CN102824656A - Zirconia, hydroxyapatite and magnesium phosphate laminar composite - Google Patents
Zirconia, hydroxyapatite and magnesium phosphate laminar composite Download PDFInfo
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- CN102824656A CN102824656A CN 201210321591 CN201210321591A CN102824656A CN 102824656 A CN102824656 A CN 102824656A CN 201210321591 CN201210321591 CN 201210321591 CN 201210321591 A CN201210321591 A CN 201210321591A CN 102824656 A CN102824656 A CN 102824656A
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- hydroxyapatite
- magnesium phosphate
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- zirconia
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Abstract
The invention discloses a zirconia, hydroxyapatite and magnesium phosphate laminar composite and belongs to the field of medical laminar composites. A method for preparing the laminar composite is characterized in that a zirconia and hydroxyapatite two-component slurry layer and a zirconia, hydroxyapatite and magnesium phosphate three-component slurry layer are coated outside a zirconia ceramic surface layer with stable yttria through a physical coating method in sequence. The flexure strength and the breaking tenacity of the laminar composite are enhanced through adjusting the addition of zirconia of an inner layer, and the bone-growth inducibility of the laminar composite is improved through regulating the addition of hydroxyapatite and magnesium phosphate of an outer layer. The prepared multilayer ceramic composite is superior to a traditional bone repair material in flexure strength and breaking tenacity. Moreover, the multilayer ceramic composite is higher in biocompatibility and inducing osteogenesis capability and can be used for repairing bone defects of parts, such as shanks, thigh joints and the like.
Description
Technical field
A kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite belong to medical laminar composite field.
Background technology
The osseous tissue damage is common clinically frequently-occurring disease; Because the bone that various pathological changes such as wound, inflammation, bone tumor excision cause is damaged to be the problem that often runs into clinically; Wherein some pathological changes causes the large defect of bone; The limit that has surpassed bone self repair ability is perhaps because pathological changes causes the forfeiture of osseous tissue function etc.Need this moment to repair, replace the tissue of damaged or pathological changes by means of biomaterial through operation.
The bone transplanting mode mainly contains autologous bone transplanting and allogenic bone transplantation.Autologous bone transplanting does not have immunological rejection, and cell in the bone graft and bioactive molecule can continue survival at acceptor site, and the performance corresponding function; Promote the damaged healing of bone; This is that other materials is incomparable, but that this method is got the bone amount is limited, and its size and dimension usually is restricted; And supply the bone district to fall ill easily, increase less patient suffering.Allograph bone can provide the cortical bone or the spongy bone of a large amount of difformities, size; But it causes immunological rejection easily; Connection speed at damaged edge of bone and host bone is very slow; And the danger of the toxicity disease that spreads disease is arranged, and the cost of sample preparation, processing and storage is high, therefore uses to be very limited.In order to overcome these limitations, people's bone renovating material that begins one's study.
At present, the artificial bone repair materials of clinical use cuts both ways, and still can not reach the requirement of repairing bone defect ideal material, as: lack the growth of uniform pore structure, its degradation speed and osseous tissue and substitute the inharmonious and mechanical strength performance of speed and do not match etc.In order to improve material mechanical performance and new bone formation speed, often introduce somatomedin or organic polymer and improve its performance.Therefore, with the hydroxyapatite be the focus that the similar composite bone substitution material of fundamental construction and nature bone has become current research.
Can be divided into ceramic material and metal material with the compound enhancing body of hydroxyapatite, as: Al
2O
3, ZrO
2, TiO
2With bio-vitric etc., silicone rubber, polylactic acid, polymethyl methacrylate, collagen, polycaprolactone and chitosan etc. are arranged with the compound organic polymer of hydroxyapatite.In recent years, people had carried out with metallic particles, metallic compound, nano-particle, whisker, long fibre and zirconium oxide and had strengthened the work of hydroxyl apatite bioceramic composite study.The result shows that the adding of granule and fiber can improve the hardness and the intensity of material, but the introducing of second phase tends to cause the biocompatibility of material to reduce, even quickens hydroxyapatite and decompose.
Magnesium is a kind of important trace element in the human body, with the mineralization of biological tissue close getting in touch is arranged, and affects indirectly the mineral metabolism.Simultaneously, people's skeleton contains the magnesium of 0.72wt.%, and magnesium is also played an important role in osteogenesis and bone reparation.Magnesium substituted apatite material that there are some researches show the calcium gained in the magnesium substituted hydroxy apatite has good biocompatibility and bone conductibility.2006, utilizations such as H.Liang were that magnesium ion source utilizes ion implantation apparatus that magnesium ion is injected 15%Al with MEVVA
2O
3/ 3YSZ prepares complex phase ceramic, and research shows that the injection of magnesium ion has improved the biological activity of zirconia ceramics, and the degree that biological activity improves is relevant with the amount that magnesium ion injects.
Magnesium phosphate can occur decomposing when temperature is higher than 1300 ℃ as a kind of phosphate that contains magnesium ion, if therefore it is added in the zirconia ceramics; Behind high temperature sintering; Can occur the pore that magnesium phosphate decomposes in the complex phase ceramic, this pore that contains magnesium ion is induced osteoplastic effect and ability, and the soft or hard at interface is organized in the hole of all growing into; Form the state of fibrous tissue and freshman bone tissue's cross coupled, and keep normal metabolism relation.
In sum; Hydroxyapatite has good biocompatibility, and magnesium ion has the effect of induced osteogenesis, and zirconia ceramics material has the good mechanical performance; With three kinds of compound a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composites prepared of raw material, can be used for the bone defect repair.
Summary of the invention
The present invention proposes zirconia ceramics top layer at stabilized with yttrium oxide; The mode that applies through physics coats zirconium oxide, hydroxyapatite two component pulp layers and zirconium oxide, hydroxyapatite, magnesium phosphate three component pulp layers successively, the zirconia base composite that preparation has higher mechanical property, good biocompatibility and induction of bone growth ability.Through the zirconic addition of adjustment internal layer, increase the bending strength and the fracture toughness of material, adjust the addition of outer hydroxyapatite, magnesium phosphate, improve the bone growth inducing ability of material.
A kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite is characterized in that: this composite can be used for the incomplete reparation of human body bone, and gross thickness is 3mm-4.5mm, and being divided into is three layers, and internal layer is a zirconia ceramic layer; The middle level is zirconium oxide, hydroxyapatite composite bed; Skin is zirconium oxide, hydroxyapatite, magnesium phosphate composite bed.Wherein, internal layer zirconia ceramics layer thickness is 1.5mm-2.5mm, is main stress layer, can carry impulsive force that bone bore in pressure and the motion of human upper limb body; The thickness of middle level zirconium oxide, hydroxyapatite composite bed is 0.4mm-0.5mm, is tack coat, and that wherein contain and inside and outside two-layer identical composition can be combined closely in sintering process each other, improves the adhesion of composite interlayer; Outer oxide zirconium, hydroxyapatite, magnesium phosphate composite bed thickness are 0.4mm-0.5mm; Be the bone inducing layer; Fusion and decomposition appears in the magnesium phosphate that wherein contains when being higher than 1300 ℃; At the outer pore that forms of composite, can induce the soft or hard tissue at interface to grow in the hole state of formation fibrous tissue and freshman bone tissue's cross coupled.
Above-mentioned a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite; The internal layer zirconia ceramic layer is that the Zirconium powder with the 2-8mol% stabilized with yttrium oxide is a raw material, ball milling 3h-48h then, and ball milling is after dried obtains powder body; Adopt dry-pressing or slip casting to obtain base substrate; Handle through the 100MPa-300MPa isostatic cool pressing and obtain green compact, green compact carried out sintering in 1-80 hour 1500 ℃-1700 ℃ insulations, naturally cooled to room temperature and obtained the internal layer zirconia ceramic layer.Middle level zirconium oxide, hydroxyapatite composite bed are raw material with Zirconium powder, hydroxy apatite powder, the high polymer binder of 2-8mol% stabilized with yttrium oxide mainly; Prepare burden according to 55wt.%-85wt.% Zirconium powder, 10wt.%-40wt.% hydroxy apatite powder, 1wt.%-5wt.% high polymer binder; Ball milling 3h-48h obtains coating paste then; This slurry is coated on internal layer zirconia ceramics surface equably; 1000 ℃-1600 ℃ insulations 1-80 hour, naturally cool to room temperature then, obtain the single treatment composite ceramic material.Outer oxide zirconium, hydroxyapatite, magnesium phosphate composite bed are to prepare burden with 40wt.%-60wt.% zirconium oxide, 20wt.%-30wt.% hydroxyapatite, 20wt.%-30wt.% magnesium phosphate, 1wt.%-5wt.% high polymer binder; Ball milling 3h-48h obtains coating paste then; This slurry is coated on above-mentioned single treatment composite ceramics surface equably; Then 1000 ℃-1600 ℃ insulations 1-80 hour; Naturally cool to room temperature, obtain final zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite.
In above-mentioned a kind of zirconium oxide, hydroxyapatite and the magnesium phosphate laminar composite; Described magnesium phosphate powder body is to be raw material (it is pure to be chemical analysis) with phosphoric acid and light magnesium carbonate; Prepare burden according to stoichiometric proportion; Both are added water to mix after drying fully, 1100 ℃-1350 ℃ synthetic the obtaining of insulation 30min-180min.
In above-mentioned a kind of zirconium oxide, hydroxyapatite and the magnesium phosphate laminar composite, described high polymer binder is: one or more in polyethylene, polypropylene, the polystyrene.
The zirconium oxide, hydroxyapatite and the magnesium phosphate laminar composite biocompatibility that adopt the present invention to prepare are good, and the induced osteogenesis effect is remarkable, and the mechanical property bending strength is up to 480MPa, and fracture toughness reaches as high as 6.1MPam
1/2, can be used for the bone defect repair, potential applicability in clinical practice is wide.
Description of drawings
Shown in Figure 1 is a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite sectional view.
The specific embodiment
Embodiment 1:
Use analytically pure H
3PO
4, 4MgCO
3Mg (OH)
2XH
2O presses Mg as experimental raw
3(PO
4)
2The stoichiometric proportion design is prepared burden, and both is added water to mix after drying fully, and after 1100 ℃ of insulation 45min were synthetic, the powder body pulverizing and jevigating with after synthetic obtained the magnesium phosphate powder body.
With the Mg for preparing
3(PO
4)
2Powder body, 3mol%Y
2O
3Stable ZrO
2Powder body, Ca10 (PO
4)
6(OH)
2Powder body, polyethylene are raw material, prepare a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite according to following method.
With 3mol%Y
2O
3Stable ZrO
2Powder body ball milling 12h obtains powder body through dried, adopts dry-pressing or slip casting to obtain base substrate; Handle through the 100MPa isostatic cool pressing and obtain green compact, green compact carry out sintering at 1550 ℃ of insulation 3h, naturally cool to room temperature; Obtain the internal layer zirconia ceramic layer, its thickness is 2.5mm.
With 35wt.%Ca
10(PO
4)
6(OH)
2Powder body, 60wt.%, 3mol%Y
2O
3Stable ZrO
2Powder body, 5wt.% polyethylene ball milling 12h obtain coating paste, and this slurry is coated on internal layer zirconia ceramics surface equably, at 1400 ℃ of insulation 3h, naturally cool to room temperature then, obtain the single treatment composite ceramic material.Wherein, the thickness of middle level hydroxyapatite, zirconia layer is 0.4mm.
With 20wt.%Mg
3(PO
4)
2Powder body, 15wt.%Ca
10(PO
4)
6(OH)
2Powder body, 60wt.%, 3mol%Y
2O
3Stable ZrO
2Powder body, 5wt.% polyethylene ball milling 12h obtain coating paste; This slurry is coated on above-mentioned single treatment composite ceramics surface equably; At 1300 ℃ of insulation 3h, naturally cool to room temperature then, obtain zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite.Wherein, the thickness of outer magnesium phosphate, hydroxyapatite and zirconia layer is 0.4mm, and the composite ceramic material gross thickness is 4.1mm.
The main performance index of made zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite is bending strength 436MPa, and fracture toughness reaches as high as 5.6MPam
1/2, satisfy the material requirements of bone defect repair.
Embodiment 2:
Use analytically pure H
3PO
4, 4MgCO
3Mg (OH)
2XH
2O presses Mg as experimental raw
3(PO
4)
2The stoichiometric proportion design is prepared burden, and both is added water to mix after drying fully, and after 1200 ℃ of insulation 90min were synthetic, the powder body pulverizing and jevigating with after synthetic obtained the magnesium phosphate powder body.
With the Mg for preparing
3(PO
4)
2Powder body, 3mol%Y
2O
3Stable ZrO
2Powder body, Ca10 (PO
4)
6(OH)
2Powder body, polypropylene are raw material, prepare a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite according to following method.
With 3mol%Y
2O
3Stable ZrO
2Powder body ball milling 24h obtains powder body through dried, adopts dry-pressing or slip casting to obtain base substrate; Handle through the 200MPa isostatic cool pressing and obtain green compact, green compact carry out sintering at 1550 ℃ of insulation 3h, naturally cool to room temperature; Obtain the internal layer zirconia ceramic layer, its thickness is 2.0mm.
With 30wt.%Ca
10(PO
4)
6(OH)
2Powder body, 67wt.%, 3mol%Y
2O
3Stable ZrO
2Powder body, 3wt.% polypropylene ball milling 24h obtain coating paste, and this slurry is coated on internal layer zirconia ceramics surface equably, at 1500 ℃ of insulation 3h, naturally cool to room temperature then, obtain the single treatment composite ceramic material.Wherein, the thickness of middle level hydroxyapatite, zirconia layer is 0.42mm.
With 25wt.%Mg
3(PO
4)
2Powder body, 22wt.%Ca
10(PO
4)
6(OH)
2Powder body, 50wt.%, 3mol%Y
2O
3Stable ZrO
2Powder body, 3wt.% polyethylene ball milling 24h obtain coating paste; This slurry is coated on above-mentioned single treatment composite ceramics surface equably; At 1400 ℃ of insulation 3h, naturally cool to room temperature then, obtain zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite.Wherein, the thickness of outer magnesium phosphate, hydroxyapatite and zirconia layer is 0.45mm, and the composite ceramic material gross thickness is 3.74mm.
The main performance index of made zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite is bending strength 480MPa, and fracture toughness reaches as high as 6.1MPam
1/2, satisfy the material requirements of bone defect repair.
Embodiment 3:
Use analytically pure H
3PO
4, 4MgCO
3Mg (OH)
2XH
2O presses Mg as experimental raw
3(PO
4)
2The stoichiometric proportion design is prepared burden, and both is added water to mix after drying fully, and after 1300 ℃ of insulation 60min were synthetic, the powder body pulverizing and jevigating with after synthetic obtained the magnesium phosphate powder body.
With the Mg for preparing
3(PO
4)
2Powder body, 3mol%Y
2O
3Stable ZrO
2Powder body, Ca
10(PO
4)
6(OH)
2Powder body, polystyrene are raw material, prepare a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite according to following method.
With 3mol%Y
2O
3Stable ZrO
2Powder body ball milling 48h obtains powder body through dried, adopts dry-pressing or slip casting to obtain base substrate; Handle through the 300MPa isostatic cool pressing and obtain green compact, green compact carry out sintering at 1600 ℃ of insulation 3h, naturally cool to room temperature; Obtain the internal layer zirconia ceramic layer, its thickness is 2.2mm.
With 40wt.%Ca
10(PO
4)
6(OH)
2Powder body, 56wt.%, 3mol%Y
2O
3Stable ZrO
2Powder body, 4wt.% polystyrene ball milling 48h obtain coating paste, and this slurry is coated on internal layer zirconia ceramics surface equably, at 1500 ℃ of insulation 3h, naturally cool to room temperature then, obtain the single treatment composite ceramic material.Wherein, the thickness of middle level hydroxyapatite, zirconia layer is 0.43mm.
With 30wt.%Mg
3(PO
4)
2Powder body, 25wt.%Ca
10(PO
4)
6(OH)
2Powder body, 41wt.%, 3mol%Y
2O
3Stable ZrO
2Powder body, 4wt.% polyethylene ball milling 48h obtain coating paste; This slurry is coated on above-mentioned single treatment composite ceramics surface equably; At 1500 ℃ of insulation 3h, naturally cool to room temperature then, obtain a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite.Wherein, the thickness of outer magnesium phosphate, hydroxyapatite and zirconia layer is 0.42mm, and the composite ceramic material gross thickness is 3.90mm.
The main performance index of made zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite is bending strength 465MPa, and fracture toughness reaches as high as 5.8MPam
1/2, satisfy the material requirements of bone defect repair.
Claims (7)
1. a zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite is characterized in that: this composite is used for that the human body bone is incomplete to be repaired, and gross thickness is 3mm-4.5mm, and being divided into is three layers, and internal layer is a zirconia ceramic layer; The middle level is zirconium oxide, hydroxyapatite composite bed; Skin is zirconium oxide, hydroxyapatite, magnesium phosphate composite bed.
2. according to claims 1 described a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite; It is characterized in that: internal layer zirconia ceramics layer thickness is 1.5mm-2.5mm; Be main stress layer, can carry impulsive force that thigh bone bore in pressure and the motion of human upper limb body.
3. according to claims 1 described a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite; It is characterized in that: the thickness of middle level zirconium oxide, hydroxyapatite composite bed is 0.4mm-0.5mm; Be tack coat; That wherein contain and inside and outside two-layer identical composition can be combined closely in sintering process each other, improve the adhesion of composite interlayer.
4. according to claims 1 described a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite; It is characterized in that: outer oxide zirconium, hydroxyapatite, magnesium phosphate composite bed thickness are 0.4mm-0.5mm; Be the bone inducing layer, fusion and decomposition appears in the magnesium phosphate that wherein contains when being higher than 1300 ℃, at the outer pore that forms of composite; Can induce the soft or hard tissue at interface to grow in the hole, form the state of fibrous tissue and freshman bone tissue's cross coupled.
5. according to claims 1 described a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite; It is characterized in that: the method for preparing of internal layer zirconia ceramic layer is that the Zirconium powder with the 2-8mol% stabilized with yttrium oxide is a raw material; Ball milling 3h-48h then, ball milling adopt dry-pressing or slip casting to obtain base substrate after dried obtains powder body; Handle through the 100MPa-300MPa isostatic cool pressing again and obtain green compact; Green compact carried out sintering in 1-80 hour 1500 ℃-1700 ℃ insulations, naturally cooled to room temperature, obtained the internal layer zirconia ceramic layer.The method for preparing of middle level zirconium oxide, hydroxyapatite composite bed is to be raw material with the Zirconium powder of 2-8mol% stabilized with yttrium oxide, hydroxy apatite powder, high polymer binder; Prepare burden according to 55wt.%-85wt.% Zirconium powder, 10wt.%-40wt.% hydroxy apatite powder, 1wt.%-5wt.% high polymer binder; Ball milling 3h-48h obtains coating paste then; This slurry is coated on internal layer zirconia ceramics surface equably; 1000 ℃-1600 ℃ insulations 1-80 hour, naturally cool to room temperature then, obtain the single treatment composite ceramic material.The method for preparing of outer oxide zirconium, hydroxyapatite, magnesium phosphate composite bed is to prepare burden with 40wt.%-60wt.% zirconium oxide, 20wt.%-30wt.% hydroxyapatite, 20wt.%-30wt.% magnesium phosphate, 1wt.%-5wt.% high polymer binder; Ball milling 3h-48h obtains coating paste then; This slurry is coated on above-mentioned single treatment composite ceramics surface equably; Then 1000 ℃-1600 ℃ insulations 1-80 hour; Naturally cool to room temperature, obtain zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite.
6. according to claims 1 described a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite; It is characterized in that: described magnesium phosphate powder body is to be raw material with phosphoric acid and light magnesium carbonate (purity >=99%); According to stoichiometric proportion prepare burden, batch mixing, prepare at 1100 ℃-1350 ℃ insulation 30min-180min then.
7. according to claims 1 described a kind of zirconium oxide, hydroxyapatite and magnesium phosphate laminar composite, it is characterized in that: described high polymer binder is: one or more in polyvinyl alcohol, polypropylene, the polystyrene.
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| CN108295307A (en) * | 2018-03-02 | 2018-07-20 | 中国医科大学附属口腔医院 | A kind of bone implantation calcium phosphorous compound-magnesium composite coating and preparation method thereof |
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| CN104446505A (en) * | 2013-09-20 | 2015-03-25 | 阿尔斯通技术有限公司 | Method for producing means with thermal resist for applying at a surface of a heat exposed component |
| CN104446386A (en) * | 2014-11-10 | 2015-03-25 | 苏州维泰生物技术有限公司 | Aluminum oxide ceramic for hip joint and preparation method thereof |
| CN107324848B (en) * | 2017-07-21 | 2020-06-26 | 湖南中科光电有限公司 | Water-resistant zirconia ceramics protector and optical fiber ceramic ferrule |
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| CN108324579A (en) * | 2018-02-27 | 2018-07-27 | 苏州凌科特新材料有限公司 | A kind of teeth repairing material and preparation method thereof |
| CN108295307A (en) * | 2018-03-02 | 2018-07-20 | 中国医科大学附属口腔医院 | A kind of bone implantation calcium phosphorous compound-magnesium composite coating and preparation method thereof |
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| CN108727056B (en) * | 2018-06-28 | 2021-04-06 | 河南省肿瘤医院 | Preparation method of magnesium-doped hydroxyapatite-zirconia biological ceramic material |
| CN111533541A (en) * | 2019-06-12 | 2020-08-14 | 南京赛诺特斯材料科技有限公司 | Oral cavity repairing material based on nano zirconia and alumina composite ceramic |
| CN114315337A (en) * | 2020-12-30 | 2022-04-12 | 佛山仙湖实验室 | Ceramic material and preparation method thereof |
| CN114315337B (en) * | 2020-12-30 | 2023-09-15 | 佛山仙湖实验室 | Ceramic material and preparation method thereof |
| CN112778016A (en) * | 2020-12-31 | 2021-05-11 | 佛山仙湖实验室 | Dental ceramic material and preparation method and application thereof |
| CN112778016B (en) * | 2020-12-31 | 2023-11-21 | 佛山仙湖实验室 | Dental ceramic material and preparation method and application thereof |
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