material 2 years
Interior, the patient for having more than 12% suffers from moderate or serious bone loss.Conventional medical material and human body compatibility and degradability
Difference, bone tissue are unable to ingrowing, it is impossible to and skeleton healing.
Invention content
The purpose of patent of the present invention is the deficiency for the alloy for being currently used for medical domain, in order to reduce implant and week
The mismatch of bone tissue is enclosed, realizes that artificial implantation is transferred to the stiffness optimization loading of adjacent bone, providing one kind has
Good bioactivity, degradable and mechanical property have the nano material of the porous structure of high opening close to people's bone.
The present invention is to realize by following technical solution：
POROUS TITANIUM magnesium base composite material provided by the invention with nanocrystal tissue with titanium, magnesium, silicon, vanadium, silver for initial constituent element,
Its composition can use aTi-bMg-cSi-dV-eAg-f（TiC-SiC-VC）It represents, wherein a=40, b=10, c=45, d=3, e=1.5, f
=0.5 and a+b+c+d+e+f=100, obtain high-strength medical nanoporous titanium magnesium base composite material eventually by chemical removal method
TiMg-3V-1.5Ag-0.5（TiC-SiC-VC）Titanium magnesium is composite porous.POROUS TITANIUM magnesium with nanocrystal tissue is compound
Material, advantage and is characterized in that：It is to use the ingredients such as titanium, magnesium, silicon, vanadium, silver as basic constituent element, the necessary micro member of human body
Plain vanadium, magnesium, wherein magnesium have good degradability, can be decomposed after human body is implanted into automatic slowly, the caustic corrosion of silicon later stage
The presence that the porous structure and titanium of high opening can be formed afterwards makes it have reliable stiffness conditions, and porous titanium
Can make it have with mechanical property similar in skeleton, hole exist for bone tissue in-growth provide may, vanadium can be with
Titanium combines well, and material is made to have good comprehensive performance.The addition of silver metal makes material have broad-spectrum antiseptic attribute, carries
The high medical function of the material.Blank is directly compressed into acetone bonding using after granular material is prepared, is avoided
Conventional metals sintering process generates noxious material, and is not have to pickup by trident die channel to squeeze shape tool repeatedly
There is into the titanium magnesium base composite material of nanocrystal tissue, the nano material of formation is placed in alkali and corrodes to be formed with high opening
Porous structure nano material, material be implanted into human body after slowly can voluntarily degrade, be bone tissue in-growth and implantation
Bone and body bone tissue healing provide may.The present invention provides a kind of high intensity, porous nanometer medical degradable titanium magnesium is compound
The preparation method of material, includes the following steps：
（1）Dispensing base：Take Cp Ti powder, Mg particles（Purity is 99.6%）, Si particles（Purity 99.9%）, V particles（It is pure
Degree 99.9%）, Ag particles（Purity 99.9%）With TiC-SiC-VC whisker particles, the gloves that powder blend is filled in argon gas
It weighs in case, is then mixed and stirred for 3 minutes for 1% isopropanol with weight ratio.Then, by the element mixture slurry from close
It is taken out in glove box in envelope container and pours into die of press access road, while is logical by the outlet of back pressure type punch obstruction
Mixture under 50MPa is cold-pressed, and is dried at room temperature for 5 minutes by road, makes the adhesion strength between isopropanol evaporation and particle
It disappears.The final bar samples for being processed into D10mm × 68mm.
（2）Obtain nano-structure：Sample is packed into jacket, jacket appearance and size is D12mm × 70mm, inner cavity D10mm
× 68mm can be realized without pickup by trident die channel and squeeze repeatedly, obtain the titanium magnesium with nanocrystal tissue
Composite material, the squeezing parameter of trident die channel are：Punch extrusion speed is 1mm/s, by rotating trident mold 6 times
Deformation enough can be accumulated and obtain high-strength nano material.
（3）Form the material of the porous structure with high opening：The rod-like nano material that will be produced by trident mold
In 60 DEG C of 5M sodium hydroxides（NaOH）12 hours are impregnated in aqueous solution to remove Si.For removing the reaction of Si： Si(s) +
2NaOH(aq) + H2O(aq) = Na2SiO3(aq) + 2H2(g)
The porous Ti/Mg composite materials for removing Si materials are washed in distillation warm water and 24 hours dry in air, finally
Obtain the porous Ti based composites with 45% porosity.
Above-mentioned steps（1）The preparation process of middle titanium carbide-titanium carbide silico-carbo vanadium whisker particle is：Titanium oxide-silicon carbide-
Vanadium carbide whisker persursor material chemical composition and weight percent are：V2O5：25.4~28.2%, Ti：19.6~19.8%,
SiO2：25.4~28.2%, C：20.2~22.6%, Mn：0.1~0.9%, NaCl：1.0~8.1%.By what is prepared in proportion
The precursor composite powder that titanium carbide-titanium carbide silico-carbo vanadium whisker can be generated adds absolute ethyl alcohol to carry out machinery in ball mill
Change ball milling 48 hours, obtaining has the ultra-fine precursor composite powder of 200-600nm crystallite dimensions, and powder is packed into crystal vessel
In, under argon gas atmosphere protection and 1550 DEG C -1800 DEG C of temperature condition, heat preservation 90min-180min synthesis.
SiO2+2C=（Heating）Si+2CO↑
Si+C=（Heating）SiC
V2O5+7C=（Heating）2VC+5CO↑
Ti+C =（Heating）TiC
Present invention employs titanium carbide-titanium carbide silico-carbo vanadium to enhance degradable nano medical porous titanium magnesium base composite material, feature
It is：The material forms the titanium carbide-titanium carbide silico-carbo vanadium whisker aligned and titanium magnesium base composite material matrix along streamline is squeezed
Material forms, diameter of whiskers 200-800nm.
The present invention provides a kind of preparation method of high-strength nano medical degradable titanium magnesium base composite material with it is existing medical
Alloy is compared and be the advantage is that：
1. innovated on formula first：Titanium, magnesium, silicon, vanadium is used to be mixed with certain proportion, wherein selecting CP Ti rather than commonly using
Titanium magnesium base composite material, be because it will not discharge XIC alloying elements in vivo, and titanium be it is a kind of can be by radiating consistent wave
The long element that cell ionization is made to adjust body current, so as to generate the physiological action beneficial to human body, titanium has excellent mechanics
Performance, corrosion resistance and biocompatibility are capable of providing enough mechanical strengths, by forming the porous structure of high opening, make
Material has and mechanical property similar in skeleton；Mg and V is the essential trace elements of the human body, and vanadium can be very good and titanium phase
With reference to；As space material, either magnesium or silicon will not all cause cytotoxicity for Mg powder and Si powder, and magnesium have it is mild,
The advantages that absorbable, good biocompatibility, the silicon later stage can fall the material to form the porous structure with high opening with caustic corrosion
Material, the degradation behavior of magnesium make it biodegradable implantation material, can voluntarily degrade in human body after implantation, be bone tissue to
Interior growth and merging bone are provided with body bone tissue healing may.
2. the secondly innovation of fabrication processing：
（a）Using granular material is uniformly prepared bonded by isopropanol after direct pressing formed blank, overcome conventional metals
There may be this shortcomings of noxious material for melting sintering.
（b）Using trident die channel, can be completed to squeeze repeatedly without pickup makes sample that severe plastic deformation occur
So as to obtain the titanium magnesium base composite material with nanocrystal tissue.The nano material of acquisition has intensity height, good toughness, mechanical property
Can it is good, there is good endurance corrosion resistance and degradable.
3. form the innovation of material shape structure：The nano material for processing formation is added in into caustic corrosion and falls silicon, and magnesium later stage
It can voluntarily degrade in human body, to form the nano material of the porous structure with high opening, material be made to have and human body phase
Near mechanical property, and magnesium slowly can voluntarily be degraded after human body is implanted into, and being provided for the original bone tissue in-growth of body can
Can, promote the healing of implantation material and the original bone tissue of body.
4. the required preparation method of the present invention is simple for process, it is easy to accomplish high-volume automated production is planted available for medicine
Enter field.
Description of the drawings：
Here is that specific embodiments of the present invention are described in detail in conjunction with the accompanying drawings and embodiments.
Fig. 1 is the schematic diagram that will be pressed after the uniform hybrid bonding of granular material by forcing press;
Fig. 2 is molding bar samples schematic diagram；
Fig. 3 is that by trident die channel, crimp is prepared with nanocrystal tissue repeatedly in the specific embodiment of the invention
Titanium magnesium base composite material schematic diagram；
Fig. 4 is the schematic diagram that club-shaped material alkali process is formed to porous material；
Label in above-mentioned figure for：
Fig. 1 is that granular material is uniformly mixed to the 1. forcing press upper covers 2. that merga pass suppresses the schematic diagram being pressed
3. forcing press lower cover of forcing press cavity, 4. bar samples squeeze out channel.
Fig. 2 is 1. jacket cover plate, 2. jacket, 3. sample of molding bar samples schematic diagram.
Fig. 3 is that by trident die channel, crimp is prepared with nanocrystal repeatedly in the specific embodiment of the invention
1. punch-pin of the schematic diagram installation drawing of the titanium magnesium base composite material of tissue, 2. extrusion blanks, 3. rotating cavity dies, 4. prestressing force folder
Tool, 5. mandrils, 6. back pressure mandrils, 7. prestress clamp pedestals.
Fig. 4 is that 1. beaker 2.NaOH solution 3. of the schematic diagram that club-shaped material alkali process is formed porous material are rodlike
Nano material.
Specific embodiment：
Example one：A kind of preparation method of high-strength nano medical porous titanium magnesium base composite material
By Ti powder, Mg particles（Purity is 99.6%）, Si particles（Purity 99.9%）, V particles, Ag particles and TiC-SiC-VC
Whisker particle is 40 by mole ratio:10:45:3:1.5:It after 0.5 uniform mixed preparing is good, is bonded with isopropanol, then pressed
It is squeezed, and is dried at room temperature for 5 minutes by die of press on power machine, make the adhesion strength between isopropanol evaporation and particle
It disappears, ultimately forms the bar samples of D10mm × 68mm；Bar samples loading jacket is rotated repeatedly by trident channel,
It squeezes 6 times, generates severe plastic deformation and obtain the titanium magnesium base composite material with nanocrystal tissue, trident die channel is given birth to
The rod-like nano material of production is put into 60 DEG C of 5L sodium hydroxides（NaOH）12 hours are impregnated in aqueous solution to remove Si, it then, will
The porous Ti/Mg composite materials of removal Si materials immerse 5L hydrochloric acid at room temperature（HCl）In 6 hours, wash and with distill temperature
Then water supersonic cleaning distills warm water washing and drying 24 hours in air, final to obtain with 55% porosity
Porous Ti based composites.Ti-10Mg-45Si-3V-1.5Ag-0.5 provided by the invention with nanocrystal tissue（TiC-
SiC-VC）Titanium magnesium base composite material can be used simple metal working equipment and prepare, and then be obtained by chemical removal method high
Intensity nanometer Ti-3V-1.5Ag-0.5（TiC-SiC-VC）Titanium magnesium is composite porous, the porous nanometer material of acquisition have and
Mechanical property similar in skeleton has reliable mechanical hardness and intensity and good toughness.And with good
Degradability, therefore, material of the present invention have potential application value, and field is implanted into available for medicine.
Claims (10)
1. a kind of preparation method of high-strength medical nanoporous titanium magnesium base composite material, it is characterized in that：Using titanium, magnesium, silicon, vanadium as group
Member directly carries out powder after mixed preparing is bonded by isopropanol according to a certain percentage as basic material, by granular material
Compacting forms blank, overcomes conventional metals melting and generates noxious material this shortcoming;Blank is passed through into trident die channel
It can occur to squeeze high-strength material of the severe plastic deformation acquisition with nanocrystal tissue repeatedly without pickup；Then it will receive
In rice material merging alkali silicon is eroded to form the nano material of the porous structure with high opening, and magnesium is after human body is implanted into
It can voluntarily degrade, be that bone tissue in-growth and merging bone may with body bone tissue healing offer.
2. a kind of preparation method of high-strength medical nanoporous titanium magnesium base composite material according to claim 1, feature
It is：POROUS TITANIUM magnesium base composite material provided by the invention with nanocrystal tissue with titanium, magnesium, silicon, vanadium, silver for initial constituent element,
Its composition can use aTi-bMg-cSi-dV-eAg-f（TiC-SiC-VC）It represents, wherein a=40, b=10, c=45, d=3, e=1.5,
F=0.5 and a+b+c+d+e+f=100 obtain high-strength medical nanoporous titanium magnesium base composite material eventually by chemical removal method
TiMg-3V-1.5Ag-0.5（TiC-SiC-VC）Titanium magnesium is composite porous.
3. a kind of preparation method of high-strength medical nanoporous titanium magnesium base composite material according to claim 1, feature
It is：Using compression moulding in forcing press is directly placed into after bonding titanium, magnesium, silicon, vanadium particle by isopropanol, conventional metals are overcome
Sintering generate noxious material this with shortcoming, magnesium, vanadium be human body must trace element, and magnesium has good degradability, and silicon exists
Later stage can fall the nano material to form the porous structure with high opening with caustic corrosion, be bone tissue in-growth, with
And merging bone and body bone tissue healing provide may, the presence of titanium makes material have a reliable mechanical strength, and vanadium can be with
Titanium combines well, and material is made to have good comprehensive performance, and silver metal has broad-spectrum antiseptic attribute, improves the doctor of the material
Use function.
4. a kind of preparation method of high-strength medical nanoporous titanium magnesium base composite material according to claim 1, feature
It is：Trident die channel uses trident channel during squeezing repeatedly, can be realized repeatedly without pickup in extrusion process
It squeezes, accumulates enough equivalent strains, reach crystal grain refinement, obtain the material with nano-structure.
5. a kind of preparation method of high-strength medical nanoporous titanium magnesium base composite material according to claim 1, feature
It is：The nano material of the porous structure with high opening is formed after material, which is placed in aqueous slkali, erodes silicon, magnesium exists
It slowly can voluntarily degrade after material implantation human body, be cured for bone tissue in-growth and merging bone with body bone tissue
Closing offer may.
6. a kind of preparation method of high-strength medical nanoporous titanium magnesium base composite material according to claim 1, feature
It is：The compacting of powder collecting end, trident channel squeeze repeatedly, caustic corrosion forms porous material, and preparation process is as follows：
（a）The initial constituent element of metallic particles provided by claim 2 is uniformly prepared in proportion, and powder blend is filled in argon gas
Glove box in weigh, then with weight ratio be 1% isopropanol be mixed and stirred for 3 minutes；
Then, which from the glove box in sealing container is taken out and pours into die of press entrance and led to
Road, while exit passageway is blocked by back pressure type punch, mixture is cold-pressed under 50MPa, and is dried at room temperature for 5 minutes,
The adhesion strength between isopropanol evaporation and particle is made to disappear；The final bar samples for being processed into D10mm × 68mm；
(b) pickup is not had to by trident die channel by compression molding by the metallic particles constituent element that claim 2 provides
Severe plastic deformation can be completed repeatedly and obtain the high strength titanium magnesium base composite material with nanocrystal tissue；Channel squeezes repeatedly
Machined parameters are：The extrusion speed of punch is 1mm/s, by rotate trident mold can accumulate for 6 times deformation enough obtain it is high-strength
Spend nano material；
(c）By the bar samples that the metallic particles constituent element that claim 2 provides is formed, in 60 DEG C of 5L sodium hydroxides（NaOH）
12 hours are impregnated in aqueous solution to remove Si, warm water washing and drying 24 hours in air is then distilled, is finally had
There is the POROUS TITANIUM magnesium base composite material of 45% porosity.
7. a kind of preparation method of high-strength medical nanoporous titanium magnesium base composite material according to claim 1, feature
It is：Trident die channel needed for the titanium magnesium base composite material with nano-structure that the present invention is formed squeezes required load repeatedly
It is low, the nanometer crystal microstructure of titanium magnesium base composite material can be realized under a much lower load.
8. a kind of preparation method of high-strength medical nanoporous titanium magnesium base composite material according to claim 1, feature
It is：Preparation method needed for invention is simple for process, can be processed in simple metal working equipment, be easy to batch metaplasia
Production can be used in medicine implantation field and do bone replacement material.
9. a kind of preparation method of high-strength medical nanoporous titanium magnesium base composite material according to claim 1, feature
It is：The preparation process of the titanium carbide-titanium carbide silico-carbo vanadium whisker particle is：Titanium oxide-silicon carbide-carbon vanadium whisker forerunner
Body material chemical composition and weight percent are：V2O5：25.4~28.2%, Ti：19.6~19.8%, SiO2：25.4~
28.2%, C：20.2~22.6%, Mn：0.1~0.9%, NaCl：1.0~8.1%, it can generate carbon by what is prepared in proportion
It is small that the precursor composite powder of change titanium-silicon carbide-carbon vanadium whisker adds absolute ethyl alcohol to carry out mechanization ball milling 48 in ball mill
When, obtaining has the ultra-fine precursor composite powder of 200-600nm crystallite dimensions, powder is fitted into crystal vessel, in argon gas gas
Atmosphere is protected under the temperature condition with 1550 DEG C -1800 DEG C, heat preservation 90min-180min synthesis.
10. a kind of preparation method of high-strength medical nanoporous titanium magnesium base composite material according to claim 1, feature
It is that titanium carbide-titanium carbide silico-carbo vanadium enhances the medical porous Titanium-magnesium alloy material of degradable nano, orientation is formed along streamline is squeezed
Titanium carbide-titanium carbide silico-carbo vanadium whisker and titanium magnesium alloy the basis material composition of arrangement, diameter of whiskers 200-800nm.
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Cited By (3)
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| CN111266592A (en) * | 2020-03-25 | 2020-06-12 | 燕山大学 | Titanium-magnesium composite material with double-communication structure and preparation method and application thereof |
| CN111996404A (en) * | 2020-08-21 | 2020-11-27 | 中南大学 | Titanium-based alloy with both quantitative magnesium loading and slow magnesium ion release functions and preparation method and application thereof |
| CN115969551A (en) * | 2023-02-20 | 2023-04-18 | 北京华益圣亚医疗器械有限公司 | Oral implant and manufacturing method thereof |
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| CN111266592A (en) * | 2020-03-25 | 2020-06-12 | 燕山大学 | Titanium-magnesium composite material with double-communication structure and preparation method and application 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 |
| CN111996404A (en) * | 2020-08-21 | 2020-11-27 | 中南大学 | Titanium-based alloy with both quantitative magnesium loading and slow magnesium ion release functions and preparation method and application thereof |
| CN111996404B (en) * | 2020-08-21 | 2021-11-12 | 中南大学 | Titanium-based alloy with both quantitative magnesium loading and slow magnesium ion release functions and preparation method and application thereof |
| CN115969551A (en) * | 2023-02-20 | 2023-04-18 | 北京华益圣亚医疗器械有限公司 | Oral implant and manufacturing method thereof |
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