CN1546178A - Technique for coating porous titanium surface with hydroxyapatite layer - Google Patents

Technique for coating porous titanium surface with hydroxyapatite layer Download PDF

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Publication number
CN1546178A
CN1546178A CNA2003101214419A CN200310121441A CN1546178A CN 1546178 A CN1546178 A CN 1546178A CN A2003101214419 A CNA2003101214419 A CN A2003101214419A CN 200310121441 A CN200310121441 A CN 200310121441A CN 1546178 A CN1546178 A CN 1546178A
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CN
China
Prior art keywords
porous titanium
solution
hour
hours
hydroxyapatite
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Pending
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CNA2003101214419A
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Chinese (zh)
Inventor
廉 周
周廉
王克光
梁芳慧
牛金龙
于振涛
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Northwest Institute for Non Ferrous Metal Research
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Northwest Institute for Non Ferrous Metal Research
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Application filed by Northwest Institute for Non Ferrous Metal Research filed Critical Northwest Institute for Non Ferrous Metal Research
Priority to CNA2003101214419A priority Critical patent/CN1546178A/en
Publication of CN1546178A publication Critical patent/CN1546178A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a method for coating hydroxyl phosphorite layer onto the porous titanium surface, wherein the coating process comprises, immersing in 3-10 mol/ 1 NaOH solution for 12-48 hours at 50 to -80 deg. C, heat preserving at 500-800 deg. C, carrying out thermal treatment, immersing in 0.1-1 mol/ 1 Na2HPO4 solution for 12-48 hours, then immersing in saturated Ca(OH)2 solution for 5-10 hours, immersing in simulated body fluid for 1-4 weeks.

Description

A kind of method that coats hydroxyapatite layer on the POROUS TITANIUM surface
Background technology
A kind of method that coats hydroxyapatite layer on the POROUS TITANIUM surface, relate to a kind of method that on the porous metals titanium of human body implantation usefulness, coats hydroxyapatite layer, particularly utilize hydroxyapatite to improve the method for the surface bioactive of POROUS TITANIUM, be used for the preparation of hard tissue substituting materials such as human body root of the tooth, osteoarthrosis displacement.
Technical field
Generally, the POROUS TITANIUM that is used for implant into body does not have surface bioactive.In human body internal skeleton position, between POROUS TITANIUM and the human body hard tissue, can not form direct synostosis.And because POROUS TITANIUM has internal void, if lack the effect of bone guided, the osseous tissue of human body is difficult to grow into, and influences medical effect.Utilize certain method that the hydroxyapatite of biologically active is compound to the outside and the inner surface of hole of POROUS TITANIUM, then can make POROUS TITANIUM have surface bioactive, and have the bone guided of hydroxyapatite.Yet what use at present is that plasma spraying method is at the porous Ti hydroxyapatite coating layer, its shortcoming is to obtain coating at outer surface, and stop up the POROUS TITANIUM hole easily, cause diminishing of POROUS TITANIUM pore-size, the clinical biological activity of POROUS TITANIUM is descended.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provide a kind of can be when the POROUS TITANIUM surface makes coating, do not stop up the POROUS TITANIUM hole, do not make the POROUS TITANIUM hole obviously reduce, can effectively improve the method that coats hydroxyapatite layer on the POROUS TITANIUM surface of POROUS TITANIUM surface bioactive.
Method of the present invention is achieved through the following technical solutions.
A kind of method that coats hydroxyapatite layer on the POROUS TITANIUM surface is characterized in that the process of coating is followed successively by:
1. POROUS TITANIUM was soaked 12-48 hour under 50 ℃ of-80 ℃ of temperature, in the 3-10mol/lNaOH solution, take out with deionized water rinsing, dry;
2. heat-treated in 1 hour with 500 ℃-800 ℃ insulations of 5 ℃ of/minute programming rates, furnace cooling is to room temperature in stove;
3. the POROUS TITANIUM behind the heat treatment is at 0.1-1mol/lNa 2HPO 4Soaked 12-48 hour in the solution, after taking-up is rinsed well, be dipped into saturated Ca (OH) again 2In the solution 5-10 hour;
4. soak in simulated body fluid, soak time is 1-4 week, soak to take out after washed with de-ionized water, and drying at room temperature is finished on the POROUS TITANIUM surface and formed the hydroxyapatite coating layer process.
Compare with imbedded body in porous titanium without coating, the porous titanium material of preparation hydroxyapatite coating on surface has kept its interconnected pore, the aperture is not subjected to tangible influence, the hydroxyapatite coating that forms 10 μ m-20 μ m at the outer surface and the hole surface of POROUS TITANIUM simultaneously, have surface bioactive and bone guided, be fit to human body and implant.
The specific embodiment
A kind of method that coats hydroxyapatite layer on the POROUS TITANIUM surface is at first soaked porosity 30%-50%, the about 240 μ m POROUS TITANIUM in aperture 12-48 hour under 50 ℃ of-80 ℃ of temperature, in the 3-10mol/lNaOH solution, takes out with deionized water rinsing, dries; Heat-treated in 1 hour with 500 ℃-800 ℃ insulations of 5 ℃ of/minute programming rates, furnace cooling is to room temperature in stove again; With the POROUS TITANIUM behind the heat treatment at 0.1-1mol/lNa 2H-PO 4Soaked 12-48 hour in the solution, after taking-up is rinsed well, be dipped into saturated Ca (OH) again 2In the solution 5-10 hour; Soaking in corresponding simulated body fluid, soak time is 1-4 week, takes out after washed with de-ionized water, and drying at room temperature is finished on the POROUS TITANIUM surface and formed the hydroxyapatite coating layer process.
Embodiment 1
The POROUS TITANIUM of porosity 30%-50%, the about 240 μ m in aperture was handled 24 hours at 60 ℃ through 5mol/lNaOH solution, take out and use deionized water rinsing three times, after drying, air gas heat-treats again, 5 ℃/minute of programming rates, 600 ℃ are incubated 1 hour, and furnace cooling takes out after room temperature in stove.Behind the heat treatment, POROUS TITANIUM by following calcification processing to improve surface bioactive: at 0.1mol/lNa 2HPO 4Soaked 12 hours in the solution, take out flushing and be dipped into saturated Ca (OH) 2In the solution 5 hours.Soak in simulated body fluid, changed liquid in per 48 hours, soak time was 1 week, had formed 10 μ m hydroxyapatite coating layers on the POROUS TITANIUM surface.Take out after washed with de-ionized water drying at room temperature.
Embodiment 2
POROUS TITANIUM was handled 12 hours at 50 ℃ through 3mol/lNaOH solution, taken out and use deionized water rinsing three times, heat-treat again after drying in the air, 5 ℃/minute of programming rates, 800 ℃ are incubated 1 hour, and furnace cooling takes out after room temperature in stove.Behind heat treatment, POROUS TITANIUM is handled to improve surface bioactive at 1mol/lNa by following calcification process 2HPO 4Soaked 48 hours in the solution, take out flushing, be dipped into saturated Ca (OH) 2In the solution 10 hours.Soak in simulated body fluid, changed liquid in per 48 hours, soak time was 4 weeks, had formed 15 μ m hydroxyapatite coating layers on the POROUS TITANIUM surface.Take out after washed with de-ionized water drying at room temperature.
Embodiment 3
POROUS TITANIUM was handled 48 hours at 50 ℃ through 3mol/lNaOH solution, taken out and use deionized water rinsing three times, heat-treat again after drying in the air, 5 ℃/minute of programming rates, 500 ℃ are incubated 1 hour, and furnace cooling takes out after room temperature in stove.Behind heat treatment, POROUS TITANIUM is crossed reason to improve surface bioactive at 0.8mol/lNa by following calcification 2HPO 4Soaked 24 hours in the solution, take out flushing, be dipped into saturated Ca (OH) 2In the solution 8 hours.Soak in simulated body fluid, changed liquid in per 48 hours, soak time was 2 weeks, had formed 15 μ m hydroxyapatite coating layers on the POROUS TITANIUM surface.Take out after washed with de-ionized water drying at room temperature.
Embodiment 4
POROUS TITANIUM was handled 30 hours at 75 ℃ through 10mol/lNaOH solution, taken out and use deionized water rinsing three times, heat-treat again after drying in the air, 5 ℃/minute of programming rates, 750 ℃ are incubated 1 hour, and furnace cooling takes out after room temperature in stove.Behind heat treatment, POROUS TITANIUM is crossed reason to improve surface bioactive at 0.7mol/lNa by following calcification 2HPO 4Soaked 12-48 hour in the solution, take out flushing, be dipped into saturated Ca (OH) 2In the solution 9 hours.Soak in simulated body fluid, changed liquid in per 48 hours, soak time was 1 week, and titanium surface, hole has formed 15 μ m hydroxyapatite coating layers.Take out after washed with de-ionized water drying at room temperature.

Claims (4)

  1. A kind of method that coats hydroxyapatite layer on the POROUS TITANIUM surface is characterized in that its process of coating is followed successively by:
    (1) POROUS TITANIUM was soaked 12-48 hour under 50 ℃ of-80 ℃ of temperature, in the 3-10mol/lNaOH solution, take out with deionized water rinsing, dry;
  2. (2) heat-treated in 1 hour with 500 ℃-800 ℃ insulations of 5 ℃ of/minute programming rates, furnace cooling is to room temperature in stove;
  3. (3) POROUS TITANIUM behind the heat treatment is at 0.1-1mol/lNa 2HPO 4Soaked 12-48 hour in the solution, after taking-up is rinsed well, be dipped into saturated Ca (OH) again 2In the solution 5-10 hour;
  4. (4) soak in simulated body fluid, soak time is 1-4 week, soak to take out after washed with de-ionized water, and drying at room temperature is finished on the POROUS TITANIUM surface and formed the hydroxyapatite coating layer process.
CNA2003101214419A 2003-12-17 2003-12-17 Technique for coating porous titanium surface with hydroxyapatite layer Pending CN1546178A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100369636C (en) * 2005-11-07 2008-02-20 中山大学 Method for preparing titanium-hydroxyapatite bioactive material
CN100430099C (en) * 2005-12-23 2008-11-05 中国科学院金属研究所 Bioactive coating on surface of Titanium or titanium alloy and its preparing method
CN100467669C (en) * 2006-08-23 2009-03-11 天津理工大学 Method of fast growing HA biologically active layer from oxidation film on titanium alloy surface by ultraviolet excitation
CN101584880B (en) * 2009-06-25 2013-03-27 上海交通大学 Material for repairing defect of human body bone and preparation method thereof
CN103083115A (en) * 2011-11-08 2013-05-08 上海交通大学医学院附属第九人民医院 Fiber porous titanium rod for repair of ischemic necrosis of femoral head
CN109602946A (en) * 2018-12-25 2019-04-12 江苏理工学院 A kind of porous titanium alloy surface constructing function gradient composite coating and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100369636C (en) * 2005-11-07 2008-02-20 中山大学 Method for preparing titanium-hydroxyapatite bioactive material
CN100430099C (en) * 2005-12-23 2008-11-05 中国科学院金属研究所 Bioactive coating on surface of Titanium or titanium alloy and its preparing method
CN100467669C (en) * 2006-08-23 2009-03-11 天津理工大学 Method of fast growing HA biologically active layer from oxidation film on titanium alloy surface by ultraviolet excitation
CN101584880B (en) * 2009-06-25 2013-03-27 上海交通大学 Material for repairing defect of human body bone and preparation method thereof
CN103083115A (en) * 2011-11-08 2013-05-08 上海交通大学医学院附属第九人民医院 Fiber porous titanium rod for repair of ischemic necrosis of femoral head
CN109602946A (en) * 2018-12-25 2019-04-12 江苏理工学院 A kind of porous titanium alloy surface constructing function gradient composite coating and preparation method thereof

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