CN105367055A - Preparation method for titanium-doped hydroxyapatite/zirconia composite ceramic material - Google Patents
Preparation method for titanium-doped hydroxyapatite/zirconia composite ceramic material Download PDFInfo
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- CN105367055A CN105367055A CN201510877239.1A CN201510877239A CN105367055A CN 105367055 A CN105367055 A CN 105367055A CN 201510877239 A CN201510877239 A CN 201510877239A CN 105367055 A CN105367055 A CN 105367055A
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- hydroxyapatite
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- doped hydroxyapatite
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Abstract
The present invention relates to a preparation method for a titanium-doped hydroxyapatite/zirconia composite ceramic material and belongs to the field of bone tissue engineering. The method comprises the steps of preparing titanium-doped hydroxyapatite; mixing the titanium-doped hydroxyapatite with zirconia powder; and sintering the composite material by using a large amount of heat released by a thermite reaction. Moreover, magnesium oxide, magnesium nitride, and the like simultaneously generated in the high-temperature environment with calcium oxide powder are taken together as a stabilizer to solve the problem of a high thermal expansion coefficient caused by independently using calcium oxide as the stabilizer. The prepared composite ceramic material disclosed by the present invention combines bioactivity of the hydroxyapatite material, and high strength and good toughness of the zirconia, and thus is a good alternative material for the bone tissue engineering.
Description
Technical field
The present invention relates to a kind of preparation method of titanium doped hydroxyapatite/zirconia composite ceramics material, belong to bone tissue engineer field.
Background technology
Hydroxyapatite, as bioceramic material, has very important meaning in the defect repair of bone and tooth and bone tissue engineer alternative aspect.Assign to from one-tenth, the inorganic components of skeleton is osteolith, usually, containing other ions many in osteolith, and such as K
+, Na
+, Mg
+, CI
one, F
oneand CO
3 2 onecan Ca to some extent in substituted apatite in, these ions
2+or OH
-, in the biological procedures in human body, play very important effect.From structure, the structure of human bone phosphatic rock is about 40 ~ 60nm, wide about 20nm, main elementary cell is needle-like or bar-shaped phosphorite crystal, their directed and multiple texture of volume arrangement formation, be conducive to the transmission of nutritive substance, the inner three-dimensional porous structure be communicated with can allow cell attachment, Differentiation and proliferation, for biofluid provides passage.Freshman bone tissue can grow in hole along the hole wall of vesicular structure, forms synostosis.From performance, the one-component hydroxyapatite intensity of synthetic is low, poor toughness, is difficult to bear larger load, limits its use as engineering material of bone tissue.
Zirconium white high specific surface area, has very high fusing point, and high-purity compact zircite product has that use temperature is high, the corroded by liquid of resistance to melting, antiscour, be not easy precipitation, good chemical stability, is a kind of broad-spectrum high-performance refractory goods.ZrO
2fusing point, up to 2690 DEG C, is a kind of high grade refractory, has fire performance high, and chemical stability is good, particular advantages stable under oxidation, reduction and vacuum state.
For a long time, for the fused quartz smelting furnace of 2000 DEG C or higher and the zircite product of superhard alloy medium-frequency induction furnace, the complete of stablizer calcium oxide content 4.4 ~ 4.7wt% is usually adopted to stablize ZrO
2produce.Adopt the zircite product produced in this way and there is following shortcoming: coefficient of thermal expansion is large, and thermal expansivity is high, with partially stabilized ZrO
2compare, thermal expansivity is almost partially stabilized ZrO
2twice, at 1500 DEG C, entirely stablize ZrO
2thermal expansivity is 11 × 10-6/ DEG C or higher.Often because coefficient of thermal expansion is excessive, heat-shock resistance is poor and squeezed off crowded broken or flake-off sheet, thus causes product rejection.
Summary of the invention
The technical problem that the present invention mainly solves: low as engineering material of bone tissue intensity for current single component hydroxyapatite, poor toughness, zirconium white has excellent room-temperature mechanical property, high strength, high-fracture toughness, corrosion-resistant and biologically inert is the toughness reinforcing preferred material of hydroxyapatite, but the zircite product coefficient of thermal expansion under high temperature is large, thermal expansivity is high, cause its heat-shock resistance difference and squeezed off crowded broken or flake-off sheet, and zirconium white is difficult to the problem of sintering under low temperature, provide a kind of preparation method of titanium doped hydroxyapatite/zirconia composite ceramics material, the method first prepares titanium doped hydroxyapatite, mix with Zirconium oxide powder afterwards, release a large amount of heat by thermite reaction and carry out sintered composite materials, and at the magnesium oxide that hot environment generates simultaneously, the materials such as magnesium nitride and lime powder solve the high problem of thermal expansivity when being used alone calcium oxide as stablizer jointly, the composite ceramic material that the present invention obtains combines the biological activity of hydroxyapatite material and zirconic high strength and excellent toughness, it is the good equivalent material of bone tissue engineer.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention:
(1) 1 ~ 2kg hydroxyapatite is taken, put into stoning machine and pulverize 40 mesh standard sieves, particle after pulverizing is moved in mortar, pulverize, and get 100 ~ 200g hydroxyapatite powder and pour in 1L beaker, add 700 ~ 800mL distilled water, be placed on magnetic stirrer, stir 20 ~ 30min with the rotating speed of 300 ~ 400r/min and obtain hydroxyapatite suspension liquid;
(2) getting 0.5 ~ 1g tetrabutyl titanate joins in 10 ~ 20mL dehydrated alcohol, stir with glass stick, by in the hydroxyapatite suspension liquid under obtained tetrabutyl titanate ethanolic soln instillation whipped state, control rate of addition to make to dropwise in its 10 ~ 20min, after dropwising, shaking table oscillatory reaction 5 ~ 6h and airtight leave standstill 24 ~ 36h;
(3) Büchner funnel poured into by the mixed solution after getting above-mentioned leaving standstill, suction filtration is washed respectively 3 ~ 5 times with dehydrated alcohol and deionized water, separation is precipitated thing, to be positioned in baking oven dry 1 ~ 2h at 65 ~ 75 DEG C, again dry sediment is moved in crucible and put into high temperature resistance furnace, be warming up to 1200 DEG C with the rate program of 5 DEG C/min, high-temperature calcination 1 ~ 2h obtains titanium doped hydroxyapatite;
(4) take in the above-mentioned obtained titanium doped hydroxyapatite of 50 ~ 60g and 70 ~ 80g Zirconium oxide powder loading steel closed reactor, add 15 ~ 25g Manganse Dioxide, 10 ~ 15g aluminium powder and 5 ~ 8g Potcrate, by container sealing after mixing, the gas mixture of nitrogen and oxygen is passed in container, passing into speed is 5mL/min, drains the air in container;
(5) magnesium rod after lighting is put into encloses container after terminating by exhaust, continue in encloses container, to pass into oxygen with the speed of 5mL/min, after reaction 1 ~ 2h, 30 ~ 40g calcium oxide is added in container, and in container, pass into acetylene gas with the speed of 20mL/min, after continuing reaction 2 ~ 3h, naturally cool to room temperature;
(6) reaction product in container after cooling is taken out, put into ball mill ball grinds, after pack, namely obtain a kind of titanium doped hydroxyapatite/zirconia composite ceramics material.
Embody rule method of the present invention: emulation aggregate made by titanium doped hydroxyapatite/zirconia composite ceramics material the present invention obtained, first by its high-temperature disinfection treatment 3 ~ 5h at 600 DEG C, after being cooled to room temperature afterwards, by scleroblast (2 × 10
4) be directly inoculated in emulation aggregate surface, in 37 DEG C of constant temperature and 5%CO
2damp atmosphere atmosphere under cultivate, detected cell number every 3 ~ 5 days, find that cell enlargement rate reaches 30 ~ 40%, prove that this material can be used for viable transplantation.
Beneficial effect of the present invention: the composite ceramic material that the present invention obtains combines the biological activity of hydroxyapatite material and zirconic high strength and excellent toughness, is the good equivalent material of bone tissue engineer.
Embodiment
Take 1 ~ 2kg hydroxyapatite, put into stoning machine and pulverize 40 mesh standard sieves, particle after pulverizing is moved in mortar, pulverize, and get 100 ~ 200g hydroxyapatite powder and pour in 1L beaker, add 700 ~ 800mL distilled water, be placed on magnetic stirrer, stir 20 ~ 30min with the rotating speed of 300 ~ 400r/min and obtain hydroxyapatite suspension liquid; Getting 0.5 ~ 1g tetrabutyl titanate joins in 10 ~ 20mL dehydrated alcohol, stir with glass stick, by in the hydroxyapatite suspension liquid under obtained tetrabutyl titanate ethanolic soln instillation whipped state, control rate of addition to make to dropwise in its 10 ~ 20min, after dropwising, shaking table oscillatory reaction 5 ~ 6h and airtight leave standstill 24 ~ 36h; Büchner funnel poured into by the mixed solution got after above-mentioned leaving standstill, suction filtration is washed respectively 3 ~ 5 times with dehydrated alcohol and deionized water, separation is precipitated thing, to be positioned in baking oven dry 1 ~ 2h at 65 ~ 75 DEG C, again dry sediment is moved in crucible and put into high temperature resistance furnace, be warming up to 1200 DEG C with the rate program of 5 DEG C/min, high-temperature calcination 1 ~ 2h obtains titanium doped hydroxyapatite; Take in the above-mentioned obtained titanium doped hydroxyapatite of 50 ~ 60g and 70 ~ 80g Zirconium oxide powder loading steel closed reactor, add 15 ~ 25g Manganse Dioxide, 10 ~ 15g aluminium powder and 5 ~ 8g Potcrate, by container sealing after mixing, the gas mixture of nitrogen and oxygen is passed in container, passing into speed is 5mL/min, drains the air in container; After exhaust terminates, the magnesium rod after lighting is put into encloses container, continue in encloses container, to pass into oxygen with the speed of 5mL/min, after reaction 1 ~ 2h, 30 ~ 40g calcium oxide is added in container, and in container, pass into acetylene gas with the speed of 20mL/min, after continuing reaction 2 ~ 3h, naturally cool to room temperature; Reaction product in container after cooling is taken out, puts into ball mill ball grinds, after pack, namely obtain a kind of titanium doped hydroxyapatite/zirconia composite ceramics material.
Example 1
Take 1kg hydroxyapatite, put into stoning machine and pulverize 40 mesh standard sieves, particle after pulverizing is moved in mortar, pulverize, and get 100g hydroxyapatite powder and pour in 1L beaker, add 700mL distilled water, be placed on magnetic stirrer, stir 20min with the rotating speed of 300r/min and obtain hydroxyapatite suspension liquid; Getting 0.5g tetrabutyl titanate joins in 10mL dehydrated alcohol, stir with glass stick, by in the hydroxyapatite suspension liquid under obtained tetrabutyl titanate ethanolic soln instillation whipped state, control rate of addition to make to dropwise in its 10min, after dropwising, shaking table oscillatory reaction 5h airtight standing 24h; Büchner funnel poured into by the mixed solution got after above-mentioned leaving standstill, suction filtration is washed respectively 3 times with dehydrated alcohol and deionized water, separation is precipitated thing, to be positioned in baking oven dry 1h at 65 DEG C, again dry sediment is moved in crucible and put into high temperature resistance furnace, be warming up to 1200 DEG C with the rate program of 5 DEG C/min, high-temperature calcination 1h obtains titanium doped hydroxyapatite; Take in the above-mentioned obtained titanium doped hydroxyapatite of 50g and 70g Zirconium oxide powder loading steel closed reactor, add 15g Manganse Dioxide, 10g aluminium powder and 5g Potcrate, by container sealing after mixing, the gas mixture of nitrogen and oxygen is passed in container, passing into speed is 5mL/min, drains the air in container; After exhaust terminates, the magnesium rod after lighting is put into encloses container, continue in encloses container, to pass into oxygen with the speed of 5mL/min, after reaction 1h, 30g calcium oxide is added in container, and in container, pass into acetylene gas with the speed of 20mL/min, after continuing reaction 2h, naturally cool to room temperature; Reaction product in container after cooling is taken out, puts into ball mill ball grinds, after pack, namely obtain a kind of titanium doped hydroxyapatite/zirconia composite ceramics material.
Embody rule method of the present invention: emulation aggregate made by titanium doped hydroxyapatite/zirconia composite ceramics material the present invention obtained, first by its high-temperature disinfection treatment 3h at 600 DEG C, after being cooled to room temperature afterwards, by scleroblast (2 × 10
4) be directly inoculated in emulation aggregate surface, in 37 DEG C of constant temperature and 5%CO
2damp atmosphere atmosphere under cultivate, detected cell number every 3 days, find that cell enlargement rate reaches 30%, prove that this material can be used for viable transplantation.
Example 2
Take 1kg hydroxyapatite, put into stoning machine and pulverize 40 mesh standard sieves, particle after pulverizing is moved in mortar, pulverize, and get 150g hydroxyapatite powder and pour in 1L beaker, add 750mL distilled water, be placed on magnetic stirrer, stir 25min with the rotating speed of 350r/min and obtain hydroxyapatite suspension liquid; Getting 0.8g tetrabutyl titanate joins in 15mL dehydrated alcohol, stir with glass stick, by in the hydroxyapatite suspension liquid under obtained tetrabutyl titanate ethanolic soln instillation whipped state, control rate of addition to make to dropwise in its 15min, after dropwising, shaking table oscillatory reaction 5h airtight standing 30h; Büchner funnel poured into by the mixed solution got after above-mentioned leaving standstill, suction filtration is washed respectively 4 times with dehydrated alcohol and deionized water, separation is precipitated thing, to be positioned in baking oven dry 1h at 70 DEG C, again dry sediment is moved in crucible and put into high temperature resistance furnace, be warming up to 1200 DEG C with the rate program of 5 DEG C/min, high-temperature calcination 1h obtains titanium doped hydroxyapatite; Take in the above-mentioned obtained titanium doped hydroxyapatite of 55g and 75g Zirconium oxide powder loading steel closed reactor, add 20g Manganse Dioxide, 13g aluminium powder and 7g Potcrate, by container sealing after mixing, the gas mixture of nitrogen and oxygen is passed in container, passing into speed is 5mL/min, drains the air in container; After exhaust terminates, the magnesium rod after lighting is put into encloses container, continue in encloses container, to pass into oxygen with the speed of 5mL/min, after reaction 1h, 35g calcium oxide is added in container, and in container, pass into acetylene gas with the speed of 20mL/min, after continuing reaction 2h, naturally cool to room temperature; Reaction product in container after cooling is taken out, puts into ball mill ball grinds, after pack, namely obtain a kind of titanium doped hydroxyapatite/zirconia composite ceramics material.
Embody rule method of the present invention: emulation aggregate made by titanium doped hydroxyapatite/zirconia composite ceramics material the present invention obtained, first by its high-temperature disinfection treatment 3h at 600 DEG C, after being cooled to room temperature afterwards, by scleroblast (2 × 10
4) be directly inoculated in emulation aggregate surface, in 37 DEG C of constant temperature and 5%CO
2damp atmosphere atmosphere under cultivate, detected cell number every 4 days, find that cell enlargement rate reaches 35%, prove that this material can be used for viable transplantation.
Example 3
Take 2kg hydroxyapatite, put into stoning machine and pulverize 40 mesh standard sieves, particle after pulverizing is moved in mortar, pulverize, and get 200g hydroxyapatite powder and pour in 1L beaker, add 800mL distilled water, be placed on magnetic stirrer, stir 30min with the rotating speed of 400r/min and obtain hydroxyapatite suspension liquid; Getting 1g tetrabutyl titanate joins in 20mL dehydrated alcohol, stir with glass stick, by in the hydroxyapatite suspension liquid under obtained tetrabutyl titanate ethanolic soln instillation whipped state, control rate of addition to make to dropwise in its 20min, after dropwising, shaking table oscillatory reaction 6h airtight standing 36h; Büchner funnel poured into by the mixed solution got after above-mentioned leaving standstill, suction filtration is washed respectively 5 times with dehydrated alcohol and deionized water, separation is precipitated thing, to be positioned in baking oven dry 2h at 75 DEG C, again dry sediment is moved in crucible and put into high temperature resistance furnace, be warming up to 1200 DEG C with the rate program of 5 DEG C/min, high-temperature calcination 2h obtains titanium doped hydroxyapatite; Take in the above-mentioned obtained titanium doped hydroxyapatite of 60g and 80g Zirconium oxide powder loading steel closed reactor, add 25g Manganse Dioxide, 15g aluminium powder and 8g Potcrate, by container sealing after mixing, the gas mixture of nitrogen and oxygen is passed in container, passing into speed is 5mL/min, drains the air in container; After exhaust terminates, the magnesium rod after lighting is put into encloses container, continue in encloses container, to pass into oxygen with the speed of 5mL/min, after reaction 2h, 40g calcium oxide is added in container, and in container, pass into acetylene gas with the speed of 20mL/min, after continuing reaction 3h, naturally cool to room temperature; Reaction product in container after cooling is taken out, puts into ball mill ball grinds, after pack, namely obtain a kind of titanium doped hydroxyapatite/zirconia composite ceramics material.
Embody rule method of the present invention: emulation aggregate made by titanium doped hydroxyapatite/zirconia composite ceramics material the present invention obtained, first by its high-temperature disinfection treatment 5h at 600 DEG C, after being cooled to room temperature afterwards, by scleroblast (2 × 10
4) be directly inoculated in emulation aggregate surface, in 37 DEG C of constant temperature and 5%CO
2damp atmosphere atmosphere under cultivate, detected cell number every 5 days, find that cell enlargement rate reaches 40%, prove that this material can be used for viable transplantation.
Claims (1)
1. a preparation method for titanium doped hydroxyapatite/zirconia composite ceramics material, is characterized in that concrete preparation process is:
(1) 1 ~ 2kg hydroxyapatite is taken, put into stoning machine and pulverize 40 mesh standard sieves, particle after pulverizing is moved in mortar, pulverize, and get 100 ~ 200g hydroxyapatite powder and pour in 1L beaker, add 700 ~ 800mL distilled water, be placed on magnetic stirrer, stir 20 ~ 30min with the rotating speed of 300 ~ 400r/min and obtain hydroxyapatite suspension liquid;
(2) getting 0.5 ~ 1g tetrabutyl titanate joins in 10 ~ 20mL dehydrated alcohol, stir with glass stick, by in the hydroxyapatite suspension liquid under obtained tetrabutyl titanate ethanolic soln instillation whipped state, control rate of addition to make to dropwise in its 10 ~ 20min, after dropwising, shaking table oscillatory reaction 5 ~ 6h and airtight leave standstill 24 ~ 36h;
(3) Büchner funnel poured into by the mixed solution after getting above-mentioned leaving standstill, suction filtration is washed respectively 3 ~ 5 times with dehydrated alcohol and deionized water, separation is precipitated thing, to be positioned in baking oven dry 1 ~ 2h at 65 ~ 75 DEG C, again dry sediment is moved in crucible and put into high temperature resistance furnace, be warming up to 1200 DEG C with the rate program of 5 DEG C/min, high-temperature calcination 1 ~ 2h obtains titanium doped hydroxyapatite;
(4) take in the above-mentioned obtained titanium doped hydroxyapatite of 50 ~ 60g and 70 ~ 80g Zirconium oxide powder loading steel closed reactor, add 15 ~ 25g Manganse Dioxide, 10 ~ 15g aluminium powder and 5 ~ 8g Potcrate, by container sealing after mixing, the gas mixture of nitrogen and oxygen is passed in container, passing into speed is 5mL/min, drains the air in container;
(5) magnesium rod after lighting is put into encloses container after terminating by exhaust, continue in encloses container, to pass into oxygen with the speed of 5mL/min, after reaction 1 ~ 2h, 30 ~ 40g calcium oxide is added in container, and in container, pass into acetylene gas with the speed of 20mL/min, after continuing reaction 2 ~ 3h, naturally cool to room temperature;
(6) reaction product in container after cooling is taken out, put into ball mill ball grinds, after pack, namely obtain a kind of titanium doped hydroxyapatite/zirconia composite ceramics material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113024247A (en) * | 2021-02-25 | 2021-06-25 | 泉州新致美义齿有限公司 | Combined prosthesis and production process |
| CN113956035A (en) * | 2021-10-28 | 2022-01-21 | 武汉理工大学 | Zirconium oxide composite calcium-phosphorus ceramic slurry and preparation method and application thereof |
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|---|---|---|---|---|
| CN1709829A (en) * | 2005-06-29 | 2005-12-21 | 上海大学 | Hydroxyapatite-zirconium dioxide composite bioceramic material and its preparing method |
| CN102910605A (en) * | 2012-09-14 | 2013-02-06 | 陕西科技大学 | Titanium-containing HA-ZrO2Preparation method of biological composite nano powder |
| CN103585672A (en) * | 2013-11-18 | 2014-02-19 | 西南科技大学 | Preparation method of bioglass fiber reinforced hydroxyapatite porous composite material |
| CN104399116A (en) * | 2014-11-10 | 2015-03-11 | 苏州维泰生物技术有限公司 | Hydroxy apatite/zirconia composite bio-ceramic and preparation method thereof |
| CN104744025A (en) * | 2015-03-31 | 2015-07-01 | 苏州维泰生物技术有限公司 | Hydroxyapatite/aluminum oxide composite bioceramic and preparation method thereof |
-
2015
- 2015-12-03 CN CN201510877239.1A patent/CN105367055A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709829A (en) * | 2005-06-29 | 2005-12-21 | 上海大学 | Hydroxyapatite-zirconium dioxide composite bioceramic material and its preparing method |
| CN102910605A (en) * | 2012-09-14 | 2013-02-06 | 陕西科技大学 | Titanium-containing HA-ZrO2Preparation method of biological composite nano powder |
| CN103585672A (en) * | 2013-11-18 | 2014-02-19 | 西南科技大学 | Preparation method of bioglass fiber reinforced hydroxyapatite porous composite material |
| CN104399116A (en) * | 2014-11-10 | 2015-03-11 | 苏州维泰生物技术有限公司 | Hydroxy apatite/zirconia composite bio-ceramic and preparation method thereof |
| CN104744025A (en) * | 2015-03-31 | 2015-07-01 | 苏州维泰生物技术有限公司 | Hydroxyapatite/aluminum oxide composite bioceramic and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113024247A (en) * | 2021-02-25 | 2021-06-25 | 泉州新致美义齿有限公司 | Combined prosthesis and production process |
| CN113956035A (en) * | 2021-10-28 | 2022-01-21 | 武汉理工大学 | Zirconium oxide composite calcium-phosphorus ceramic slurry and preparation method and application thereof |
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Application publication date: 20160302 |