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CN101229587A - Bioceramic titanium-based composite material and preparation method thereof - Google Patents

Bioceramic titanium-based composite material and preparation method thereof Download PDF

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Publication number
CN101229587A
CN101229587A CNA2008100263783A CN200810026378A CN101229587A CN 101229587 A CN101229587 A CN 101229587A CN A2008100263783 A CNA2008100263783 A CN A2008100263783A CN 200810026378 A CN200810026378 A CN 200810026378A CN 101229587 A CN101229587 A CN 101229587A
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composite material
powder
titanium
nano
bioceramic
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李卫
刘�英
庞鹏沙
夏东升
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Jinan University
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Jinan University
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Abstract

The invention relate to a method for preparing powder metallurgy of bioceramic titanium matrix composite material, which is characterized in that: (1) metal titanium powder with granularity of 5Mum-100Mum and nano-sized hydroxyapatite powder with the granularity less than 100nm are mixed uniformly, wherein, volume fraction of the nano-sized hydroxyapatite powder is 1 percent to 10 percent; (2) the mixing powder is shaped by using isostatic pressing and is vacuum sintered under 1050 DEG C to 1200 DEG C to prepare the bioceramic titanium matrix composite material. bioactivity of the prepared composite material is higher than that of pure titanium material prepared by a powder metallurgy method; bending strength of the composite material is larger than 140MPa, which is higher than or equal to that of human bones; compressive elastic modulus of the composite material is 7.9GPa to18.5GPa, which is close to that of the human bones. The invention can be used for preparing biological replacement (restoration) bodies which are used by hard tissues such as human skeletons, teeth, and so on.

Description

生物陶瓷钛基复合材料及其制备方法 Bioceramic titanium-based composite material and preparation method thereof

技术领域technical field

本发明涉及生物医用金属基复合材料,具体是生物陶瓷钛基复合材料及其制备方法。The invention relates to a biomedical metal-based composite material, in particular to a bioceramic titanium-based composite material and a preparation method thereof.

背景技术Background technique

目前人体骨骼和牙齿等生物硬组织用置换(修复)材料大多为轧制或铸造钛材料,钛材料具有耐腐蚀、强度高和生物相容性等特点。但是轧制或铸造钛材料的弹性模量明显高于人体骨,因而降低了材料的生物力学相容性,限制了钛材料的应用。粉末冶金方法制备的钛材料因具有适量的孔隙,因而使材料的弹性模量下降,材料的生物力学相容性有所改善。然而粉末冶金方法制备的钛材料生物活性有欠缺,材料的生物力学相容性还有待提高。At present, most of the replacement (repair) materials for biological hard tissues such as human bones and teeth are rolled or cast titanium materials. Titanium materials have the characteristics of corrosion resistance, high strength and biocompatibility. However, the elastic modulus of rolled or cast titanium materials is significantly higher than that of human bone, thus reducing the biomechanical compatibility of materials and limiting the application of titanium materials. The titanium material prepared by the powder metallurgy method has an appropriate amount of pores, which reduces the elastic modulus of the material and improves the biomechanical compatibility of the material. However, the biological activity of titanium materials prepared by powder metallurgy methods is lacking, and the biomechanical compatibility of materials needs to be improved.

发明内容Contents of the invention

本发明的目的在于提供一种生物陶瓷钛基复合材料的粉末冶金制备方法,解决现有技术存在的钛材料生物活性有欠缺,材料的弹性模量较高的问题。The purpose of the present invention is to provide a powder metallurgy preparation method for bioceramic titanium-based composite materials, which solves the problems of lack of biological activity of titanium materials and high elastic modulus of materials in the prior art.

本发明的目的还在于提供所述方法制备的生物陶瓷钛基复合材料。The object of the present invention is also to provide the bioceramic titanium-based composite material prepared by the method.

本发明的生物陶瓷钛基复合材料的制备方法,包括如下步骤:The preparation method of the bioceramic titanium-based composite material of the present invention comprises the following steps:

(1)将粒度为5μm~100μm的金属钛粉与粒度小于100nm的纳米羟基磷灰石粉混合均匀,其中纳米羟基磷灰石的体积分数为1%~10%,优选1~9%,进一步优选2~4.9%;(1) Mix uniformly the titanium metal powder with a particle size of 5 μm to 100 μm and the nano-hydroxyapatite powder with a particle size less than 100 nm, wherein the volume fraction of the nano-hydroxyapatite is 1% to 10%, preferably 1 to 9%, further Preferably 2-4.9%;

(2)混合粉末采用等静压成形,然后真空烧结,烧结温度为1050℃~1200℃。(2) The mixed powder is formed by isostatic pressing, and then vacuum sintered at a sintering temperature of 1050°C to 1200°C.

本发明生物陶瓷钛基复合材料及其制备方法的设计依据及主要特点如下:钛粉末加入具有生物活性的纳米羟基磷灰石粉之后,粉末冶金制备的复合材料生物活性提高,复合材料生物活性高于粉末冶金制备的纯钛材料;钛粉末加入纳米羟基磷灰石粉之后,增加了粉末冶金制备的复合材料的孔隙率,进一步降低了复合材料的弹性模量,复合材料压缩弹性模量7.9GPa~18.5GPa,与人体骨接近;钛粉末加入纳米羟基磷灰石粉之后,粉末冶金制备的复合材料的孔隙率增加,使得复合材料的强度有所下降,但是复合材料抗弯强度大于140MPa,仍高于或相当于人体骨。生物陶瓷钛基复合材料可用于制备人体骨骼和牙齿等硬组织用生物置换(修复)体。The design basis and main features of the bioceramic titanium-based composite material and its preparation method of the present invention are as follows: after the titanium powder is added with nano-hydroxyapatite powder with biological activity, the biological activity of the composite material prepared by powder metallurgy is improved, and the biological activity of the composite material is high. Pure titanium material prepared by powder metallurgy; adding nano-hydroxyapatite powder to titanium powder increases the porosity of the composite material prepared by powder metallurgy, further reduces the elastic modulus of the composite material, and the compressive elastic modulus of the composite material is 7.9GPa ~18.5GPa, which is close to human bone; after titanium powder is added with nano-hydroxyapatite powder, the porosity of the composite material prepared by powder metallurgy increases, which makes the strength of the composite material decrease, but the bending strength of the composite material is greater than 140MPa, still Higher than or equivalent to human bone. Bioceramic titanium-based composite materials can be used to prepare biological replacement (restoration) bodies for hard tissues such as human bones and teeth.

具体实施方式Detailed ways

实施例1:将粒度为5μm~100μm的金属钛粉与粒度小于100nm的纳米羟基磷灰石粉(纳米羟基磷灰石粉加入量体积分数10%)混合均匀,混合粉末采用等静压成形,然后在1100℃真空烧结,制备得到生物陶瓷钛基复合材料。复合材料的生物活性高于粉末冶金方法制备的纯钛材料,复合材料抗弯强度154MPa,压缩弹性模量9.3GPa。Embodiment 1: Mix the titanium metal powder with a particle size of 5 μm to 100 μm and the nano-hydroxyapatite powder (the volume fraction of nano-hydroxyapatite powder added is 10%) with a particle size less than 100 nm, and the mixed powder is formed by isostatic pressing. Then vacuum sintering at 1100° C. to prepare a bioceramic titanium-based composite material. The biological activity of the composite material is higher than that of the pure titanium material prepared by powder metallurgy method, the bending strength of the composite material is 154MPa, and the compressive elastic modulus is 9.3GPa.

实施例2:将粒度为5μm~100μm的金属钛粉与粒度小于100nm的纳米羟基磷灰石粉(纳米羟基磷灰石粉加入量体积分数2%)混合均匀,混合粉末采用等静压成形,然后在1100℃真空烧结,制备得到生物陶瓷钛基复合材料。复合材料的生物活性高于粉末冶金方法制备的纯钛材料,复合材料抗弯强度860MPa,压缩弹性模量17GPa。Embodiment 2: the titanium metal powder with a particle size of 5 μm to 100 μm is mixed evenly with nano-hydroxyapatite powder (the volume fraction of nano-hydroxyapatite powder added is 2%) with a particle size less than 100 nm, and the mixed powder is formed by isostatic pressing. Then vacuum sintering at 1100° C. to prepare a bioceramic titanium-based composite material. The biological activity of the composite material is higher than that of the pure titanium material prepared by powder metallurgy method, the bending strength of the composite material is 860MPa, and the compressive elastic modulus is 17GPa.

实施例3:将粒度为5μm~100μm的金属钛粉与粒度小于100nm的纳米羟基磷灰石粉(纳米羟基磷灰石粉加入量体积分数4.9%)混合均匀,混合粉末采用等静压成形,然后在1150℃真空烧结,制备得到生物陶瓷钛基复合材料。复合材料的生物活性高于粉末冶金方法制备的纯钛材料,复合材料抗弯强度435MPa,压缩弹性模量14GPa。Embodiment 3: Mix the titanium metal powder with a particle size of 5 μm to 100 μm and the nano-hydroxyapatite powder with a particle size less than 100 nm (the volume fraction of nano-hydroxyapatite powder added is 4.9%), and the mixed powder is formed by isostatic pressing. Then vacuum sintering at 1150° C. to prepare a bioceramic titanium-based composite material. The biological activity of the composite material is higher than that of the pure titanium material prepared by powder metallurgy method, the bending strength of the composite material is 435MPa, and the compressive elastic modulus is 14GPa.

实施例4:将粒度为5μm~100μm的金属钛粉与粒度小于100nm的纳米羟基磷灰石粉(纳米羟基磷灰石粉加入量体积分数10%)混合均匀,混合粉末采用等静压成形,然后在1050℃真空烧结,制备得到生物陶瓷钛基复合材料。复合材料的生物活性高于粉末冶金方法制备的纯钛材料,复合材料抗弯强度144MPa,压缩弹性模量7.9GPa。Embodiment 4: Mix the titanium metal powder with a particle size of 5 μm to 100 μm and the nano-hydroxyapatite powder with a particle size less than 100 nm (the volume fraction of nano-hydroxyapatite powder added is 10%), and the mixed powder is formed by isostatic pressing. Then vacuum sintering at 1050° C. to prepare a bioceramic titanium-based composite material. The biological activity of the composite material is higher than that of the pure titanium material prepared by powder metallurgy method, the bending strength of the composite material is 144MPa, and the compressive elastic modulus is 7.9GPa.

实施例5:将粒度为5μm~100μm的金属钛粉与粒度小于100nm的纳米羟基磷灰石粉(纳米羟基磷灰石粉加入量体积分数9%)混合均匀,混合粉末采用等静压成形,然后在1100℃真空烧结,制备得到生物陶瓷钛基复合材料。复合材料的生物活性高于粉末冶金方法制备的纯钛材料,复合材料抗弯强度170MPa,压缩弹性模量9.8GPa。Embodiment 5: Mix the titanium metal powder with a particle size of 5 μm to 100 μm and the nano-hydroxyapatite powder (nano-hydroxyapatite powder addition volume fraction 9%) with a particle size less than 100 nm, and the mixed powder is formed by isostatic pressing. Then vacuum sintering at 1100° C. to prepare a bioceramic titanium-based composite material. The biological activity of the composite material is higher than that of the pure titanium material prepared by powder metallurgy method, the bending strength of the composite material is 170MPa, and the compressive elastic modulus is 9.8GPa.

实施例6:将粒度为5μm~100μm的金属钛粉与粒度小于100nm的纳米羟基磷灰石粉(纳米羟基磷灰石粉加入量体积分数1%)混合均匀,混合粉末采用等静压成形,然后在1200℃真空烧结,制备得到生物陶瓷钛基复合材料。复合材料的生物活性高于粉末冶金方法制备的纯钛材料,复合材料抗弯强度950MPa,压缩弹性模量18.5GPa。Embodiment 6: Mix the titanium metal powder with a particle size of 5 μm to 100 μm and the nano-hydroxyapatite powder with a particle size less than 100 nm (the volume fraction of nano-hydroxyapatite powder added is 1%), and the mixed powder is formed by isostatic pressing. Then vacuum sintering at 1200° C. to prepare a bioceramic titanium-based composite material. The biological activity of the composite material is higher than that of the pure titanium material prepared by powder metallurgy method, the bending strength of the composite material is 950MPa, and the compressive elastic modulus is 18.5GPa.

实施例7:将粒度为5μm~100μm的金属钛粉与粒度小于100nm的纳米羟基磷灰石粉(纳米羟基磷灰石粉加入量体积分数3%)混合均匀,混合粉末采用等静压成形,然后在1200℃真空烧结,制备得到生物陶瓷钛基复合材料。复合材料的生物活性高于粉末冶金方法制备的纯钛材料,复合材料抗弯强度720MPa,压缩弹性模量16GPa。Example 7: Mix the titanium metal powder with a particle size of 5 μm to 100 μm and the nano-hydroxyapatite powder with a particle size less than 100 nm (the volume fraction of nano-hydroxyapatite powder added is 3%), and the mixed powder is formed by isostatic pressing. Then vacuum sintering at 1200° C. to prepare a bioceramic titanium-based composite material. The biological activity of the composite material is higher than that of the pure titanium material prepared by powder metallurgy method, the bending strength of the composite material is 720MPa, and the compressive elastic modulus is 16GPa.

Claims (4)

1.一种生物陶瓷钛基复合材料的粉末冶金制备方法,其特征在于包括如下步骤:1. A powder metallurgy preparation method of bioceramic titanium-based composite material, characterized in that it comprises the steps: (1)将粒度为5μm~100μm的金属钛粉与粒度小于100nm的纳米羟基磷灰石粉混合均匀,其中纳米羟基磷灰石体积分数为1%~10%;(1) uniformly mixing metal titanium powder with a particle size of 5 μm to 100 μm and nano-hydroxyapatite powder with a particle size of less than 100 nm, wherein the volume fraction of nano-hydroxyapatite is 1% to 10%; (2)混合粉末采用等静压成形,然后真空烧结,烧结温度为1050℃~1200℃。(2) The mixed powder is formed by isostatic pressing, and then vacuum sintered at a sintering temperature of 1050°C to 1200°C. 2.根据权利要求1所述的方法,其特征在于所述纳米羟基磷灰石的体积分数为1%~9%。2. The method according to claim 1, characterized in that the volume fraction of the nano-hydroxyapatite is 1% to 9%. 3.根据权利要求2所述的方法,其特征在于所述纳米羟基磷灰石的体积分数为2%~4.9%。3. The method according to claim 2, characterized in that the volume fraction of the nano-hydroxyapatite is 2%-4.9%. 4.权利要求1~3任一项所述方法制备得到的生物陶瓷钛基复合材料。4. The bioceramic titanium-based composite material prepared by the method according to any one of claims 1 to 3.
CNA2008100263783A 2008-02-20 2008-02-20 Bioceramic titanium-based composite material and preparation method thereof Pending CN101229587A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101967613A (en) * 2010-10-28 2011-02-09 天津大学 Titanium-based metal glass/hydroxyapatite composite material and preparation method thereof
CN104436297A (en) * 2014-11-28 2015-03-25 中国船舶重工集团公司第七○二研究所 Power material for manufacturing artificial bone and preparation method of power material
CN105251057A (en) * 2015-10-30 2016-01-20 昆明理工大学 Preparation method of porous titanium/hydroxyapatite composite material
WO2017152541A1 (en) * 2016-03-11 2017-09-14 安徽拓宝增材制造科技有限公司 Composite biomedical implant material and preparation method therefor
CN111299572A (en) * 2019-11-28 2020-06-19 天钛隆(天津)金属材料有限公司 Production method of titanium and titanium alloy seamless tube
CN115591013A (en) * 2022-10-14 2023-01-13 中山大学附属口腔医院(Cn) Metal-ceramic mixed gradient 3D printing material and preparation method and application thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101967613A (en) * 2010-10-28 2011-02-09 天津大学 Titanium-based metal glass/hydroxyapatite composite material and preparation method thereof
CN101967613B (en) * 2010-10-28 2012-05-09 天津大学 Titanium-based metal glass/hydroxyapatite composite material and preparation method thereof
CN104436297A (en) * 2014-11-28 2015-03-25 中国船舶重工集团公司第七○二研究所 Power material for manufacturing artificial bone and preparation method of power material
CN104436297B (en) * 2014-11-28 2016-02-03 中国船舶重工集团公司第七○二研究所 Dusty material of a kind of manufacture of intraocular bone and preparation method thereof
CN105251057A (en) * 2015-10-30 2016-01-20 昆明理工大学 Preparation method of porous titanium/hydroxyapatite composite material
WO2017152541A1 (en) * 2016-03-11 2017-09-14 安徽拓宝增材制造科技有限公司 Composite biomedical implant material and preparation method therefor
CN111299572A (en) * 2019-11-28 2020-06-19 天钛隆(天津)金属材料有限公司 Production method of titanium and titanium alloy seamless tube
CN111299572B (en) * 2019-11-28 2022-05-03 天钛隆(天津)金属材料有限公司 Production method of titanium and titanium alloy seamless tube
CN115591013A (en) * 2022-10-14 2023-01-13 中山大学附属口腔医院(Cn) Metal-ceramic mixed gradient 3D printing material and preparation method and application thereof
CN115591013B (en) * 2022-10-14 2024-01-02 中山大学附属口腔医院 Metal-ceramic mixed gradient 3D printing material and preparation method and application thereof

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