CN1827059A - Surface bone-inducting active titanium bone plate and method for manufacturing the same - Google Patents
Surface bone-inducting active titanium bone plate and method for manufacturing the same Download PDFInfo
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- CN1827059A CN1827059A CN 200510048343 CN200510048343A CN1827059A CN 1827059 A CN1827059 A CN 1827059A CN 200510048343 CN200510048343 CN 200510048343 CN 200510048343 A CN200510048343 A CN 200510048343A CN 1827059 A CN1827059 A CN 1827059A
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Abstract
There is a surface-bone induction active-titanium bone plate, whose basal body is medical-grade titanium or titanium alloy. On basal body surface there are micro bores and biology active material layer TiO2-agustite composite bed, whose thickness is 2-10 mum. The manufacturing method of this bone plate is: (1) Adopt alkali treatment-heat treatment, acid-alkali two-steps treatment, anode oxidation treatment and H2O2 immersion to make the titanium or titanium alloy basal body surface form porous TiO2 layer. (2) Dip the porous TiO2 layer covered titanium or titanium alloy bone plate in 36-37deg C SBF cushion liquid for 1-4 weeks, and dry after cleaning to form TiO2-agustite composite bed. (3) Put the dried, porous TiO2 layer covered titanium or titanium alloy bone plate in heat treatment equipment, heat to 610-650deg C and insulate heat for 20-40 minutes, then shut off power supply and cool to room temperature.
Description
The application is for dividing an application the application number of original application: 03117674.7, and the applying date: on April 11st, 2003, denomination of invention: strong internal fixation titanium bone plate of surface activity and manufacture method thereof.
Technical field
The invention belongs to technical field of biological material, the bone that particularly a kind of bone wound surgery, reconstruction surgery, shaping and beauty are used is induced titanium bone plate and manufacture method thereof.
Background technology
Existing bone fracture internal fixation material is most widely used general with the titanium clamping plate, yet the titanium clamping plate mainly concentrate on the morphosis design, do not make surface modification treatment more, can not satisfy the requirement of the inferior light of operation device, more can not reach surface bioactive.As: application number be 00240389, the authorization notification number is 2452458 " repair of cranial defects titanium mesh "; Application number is 01106471, " the chin portion special titanium alloy plintlet " of authorization notification number 2507426 etc.Surface treatment also has some patents to the titanio material, as: application number is that 01132069 Chinese patent application discloses a kind of wollastonite coating one titanium alloy loading bone substitution material and preparation method thereof, this method is chosen the bulk of grain shape or granular silicon lime stone raw material and to two kinds of technologies of its nodularization, then the wollastonite powder is sprayed at it on titanium alloy substrate that cleans with sandblast with atmospheric plasma spraying technology, thereby on titanium alloy substrate, deposits wollastonite coating.Though bearing bone substitution material matrix and Bond Strength of Coating that said method is prepared can reach 35～42MPa, but still can not satisfy the requirement of using as the internal fixation blade plate fully, in addition, the binding ability of wollastonite coating and bone is not good enough, directly affects the serviceability of internal fixation blade plate.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, a kind of surface bone-inducting active titanium bone plate and manufacture method thereof are provided, this kind blade plate not only biology performance is good, and is convenient to clinical figuration.
Surface bone-inducting active titanium bone plate provided by the invention is a matrix with titanium or titanium alloy, and matrix surface is coated with the bioactive materials layer, and this bioactive materials layer and matrix bond are one.The bioactive materials layer has four types: can form TiO
2The porous TiO of gel
2Layer; TiO
2One apatite composite bed; Rutile TiO
2Layer; Hydroxyapatite coating layer.
In order further to improve the biology performance of blade plate, matrix surface is distributed with micropore.In order to satisfy the requirement of clinical figuration, the THICKNESS CONTROL of bioactive materials layer is at 2～10 μ m.
Surface coverage can form TiO
2The porous TiO of gel
2The surface bone-inducting active titanium bone plate of layer has four kinds of manufacture methods: alkali treatment-heat treatment two-step method, Acid-Base two-step process, anodized method and hydrogen peroxide dipping method, the technology of each method is as follows.
1, alkali treatment-heat treatment two-step method
(1) alkali treatment
It is that 50～70 ℃, concentration are that 5～10 moles NaOH solution soaks that titanium or titanium alloy substrate are placed temperature, the Na that generates until matrix surface
2TiO
3Meet till the biological activity requirement, the time was generally 1～24 hour, and the length of soak time is according to the concentration and the Na of NaOH solution
2TiO
3Thickness determine.So-called " biological activity " is meant that material surface can form osteoid apatite in simulated body fluid.
(2) clean with dry
The alkali treatment rear surface is coated with Na
2TiO
3Titanium or titanium alloy substrate water make its drying after cleaning, form porous TiO
2Layer.
(3) heat treatment
Dried surface coverage there is porous TiO
2The titanium or the titanium alloy blade plate of layer are put into Equipment for Heating Processing, be heated to 20～40 minutes (heat treatment temperature is prescribed a time limit on the upper side, and temperature retention time is limit on the lower side, and vice versa) of 610～650 ℃ of insulations with 5 ℃/minute speed, powered-down cools to room temperature with the furnace then, to improve crystal property.
2, Acid-Base two-step process
(1) acid treatment
Treatment fluid is formulated by 98% sulphuric acid, 36% hydrochloric acid and deionized water, sulphuric acid: hydrochloric acid: deionized water=1: 1: 2, at room temperature place above-mentioned treatment fluid to soak 10～60 minutes titanium or titanium alloy substrate, take out then with deionized water or distilled water and clean.
(2) alkali treatment
It is that 120～160 ℃, concentration are that 0.1～0.3 mole NaOH solution boiled 4～6 hours that titanium after the acid treatment or titanium alloy substrate are placed temperature, takes out water then and cleans, and dry back forms porous TiO
2Layer.
3, anodized method
(1) anodized
Electrolyte is the H of 1～3 mole of concentration
2SO
4, at room temperature titanium or titanium alloy substrate are placed the unidirectional current 40～80 seconds of the logical 90～180V of electrolysis unit, carry out anodized.
(2) heat treatment
Titanium after the anodized or titanium alloy substrate are put into Equipment for Heating Processing, be heated to 580～610 ℃ of insulations 40～80 minutes with 5 ℃/minute speed, powered-down cools to room temperature with the furnace and can form porous TiO then
2Layer.
4, hydrogen peroxide dipping method
At room temperature titanium or titanium alloy substrate are placed saturated H
2O
2Soaked in the water 10～40 days, and took out drying then and can form porous TiO
2Layer.
Surface coverage TiO
2The technology of the surface bone-inducting active titanium bone plate manufacture method of one apatite composite bed is as follows:
(1) adopt alkali treatment-heat treating process, Acid-Base two-step process, anodized method, hydrogen peroxide dipping method to make titanium or titanium alloy-based surface form porous TiO
2Layer.
(2) buffer soaks
Surface coverage there is porous TiO
2The SBF buffer that the titanium of layer or titanium alloy blade plate are put into 36～37 ℃ soaked for 1～4 week, carried out drying after the cleaning, can form TiO
2One apatite composite bed.
(3) heat treatment
Dried surface coverage there is TiO
2The titanium of one apatite composite bed or titanium alloy blade plate are put into Equipment for Heating Processing, are heated to 610～650 ℃ of insulations 20～40 minutes with 5 ℃/minute speed, and powered-down cools to room temperature with the furnace then.
The surface coverage rutile TiO
2The manufacture method of the surface bone-inducting active titanium bone plate of layer has two kinds: boiling method and heat treating process.
1, boiling method
Titanium or titanium alloy substrate are placed the boiling pure water 10～20 hours of resistance 1M Ω, take out dry then.
2, heat treating process
Titanium or titanium alloy substrate are put into Equipment for Heating Processing, be heated to 400～600 ℃ of insulations 20～45 minutes with 10 ℃/minute speed, powered-down cools to room temperature with the furnace then.
The technology of the surface bone-inducting active titanium bone plate manufacture method of surface coverage hydroxyapatite coating layer is as follows:
(1) cleans with dry
With titanium or titanium alloy-based body and function ultrasonic waves for cleaning, take out dry then.
(2) make target
With pure ha in 1250 ℃ of sintering in bulk as target.
(3) ion beam diffusion deposition processes
Adopting ion beam to spread the lodgment logos makes the target diffusion and is deposited on titanium or titanium alloy-based surface formation hydroxyapatite coating layer.
(4) argon ion bombardment
In vacuum is 1 * 10
-4～5 * 10
-5In the vacuum of Pa, under 50～75KeV condition, hydroxyapatite coating layer is bombarded argon ion (Ar
+) reach 5 * 10
16Ions/cm
2Get final product, hydroxyapatite coating layer is combined with titanium or titanium alloy substrate.
(5) heat treatment
Titanium that is coated with hydroxyapatite coating layer or titanium alloy blade plate after the argon ion bombardment processing are put into Equipment for Heating Processing, and powered-down cools to room temperature with the furnace when being heated to 400～600 ℃ with 10 ℃/minute speed, to improve crystal property.
The present invention has following beneficial effect:
1, the bioactive materials layer of titanium or titanium alloy substrate surface coverage is for can form TiO
2The porous TiO of gel
2Layer or TiO
2One apatite composite bed or rutile TiO
2Layer or hydroxyapatite coating layer, thereby make surface bone-inducting active titanium bone plate have good biology performance.
2, the thickness of the bioactive materials layer of titanium or titanium alloy substrate surface coverage is 2～10 μ m, thereby surface bone-inducting active titanium bone plate is convenient to clinical figuration.
3, the surface bone-inducting active titanium bone plate surface reaches inferior light, good operability during clinical practice.
4, various manufacturing approach crafts are simple relatively, and raw material is easy to obtain, and are convenient to carry out suitability for industrialized production.
Description of drawings
Fig. 1 is a kind of structure chart of surface bone-inducting active titanium bone plate provided by the present invention;
Fig. 2 is the A-A profile of Fig. 1;
Fig. 3 is another structure chart of surface bone-inducting active titanium bone plate provided by the present invention;
Fig. 4 is the B-B profile of Fig. 3.
Among the figure, 1-titanium or titanium alloy substrate, 2-micropore, 3-porous TiO
2Layer or rutile TiO
2Layer or hydroxyapatite coating layer, 4-TiO
2One apatite composite bed.
The specific embodiment
Embodiment 1: alkali treatment-heat treatment two-step method is made the covering of titanio surface can form TiO
2The porous TiO of gel
2The surface bone-inducting active titanium bone plate of layer
(1) alkali treatment
It is that 60 ℃, concentration are that 8 moles NaOH solution soaked 12 hours that accurately machined medical titanium blade plate matrix is placed temperature, makes matrix surface generate Na
2TiO
3Layer.
(2) clean with dry
The alkali treatment rear surface is coated with Na
2TiO
3The titanium bone plate matrix of layer makes its natural drying after cleaning with distilled water, can form the porous TiO of about 6 micron thickness on titanio body 1 surface
2Layer 3, as shown in Figure 1 and Figure 2.
(3) heat treatment
Dried surface coverage there is porous TiO
2The titanium bone plate matrix of layer is put into Equipment for Heating Processing, carries out temperature programming (as 5 ℃/minute) to 620 ℃ of insulations 30 minutes, and powered-down cools to room temperature with the furnace then, to improve crystal property.
Embodiment 2: the Acid-Base two-step process is made the covering of titanio surface can form TiO
2The porous TiO of gel
2The surface bone-inducting active titanium bone plate of layer
(1) acid treatment
Treatment fluid is formulated by 98% sulphuric acid, 36% hydrochloric acid and deionized water, sulphuric acid: hydrochloric acid: deionized water=1: 1: 2, under room temperature (20 ℃), place above-mentioned treatment fluid to soak 60 minutes accurately machined medical titanium blade plate matrix 1, take out then and use washed with de-ionized water.
(2) alkali treatment
It is that 150 ℃, concentration are that 0.2 mole NaOH solution boiled 4 hours that titanium bone plate matrix 1 after the acid treatment is placed temperature, takes out water then and cleans, and can form the porous TiO of about 5 micron thickness after drying naturally in the titanio surface
2Layer 3, as shown in Figure 1 and Figure 2.
Embodiment 3: anodized manufactured titanium alloy substrate surface coverage can form TiO
2The porous TiO of gel
2The surface bone-inducting active titanium bone plate of layer
(1) anodized
Electrolyte is the H of 1 mole of concentration
2SO
4, under room temperature (20 ℃), place electrolysis unit to carry out anodized accurately machined medical titanium alloy blade plate matrix 1, the unidirectional current of logical 150V 60 seconds.
(2) heat treatment
Titanium alloy blade plate matrix 1 after the anodized is put into Equipment for Heating Processing, carry out temperature programming (as 5 ℃/minute) to 600 ℃ of insulations 60 minutes, powered-down cools to room temperature with the furnace then, can form the porous TiO of about 5 micron thickness in titanium alloy-based surface
2Layer 3, as shown in Figure 1 and Figure 2.
Embodiment 4: hydrogen peroxide dipping manufactured titanium alloy substrate surface coverage can form TiO
2The porous TiO of gel
2The surface bone-inducting active titanium bone plate of layer
At room temperature medical titanium alloy matrix 1 is placed saturated H
2O
2Soaked 20 days in the water, take out the dry porous TiO that can form about 6 micron thickness then in titanium alloy-based surface
2Layer 3, as shown in Figure 1 and Figure 2.
Embodiment 5: alkali treatment-buffer immersion-heat treating process is made titanium alloy substrate surface coverage TiO
2The surface bone-inducting active titanium bone plate of one apatite composite bed
(1) alkali treatment
It is that 70 ℃, concentration are that 5 moles NaOH solution soaked 15 hours that medical titanium alloy matrix 1 is placed temperature, makes matrix surface generate Na
2TiO
3Layer.
(2) clean with dry
The alkali treatment rear surface is coated with Na
2TiO
3Titanium alloy substrate 1 water make its natural drying form porous TiO after cleaning
2Layer.
(3) buffer soaks
Dried surface coverage there is porous TiO
2The titanium alloy blade plate of layer is put into 37 ℃ 2 weeks of SBF buffer immersion and is cleaned once more and drying, can form the TiO of about 8 micron thickness in titanium alloy-based surface
2One apatite composite bed 4, as shown in Figure 3, Figure 4.
(4) heat treatment
Dried surface coverage there is TiO
2The titanium alloy substrate of one apatite composite bed is put into Equipment for Heating Processing, is heated to 650 ℃ of insulations 20 minutes with 5 ℃/minute speed, and powered-down cools to room temperature with the furnace then, to improve crystal property.
Embodiment 6: boiling method is made the titanio surface and is covered rutile TiO
2The bone-inducting active titanium bone plate of layer
Medical titanium matrix 1 is placed the boiling pure water 15 hours of resistance 1M Ω, take out the dry rutile TiO that can form about 4 micron thickness then in the titanio surface
2Layer 3, as shown in Figure 1 and Figure 2.
Embodiment 7: heat treating process is made the titanio surface and is covered rutile TiO
2The surface bone-inducting active titanium bone plate of layer
Medical titanium matrix 1 is put into Equipment for Heating Processing, be heated to 400 ℃ of insulations 45 minutes with 10 ℃/minute speed, powered-down cools to the rutile TiO that room temperature can form about 4 micron thickness in the titanio surface with the furnace then
2 Layer 3, as shown in Figure 1 and Figure 2.
Embodiment 8: the surface bone-inducting active titanium bone plate of ion implantation manufactured titanium alloy substrate surface coverage hydroxyapatite coating layer
(1) cleans with dry
With medical titanium alloy matrix ultrasonic waves for cleaning, take out dry then.
(2) make target
With pure ha in 1250 ℃ of sintering in bulk as target.
(3) ion beam diffusion deposition processes
Adopt ion beam to spread the lodgment logos and make the target diffusion and be deposited on the hydroxyapatite coating layer 3 that titanium alloy substrate 1 surface forms about 4 micron thickness, as shown in Figure 1 and Figure 2.
(4) argon ion bombardment
In vacuum is 1 * 10
-4In the vacuum of Pa, under the 60KeV condition, hydroxyapatite coating layer is bombarded argon ion (Ar
+) reach 5 * 10
16Ions/cm
2Get final product, hydroxyapatite coating layer 3 is combined with titanium alloy substrate 1.
(5) heat treatment
The titanium alloy substrate that is coated with hydroxyapatite coating layer after the argon ion bombardment processing is put into Equipment for Heating Processing, and powered-down cools to room temperature with the furnace when being heated to 450 ℃ with 10 ℃/minute speed, to improve crystal property.
Claims (5)
1, a kind of surface bone-inducting active titanium bone plate, matrix (1) is titanium or titanium alloy, and matrix (1) surface coverage has the bioactive materials layer, it is characterized in that matrix (1) surface distributed has micropore (2), and the bioactive materials layer of matrix (1) surface coverage is TiO
2-apatite composite bed (4), this composite bed thickness are 2～10 μ m.
2, the manufacture method of the described surface bone-inducting active titanium bone plate of a kind of claim 1 is characterized in that processing step is as follows:
(1) alkali treatment
It is that 50～70 ℃, concentration are that 5～10 moles NaOH solution soaks that titanium or titanium alloy substrate are placed temperature, the Na that generates until matrix surface
2TiO
3Meet till the biological activity requirement,
(2) clean with dry
The alkali treatment rear surface is coated with Na
2TiO
3Titanium or titanium alloy substrate water make its drying after cleaning,
(3) surface coverage there is porous TiO
2The SBF buffer that the titanium of layer or titanium alloy blade plate are put into 36～37 ℃ soaked for 1～4 week, cleaned after drying and heat-treated, and was heated to 610～650 ℃ of insulations 20～40 minutes with 5 ℃/minute speed, and powered-down cools to room temperature with the furnace then.
3, the manufacture method of the described surface bone-inducting active titanium bone plate of a kind of claim 1 is characterized in that processing step is as follows:
(1) acid treatment
Treatment fluid is formulated by 98% sulphuric acid, 36% hydrochloric acid and deionized water, sulphuric acid: hydrochloric acid: deionized water=1: 1: 2, at room temperature place above-mentioned treatment fluid to soak 10～60 minutes titanium or titanium alloy substrate, take out then with deionized water or distilled water and clean
(2) alkali treatment
It is that 120～160 ℃, concentration are that 0.1～0.3 mole NaOH solution boiled 4～6 hours that titanium after the acid treatment or titanium alloy substrate are placed temperature, takes out then that water cleans and dry,
(3) surface coverage there is porous TiO
2The SBF buffer that the titanium of layer or titanium alloy blade plate are put into 36～37 ℃ soaked for 1～4 week, cleaned after drying and heat-treated, and was heated to 610～650 ℃ of insulations 20～40 minutes with 5 ℃/minute speed, and powered-down cools to room temperature with the furnace then.
4, the manufacture method of the described surface bone-inducting active titanium bone plate of a kind of claim 1 is characterized in that processing step is as follows:
(1) anodized
Electrolyte is the H of 1～3 mole of concentration
2SO
4, at room temperature place electrolysis unit to carry out anodized titanium or titanium alloy substrate, the unidirectional current of logical 90～180V 40～80 seconds,
(2) surface coverage there is porous TiO
2The SBF buffer that the titanium of layer or titanium alloy blade plate are put into 36～37 ℃ soaked for 1～4 week, cleaned after drying and heat-treated, and was heated to 610～650 ℃ of insulations 20～40 minutes with 5 ℃/minute speed, and powered-down cools to room temperature with the furnace then.
5, the manufacture method of the described surface bone-inducting active titanium bone plate of a kind of claim 1 is characterized in that processing step is as follows:
(1) at room temperature titanium or titanium alloy substrate are placed saturated H
2O
2Soaked in the water 10～40 days, and took out drying then,
(2) surface coverage there is porous TiO
2The SBF buffer that the titanium of layer or titanium alloy blade plate are put into 36～37 ℃ soaked for 1～4 week, cleaned after drying and heat-treated, and was heated to 610～650 ℃ of insulations 20～40 minutes with 5 ℃/minute speed, and powered-down cools to room temperature with the furnace then.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100483436A CN100367917C (en) | 2003-04-11 | 2003-04-11 | Surface bone-inducting active titanium bone plate and method for manufacturing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100483436A CN100367917C (en) | 2003-04-11 | 2003-04-11 | Surface bone-inducting active titanium bone plate and method for manufacturing the same |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03117674 Division CN1242730C (en) | 2003-04-11 | 2003-04-11 | Surface active strong internal fixed titanium bone connection plate and its making method |
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| CN1827059A true CN1827059A (en) | 2006-09-06 |
| CN100367917C CN100367917C (en) | 2008-02-13 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101745144B (en) * | 2009-12-31 | 2013-04-10 | 四川大学 | Preparation method of bone inducing porous titanium artificial bone |
| CN103784210A (en) * | 2014-01-27 | 2014-05-14 | 苏州瑞世医疗科技有限公司 | Novel bone nail and bone plate fixing system matched with bone surface for pet |
| CN104911674A (en) * | 2015-06-30 | 2015-09-16 | 四川大学 | Bioactive coating on surface of porous metal material and preparation method of bioactive coating |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06105900A (en) * | 1992-09-22 | 1994-04-19 | Mitsubishi Materials Corp | Bioactive ceramic coated implant |
| ATE191856T1 (en) * | 1993-11-09 | 2000-05-15 | Found Promotion Ind Science | BONE REPLACEMENT MATERIAL AND METHOD FOR PRODUCING IT |
| JP3026074B2 (en) * | 1997-07-02 | 2000-03-27 | 株式会社ブレーンベース | Implant and manufacturing method thereof |
| CN1147625C (en) * | 2002-03-01 | 2004-04-28 | 西安交通大学 | Porous nano titanium oxide base heterogeneous bioactive surface and its preparing process |
| CN2613245Y (en) * | 2003-04-11 | 2004-04-28 | 四川大学 | Surface active strong internal fixing titanium fracture plate |
-
2003
- 2003-04-11 CN CNB2005100483436A patent/CN100367917C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101745144B (en) * | 2009-12-31 | 2013-04-10 | 四川大学 | Preparation method of bone inducing porous titanium artificial bone |
| CN103784210A (en) * | 2014-01-27 | 2014-05-14 | 苏州瑞世医疗科技有限公司 | Novel bone nail and bone plate fixing system matched with bone surface for pet |
| CN103784210B (en) * | 2014-01-27 | 2016-02-10 | 苏州瑞世医疗科技有限公司 | A kind of nail bone plating fixation system of Novel pet coupling surface of bone |
| CN104911674A (en) * | 2015-06-30 | 2015-09-16 | 四川大学 | Bioactive coating on surface of porous metal material and preparation method of bioactive coating |
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|---|---|
| CN100367917C (en) | 2008-02-13 |
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