CN100406069C - CaO-P2O5-NaO-TiO-Zro-biological glass ceramic and its production - Google Patents

CaO-P2O5-NaO-TiO-Zro-biological glass ceramic and its production Download PDF

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CN100406069C
CN100406069C CNB2005100472836A CN200510047283A CN100406069C CN 100406069 C CN100406069 C CN 100406069C CN B2005100472836 A CNB2005100472836 A CN B2005100472836A CN 200510047283 A CN200510047283 A CN 200510047283A CN 100406069 C CN100406069 C CN 100406069C
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李述军
郑彩云
郝玉琳
杨锐
郭正晓
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Institute of Metal Research of CAS
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/16—Silica-free oxide glass compositions containing phosphorus
    • C03C3/21—Silica-free oxide glass compositions containing phosphorus containing titanium, zirconium, vanadium, tungsten or molybdenum
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00—Compositions for glass with special properties
    • C03C4/0007—Compositions for glass with special properties for biologically-compatible glass

Abstract

A biologic glass ceramic CaO-P2O5-Na2O-TiO2-ZrO2 is proportionally prepared from CaO and P2O5 (80-90 mol%), Na2O (4-7), and TiO2 and ZrO2 (rest) through proportional mixing, drying, heating for smelting, pouring on stainless steel plate, punching to obtain glass balls, grinding, cold pressing and sintering. It can be used as the substitute of human hard tissue. Its advantages are no SiO2 and toxic elements, high bioactivity and biologic compatibility, and high strength and machinability.

Description

A kind of CaO-P 2O 5-Na 2O-TiO 2-ZrO 2Biological glass ceramic and preparation method thereof
Technical field:
The present invention relates to the glass ceramics field, particularly relate to the CaO-P that clinical medicine is used with high strength and high bioactivity 2O 5-Na 2O-TiO 2-ZrO 2Biological glass ceramic and preparation method thereof.
Background technology:
Human body hard tissue reparation and reconstruction biomaterials be in the biomedical material development the earliest, the most sophisticated field.Up to now, the material that is used for hard tissue repair and replacement has skeleton derivant of Metal and Alloy, biological glass ceramic, polymer, composite and humans and animals etc., document [1]: Yu Yaoting sees reference. bio-medical material. and Tianjin: publishing house of University Of Tianjin, 2000:116.Biological active glass ceramic be a class can with the biomaterial of biologic soft tissue or osseous tissue bonding, have the incomparable advantage of metal, macromolecule and bio-inert material.Therefore, people have produced keen interest to this class new material, and develop multiple biological active glass ceramic, for example:
Figure C20051004728300031
Bio-vitric (Na 2O-CaO-SiO 2-P 2O 5System), Ceravital devitrified glass (Na 2O-K 2O-MgO-CaO-P 2O5-SiO 2System), A-W biological glass ceramic (MgO-CaO-SiO 2-P 2O 5System), (HA consists of the hydroxyapatite bioactive pottery: Ca 10(PO 4) 6(OH) 2) or the like, the document that sees reference [2] and [3], list of references [2]: Larry L.Hench.Bioceramics.J.Am.Ceram.Soc.1998,81[7]: 1705-1728; List of references [3]: Yang Weizhong, Zhou Dali, Yin Guangfu and Zheng Changqiong. the magazine .2003 of biomedical engineering, 20 (3): 541-545.Compare with other bio-inert material, biological glass ceramic has better biocompatibility, higher bone bond strength and osteogenic ability faster, the document that sees reference [4]: Li Yubao. biomedical material. and Beijing: Chemical Industry Press, 2003:82.But most of bioactivity glass all contain a large amount of SiO 2And Nagase et al. finds mouse death when experiment mouse lumbar injection contains the normal saline of titanium dioxide silico-calcium phosphorus glass, then do not show toxicity when not containing silicon dioxide, document [5] sees reference: Nagase M, Abe Y, Chigira M and Udagawa E.Toxicity of silica-containing calciumposphate glasses demonstrated in mice.Biomaterials.1992,13:172-175.
Biological glass ceramic is finished by bone conduction passage as bone alternate material clinically.Because its excellent biological compatibility does not cause significant reaction behind the implanting to human body, host's callus can be converged by the face of creeping around the implant, and with the implant parcel, makes it to play the filling effect damaged with being connected bone.But its lower toughness has limited applying of it.Zirconia ceramics is a kind of very important structural ceramics that is only second to aluminium oxide that newly-developed gets up.Because its superperformance, thereby more and more is subject to people's attention the document that sees reference [6]: Liu Weiliang as high rigidity, high strength and higher fracture toughness. advanced ceramics technology. Wuhan: the .2004:176-180 of publishing house of Wuhan University of Technology.Zirconium oxide joins in the glass ceramics as the nucleus agent very early.In the glass composition, add the zirconium oxide microgranule, can make glass fracture strength bring up to 3MPa from 2MPa, document [7] sees reference: Tang Jiwen, Zhang Yude and Liu Chunmei. the progress of bio-active devitroceram artificial material. and Shandong medicine .1997,37[5]: 45-50.CaO-P 2O 5Series vitro-ceramic is a kind of new bio glass ceramics that newly-developed gets up, this be the pottery composition and body bone tissue approaching, has good biological activity and nontoxic, document [8] sees reference: Kasuga T and Abe Y.Calcium phosphate invert glasses with soda andtitania.J.Non-cryst.Solids.1999,243:70-74.The present invention is at CaO-P 2O 5On the series vitro-ceramic basis, introduce ZrO 2, form CaO-P 2O 5-Na 2O-TiO 2-ZrO 2Series vitro-ceramic.It is a kind of SiO that do not contain 2Bio-vitric, have higher Ca/P than and the composition similar with human body hard tissue, have higher fracture strength and biological activity, be more suitable for doing the human body embedded material.
Summary of the invention
The purpose of this invention is to provide a kind of novel C aO-P 2O 5-Na 2O-TiO 2-ZrO 2Biological glass ceramic and preparation method thereof.This glass ceramics has good biological activity, higher hardness, intensity and machinability, has the composition similar with human body hard tissue, can be used as human body hard tissue and substitutes and repair materials.
Technical scheme of the present invention is:
The invention provides a kind of CaO-P 2O 5-Na 2O-TiO 2-ZrO 2Biological glass ceramic, CaO and P 2O 5Total content is at 80～90mol%, Na 2The content of O is at 4～7mol%, and all the other are TiO 2And ZrO 2
CaO-P provided by the invention 2O 5-Na 2O-TiO 2-ZrO 2Biological glass ceramic, in the described glass ceramics, Ca and P mol ratio are 0.5～1.5.
CaO-P provided by the invention 2O 5-Na 2O-TiO 2-ZrO 2Biological glass ceramic, in the described glass ceramics, ZrO 2Content at 0.5～10mol%.
CaO-P provided by the invention 2O 5-Na 2O-TiO 2-ZrO 2The preparation method of biological glass ceramic comprises the preparation of glass and the preparation of pottery, and concrete steps are as follows:
(1) preparation of glass
With CaCO 3, Na 2CO 3, TiO 2, ZrO 2And H 3PO 4Be raw material, with the raw material mix homogeneously, the formulate glass serosity is smashed heating and melting after drying to pieces by described composition, takes out then and is poured on punching press on the stainless-steel sheet;
(2) Tao Ci preparation
After punching press gained glass bead worn into powder, cold pressing in bulk and sintering.
In the described step 1, glass pulp is smashed to pieces after drying, and the granularity of smashing the back powder to pieces is 5～10 μ m.
In the described step 1, in 1300～1400 ℃ of following heating and meltings, temperature retention time after 0.5～1 hour, take out immediately and be poured on that punching press gets glass on the stainless-steel sheet.
In the described step 2, the glass bead of punching press gained is worn into powder, the granularity of powder is 1～10 μ m.
In the described step 2, the pressure of colding pressing is 80～150MPa, and the glass dust sintering temperature is 800～850 ℃, and the time is 1～2/ hour.
CaO-P provided by the invention 2O 5-Na 2O-TiO 2-ZrO 2The preparation method of biological glass ceramic, described glass is raw materials used to be chemical reagent: CaCO 3, Na 2CO 3, TiO 2, ZrO 2And H 3PO 4(liquid, percentage by weight are 85%) is analytical pure.
CaO-P provided by the invention 2O 5-Na 2O-TiO 2-ZrO 2The preparation method of biological glass ceramic, soaking 4-7 days surfaces in simulated body fluid has the hydroxyapatite of even compact to generate the surface activity height.
CaO-P provided by the invention 2O 5-Na 2O-TiO 2-ZrO 2The preparation method of biological glass ceramic, prepared ceramic bending strength is better than greater than 90MPa
Figure C20051004728300051
Bio-vitric.
CaO-P provided by the invention 2O 5-Na 2O-TiO 2-ZrO 2Series vitro-ceramic has good biological activity, and soaking 4-7 days rear surfaces in simulated body fluid (SBF) has hydroxyapatite to generate.Biological activity that it is good and mechanical property not only can be used as tooth, maxillofacial bone and middle otica and also can be used as medical materials such as artificial vertebral body, intervertebral disc and crista iliaca.
The invention has the beneficial effects as follows:
Glass ceramics of the present invention does not contain SiO 2, there is not poisonous element, have good biological activity, soaking in simulated body fluid had the fine and close uniform hydroxylapatite of one deck to generate in 4 days; Have higher-strength (greater than 90MPa), can cut, be convenient to processing; Have higher Ca/P ratio and the composition similar, can be used as human body hard tissue and substitute and repair materials with human body hard tissue.This biological glass ceramic has the general character of biological glass ceramic, compares with metal implant to be expected to obtain the bone bond strength of osteogenic ability and Geng Gao faster.
Description of drawings:
The quick punching press gained of Fig. 1 CaO-P 2O 5-Na 2O-TiO 2-ZrO 2Glass;
The quick punching press gained of Fig. 2 60CaO30P 2O 54Na 2O3TiO 23ZrO 2Glass is shape appearance figure after the 1000# sand papering;
Figure 36 0CaO30P 2O 54Na 2O3TiO 23ZrO 2Glass soaks the shape appearance figure after 4 days in simulated body fluid;
Figure 46 0CaO30P 2O 54Na 2O3TiO 23ZrO 2Glass soaks the enlarged photograph of the shape appearance figure after 4 days in simulated body fluid;
Figure 56 0CaO30P 2O 55Na 2O3TiO 22ZrO 2Glass soaks the shape appearance figure after 7 days in simulated body fluid;
Figure 66 0CaO30P 2O 55Na 2O3TiO 22ZrO 2Soak the X-ray diffracting spectrum after 7 days in the glass simulated body fluid;
Fig. 7 CaO-P 2O 5-Na 2O-TiO 2-ZrO 2Glass is pulverized cold-rolled sintered back gained glass ceramics;
Figure 86 0CaO30P 2O 55Na 2O3TiO 22ZrO 2The composition diffracting spectrum of glass ceramics;
Figure 96 0CaO30P 2O 54Na 2O3TiO 23ZrO 2Glass ceramics is soaked the shape appearance figure after 7 days in simulated body fluid.
The specific embodiment:
Embodiment 1
Use analytical pure CaCO 3, Na 2CO 3, TiO 2, ZrO 2And H 3PO 4(85%) presses the described composition glass pulp of table 1 for preparation of raw material, with the raw material mix homogeneously, place 50 ℃ of drying baker inner drying 24h then with electric blender.Raw material after the drying is smash powdered (granularity is 5-10 μ m) place the inherent 1350 ℃ of insulation 0.5h of platinum crucible, taking-up immediately is poured on the stainless-steel sheet and quick punching press promptly gets glass.Gained glass macro morphology is seen Fig. 1.
Table 1CaO-P 2O 5-Na 2O-TiO 2-ZrO 2The glass composition
Figure C20051004728300061
Embodiment 2
With punching press gained 60CaO30P 2O 54Na 2O3TiO 23ZrO 237 ℃ of immersions are after 4 days in simulated body fluid (table 2) for glass, and the surface has the fine and close uniform hydroxylapatite of one deck to generate.Microscopic appearance soaked the back microscopic appearance as shown in Figure 3, Figure 4 as shown in Figure 2 before it soaked.
Ion concentration (mM) in blood plasma in table 2 human body and the simulated body fluid (SBF)
Figure C20051004728300071
Embodiment 3
With punching press gained 60CaO30P 2O 55Na 2O3TiO 22ZrO 2Glass soaked in 37 ℃ of simulated body fluids (table 2) after 7 days, and the surface has the fine and close uniform hydroxylapatite of one deck to generate.Soak the back microscopic appearance as shown in Figure 5, its X-ray diffracting spectrum as shown in Figure 6.
Embodiment 4
Punching press gained glass is cold-pressed into 40 * 9 * 6mm sample after ball mill is pulverized, the pressure of colding pressing is 100MPa, heats up with stove with 10 ℃/min speed, at 850 ℃ of insulation 1h, furnace cooling.Gained pottery macro morphology as shown in Figure 7, its composition is mainly β-Ca 3(PO 4) 2And β-Ca 2P 2O 7(as Fig. 8).
Embodiment 5
With punching press gained 60CaO30P 2O 55Na 2O3TiO 22ZrO 237 ℃ of immersions are after 7 days in simulated body fluid (table 2) for glass ceramics, and the surface has the fine and close uniform hydroxylapatite of one deck to generate.Soak the back microscopic appearance as shown in Figure 9.
Embodiment 6
Punching press gained glass is colded pressing after ball mill is pulverized and sintering gained pottery carries out the three-point bending experiment, and test result shows CaO-P 2O 5-Na 2O-TiO 2-ZrO 2The bending strength of series vitro-ceramic is greater than 90MPa, and its performance is better than
Figure C20051004728300072
Bio-vitric.
Embodiment 7
Use analytical pure CaCO 3, Na 2CO 3, TiO 2, ZrO 2And H 3PO 4(liquid, percentage by weight are 85%) presses the described composition glass pulp of table 1 for preparation of raw material, with the raw material mix homogeneously, places 50 ℃ of drying baker inner drying 24h with electric blender then.Raw material after the drying is smash powdered (granularity is 5-10 μ m) place the inherent 1300 ℃ of insulation 1h of platinum crucible, taking-up immediately is poured on the stainless-steel sheet and quick punching press promptly gets glass.
Table 3CaO-P 2O 5-Na 2O-TiO 2-ZrO 2The glass composition
Figure C20051004728300081
Punching press gained glass soaked 7 days in 37 ℃ of simulated body fluids (table 2) after, the surface has the fine and close uniform hydroxylapatite of one deck to generate the surface activity height.
Punching press gained glass is cold-pressed into 40 * 9 * 6mm sample with 150MPa pressure after ball mill is pulverized, heats up with stove with 10 ℃/min speed then, at 800 ℃ of insulation 2h, furnace cooling.Gained pottery macro morphology, its composition is mainly β-Ca 3(PO 4) 2And β-Ca 2P 2O 7
With punching press gained glass ceramics in simulated body fluid (table 2) 37 ℃ soak 7 days after, the surface has the fine and close uniform hydroxylapatite of one deck to generate, and biological activity that it is good and mechanical property not only can be used as tooth, maxillofacial bone and middle otica and also can be used as medical materials such as artificial vertebral body, intervertebral disc and crista iliaca.
Embodiment 8
Use analytical pure CaCO 3, Na 2CO 3, TiO 2, ZrO 2And H 3PO 4(liquid, percentage by weight are 85%) presses the described composition glass pulp of table 1 for preparation of raw material, with the raw material mix homogeneously, places 50 ℃ of drying baker inner drying 24h with electric blender then.Raw material after the drying is smash powdered (granularity is 5-10 μ m) place the inherent 1400 ℃ of insulation 0.8h of platinum crucible, taking-up immediately is poured on the stainless-steel sheet and quick punching press promptly gets glass.
Table 4CaO-P 2O 5-Na 2O-TiO 2-ZrO 2The glass composition
Punching press gained glass soaked 7 days in 37 ℃ of simulated body fluids (table 2) after, the surface has the fine and close uniform hydroxylapatite of one deck to generate the surface activity height.
Punching press gained glass is cold-pressed into 40 * 9 * 6mm sample with 80MPa pressure after ball mill is pulverized, heats up with stove with 10 ℃/min speed then, at 800 ℃ of insulation 2h, furnace cooling.Gained pottery macro morphology, its composition is mainly β-Ca 3(PO 4) 2And β-Ca 2P 2O 7
With punching press gained glass ceramics in simulated body fluid (table 2) 37 ℃ soak 7 days after, the surface has the fine and close uniform hydroxylapatite of one deck to generate, and biological activity that it is good and mechanical property not only can be used as tooth, maxillofacial bone and middle otica and also can be used as medical materials such as artificial vertebral body, intervertebral disc and crista iliaca.

Claims (8)

1. CaO-P 2O 5-Na 2O-TiO 2-ZrO 2Biological glass ceramic is characterized in that: CaO and P 2O 5Total content is at 80～90mol%, Na 2The content of O is at 4～7mol%, and all the other are TiO 2And ZrO 2
2. according to the described CaO-P of claim 1 2O 5-Na 2O-TiO 2-ZrO 2Biological glass ceramic is characterized in that: in the described glass ceramics, Ca and P mol ratio are 0.5～1.5.
3. according to the described CaO-P of claim 1 2O 5-Na 2O-TiO 2-ZrO 2Biological glass ceramic is characterized in that: in the described glass ceramics, and ZrO 2Content at 0.5～10mol%.
4. according to the described CaO-P of claim 1 2O 5-Na 2O-TiO 2-ZrO 2The preparation method of biological glass ceramic is characterized in that comprising the preparation of glass and the preparation of pottery, and concrete steps are as follows:
(1) preparation of glass
With CaCO 3, Na 2CO 3, TiO 2, ZrO 2And H 3PO 4Be raw material, with the raw material mix homogeneously, the formulate glass serosity is smashed heating and melting after drying to pieces by the described composition of claim 1, takes out then and is poured on punching press on the stainless-steel sheet;
(2) Tao Ci preparation
After punching press gained glass bead worn into powder, cold pressing in bulk and sintering.
5. according to the described CaO-P of claim 4 2O 5-Na 2O-TiO 2-ZrO 2The preparation method of biological glass ceramic is characterized in that: in the described step 1, glass pulp is smashed to pieces after drying, and the granularity of smashing the back powder to pieces is 5～10 μ m.
6. according to the described CaO-P of claim 4 2O 5-Na 2O-TiO 2-ZrO 2The preparation method of biological glass ceramic is characterized in that: in the described step 1, in 1300～1400 ℃ of following heating and meltings, temperature retention time after 0.5～1 hour, take out immediately and be poured on that punching press gets glass on the stainless-steel sheet.
7. according to the described CaO-P of claim 4 2O 5-Na 2O-TiO 2-ZrO 2The preparation method of biological glass ceramic is characterized in that: in the described step 2, the glass bead of punching press gained is worn into powder, the granularity of powder is 1～10 μ m.
8. according to the described CaO-P of claim 4 2O 5-Na 2O-TiO 2-ZrO 2The preparation method of biological glass ceramic is characterized in that: in the described step 2, the pressure of colding pressing is 80～150MPa, and the glass dust sintering temperature is 800～850 ℃, and the time is 1～2 hour.
CNB2005100472836A 2005-09-28 2005-09-28 CaO-P2O5-NaO-TiO-Zro-biological glass ceramic and its production Expired - Fee Related CN100406069C (en)

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CN101618230B (en) * 2008-07-01 2013-03-27 叶南辉 Method for manufacturing biomedical glass ceramic material
CN103626396A (en) * 2013-12-13 2014-03-12 天津工业大学 Preparation method of titanium-containing mesoporous bioglass
CN104803673B (en) * 2015-03-31 2017-03-08 佛山市三水宝力高无机材料有限公司 A kind of hydroxyapatite/Ti acid sodium composite boilogical ceramic and preparation method thereof
CN110418771B (en) * 2017-03-16 2022-07-26 尼拉伊贾扬特·拉克加 Preparation of porous glass and glass ceramic particle structure by gel casting
CN109574507B (en) * 2019-01-21 2022-07-05 河南理工大学 Nano-scale spherical bioactive glass and preparation method thereof

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GB2199028A (en) * 1986-05-21 1988-06-29 Univ Sheffield Glass ceramics
US5196381A (en) * 1990-01-16 1993-03-23 E. I. Du Pont De Nemours And Company Metaphosphate glass composition
US5618763A (en) * 1994-08-01 1997-04-08 Ivoclar Ag Alkali-zinc-silicate glass-ceramics and glasses
US6130178A (en) * 1998-04-16 2000-10-10 Corning Incorporated Strong miserite glass-ceramics

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GB2199028A (en) * 1986-05-21 1988-06-29 Univ Sheffield Glass ceramics
US5196381A (en) * 1990-01-16 1993-03-23 E. I. Du Pont De Nemours And Company Metaphosphate glass composition
US5618763A (en) * 1994-08-01 1997-04-08 Ivoclar Ag Alkali-zinc-silicate glass-ceramics and glasses
US6130178A (en) * 1998-04-16 2000-10-10 Corning Incorporated Strong miserite glass-ceramics

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