CN100345794C - Method for synthesizing akermanite powder by two-step deposition - Google Patents
Method for synthesizing akermanite powder by two-step deposition Download PDFInfo
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- CN100345794C CN100345794C CNB2004100540824A CN200410054082A CN100345794C CN 100345794 C CN100345794 C CN 100345794C CN B2004100540824 A CNB2004100540824 A CN B2004100540824A CN 200410054082 A CN200410054082 A CN 200410054082A CN 100345794 C CN100345794 C CN 100345794C
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Abstract
The present invention relates to a method for synthesizing akermanite powder by two-step deposition, which is characterized in that Na2SiO3.9H2O, Ca(NO3)2.4H2O, Mg(NO3)2.6H2O, and NH3. H2O are used as raw materials. The method for synthesizing akermanite powder by two-step deposition comprises the following steps that firstly, sodium silicate reacts with calcium nitrate so as to obtain calcium silicate suspension, and ammonia water is used for regulating the pH value of the suspension so that the magnesium hydroxide is precipitated; secondly, the mixed precipitation object of calcium silicate and magnesium hydroxide obtained from the former two precipitation steps is calcined at 1200DEGC so that pure akermanite powder can be obtained. The particle diameter of the akermanite powder produced according to the method is approximate to 0.5 to 5 mum, and the distribution of akermanite powder is uniform. The synthesized akermanite powder has favorable capacity of inducing hydroxyapatite in simulated body fluid.
Description
Technical field
The present invention relates to the akermanite (Ca of the synthetic biologically active of a kind of two-step precipitation
2MgSi
2O
7) method of powder, belong to technical field of biological material.
Background technology
The wollastonite ceramics that contains Ca and Si is as the more existing bibliographical informations of biomaterial.Its outstanding feature is exactly that it has and good induces hydroxyapatite to form and the ability of the propagation of stimulating osteoblast, has embodied biological activity preferably.And, mussite (CaMgSi
2O
6), this pottery that contains the ternary component of Ca, Mg and Si can be induced the formation of hydroxyapatite in simulated body fluid, implant in the rabbit bone and can form synostosis [(1) Miake Y with host bone, Yanagisawa T, Yajima Y, et al.JDent Res, 1995,74:1756-1763. (2) Nonami T, Tsutsumi S.J Mater SciM, 1999,10:475-479.].And akermanite is as a kind of material that contains the ternary component of Ca, Mg and Si, is similar to mussite on forming, and therefore explores akermanite and has certain meaning as the research of biomaterial with using.
In recent years, various wet chemical methods such as sol-gel method, hydrothermal method and coprecipitation method etc. have obtained using widely in the preparation ceramic powder material.But the ceramic powder material for forming complicated ternary component is difficult to obtain highly purified product with general method.Some ternary component ceramic powder of forming more complicated is a kind of simple and feasible method and the two-step precipitation method is for preparation.
Akermanite is exactly the material of the ternary composition of a kind of Ca of containing, Mg and Si, previous studies show that by sol-gel method synthetic akermanite powder needs very high calcining temperature, and the powder granularity that is synthesized is big, serious, inhomogeneous [the Wu C T of size-grade distribution reunite, Chang J.Mater Lett, 2004,58:2415-2417.].Therefore, attempt using the synthetic granularity of two-step precipitation method little, finely dispersed akermanite powder, application has very strong Practical significance as biomaterial to the akermanite powder.
Summary of the invention
The objective of the invention is to synthesize the akermanite powder of forming more complicated by the two-step precipitation method.And have lower calcining temperature with respect to the akermanite that sol-gel method synthesizes, and particle diameter is littler, and size distribution is advantage of uniform more.This is next step densified sintering product, and having highly active akermanite pottery provides better condition.Simultaneously, two-step precipitation method cost is relatively low, is easy to be extended and applied.
Embodiment of the present invention is summarized as follows:
(1) adopts analytical pure Ca (NO
3)
24H
2The ca nitrate soln of O (calcium nitrate tetrahydrate) preparation 0.05-0.1M, and be 12-13 with the pH value of dropping ammonia regulator solution.Same method adopts analytical pure Na
2SiO
39H
2The sodium silicate solution 100ml of O (nine hydrated sodium silicates) preparation 0.05-0.1M, and be 13.0 with the pH value of dropping ammonia method regulator solution.Then sodium silicate solution is contained in funnel, slowly be added drop-wise in the ca nitrate soln, vigorous stirring is 12-24 hour simultaneously, generates Calucium Silicate powder suspension.
(2) adopt analytical pure Mg (NO
3)
26H
2The magnesium nitrate solution of O (magnesium nitrate hexahydrate) preparation 0.05-0.1M, and pass through the slow dropping of funnel in the Calucium Silicate powder suspension that step (1) generates, vigorous stirring, dropping ammonia makes the pH value of whole system maintain 12.0 in suspension simultaneously.After dripping, sealed vessel fully stirred 6-12 hour, made it to generate the throw out that magnesium hydroxide and precipitated calcium silicate mix.
(3) magnesium hydroxide and precipitated calcium silicate mixing suspension are filtered, and be 12.0 ammonia soln cleaning with pH value, ethanol dehydration, in 60-80 ℃ dry 20-24 hour again, cleaning usually and dewatering respectively was three times.
(4) drying is good powder was calcined 2 hours in 1200 ℃, obtained pure akermanite powder.
Yet, the powder of preparation is XRD, sem analysis is got the powder that 0.3g makes, and is immersed in the 200ml simulated body fluid, takes out after 5 days, and dry powder is XRD, and sem analysis is to show effect of the present invention.
The akermanite powder purity height of the present invention's preparation, particle diameter is 0.5-5 μ m, and is uniformly dispersed.Simulated body fluid soaks thinks that tentatively the akermanite powder has good hydroxyapatite (HAP) formation ability, and the HAP that the surface generates has nanometer worm shape structure, is a kind of potential biological active materials.(seeing embodiment for details)
Description of drawings
In conjunction with the accompanying drawings to the detailed description that the present invention did, can understand content mentioned above by following better.Wherein,
Fig. 1 is a two-step precipitation method synthetic akermanite powder XRD figure.
Fig. 2 is two-step precipitation method synthetic akermanite powder SEM figure.
Fig. 3 is that the akermanite powder soaks the XRD figure after 5 days in simulated body fluid.
Fig. 4 is that the akermanite powder soaks the SEM figure after 5 days in simulated body fluid.
Embodiment
The invention will be further described below in conjunction with example, but they are not that the present invention is imposed any restrictions.
Example 1: raw materials used purity as mentioned above.
(1) the ca nitrate soln 100ml of preparation 0.1M, and be 12.0 with the pH value of ammoniacal liquor regulator solution.The sodium silicate solution 100ml of same method preparation 0.1M, and be 13.0 with the pH value of ammoniacal liquor regulator solution.Then sodium silicate solution is contained in funnel, slowly be added drop-wise in the ca nitrate soln, vigorous stirring is 12 hours simultaneously, generates Calucium Silicate powder suspension.
(2) the magnesium nitrate solution 50ml of preparation 0.1M, and pass through the slow dropping of funnel in Calucium Silicate powder suspension, vigorous stirring, dropping ammonia makes the pH value of whole system maintain 12.0 in suspension simultaneously.After dripping, sealed vessel fully stirred 6 hours, and magnesium hydroxide and precipitated calcium silicate are mixed.
(3) magnesium hydroxide and precipitated calcium silicate mixing suspension are filtered, and be that 12.0 ammonia soln cleans three times, ethanol dehydration three times, drying 24 hours in 60 ℃ again with pH value.
(4) drying is good powder was calcined 2 hours in 1200 ℃, obtained pure akermanite powder.Its XRD and SEM as depicted in figs. 1 and 2, the result of Fig. 1 shows and has generated pure akermanite phase that the result of Fig. 2 shows the particle diameter and the dispersiveness of two-step precipitation method synthetic akermanite powder.Fig. 3 shows after the akermanite powder that obtains soaks and has generated hydroxyapatite that the stereoscan photograph of Fig. 4 shows that the hydroxyapatite of generation has nanometer worm shape structure, illustrates that akermanite has the ability of good deposited hydroxyl apatite in simulated body fluid.
Example 2:
(1) the ca nitrate soln 100ml of preparation 0.05M, and be 13.0 with the pH value of ammoniacal liquor regulator solution.The sodium silicate solution 100ml of same method preparation 0.05M, and be 13.0 with the pH value of ammoniacal liquor regulator solution.Then sodium silicate solution is contained in funnel, slowly be added drop-wise in the ca nitrate soln, vigorous stirring is 24 hours simultaneously, generates Calucium Silicate powder suspension.
(2) the magnesium nitrate solution 50ml of preparation 0.05M, and pass through the slow dropping of funnel in Calucium Silicate powder suspension, vigorous stirring, dropping ammonia makes the pH value of whole system maintain 13.0 in suspension simultaneously.After dripping, sealed vessel fully stirred 12 hours, and magnesium hydroxide and precipitated calcium silicate are mixed.
(3) magnesium hydroxide and precipitated calcium silicate mixing suspension are filtered, and be that 13.0 ammonia soln cleans three times, ethanol dehydration three times, drying 20 hours in 80 ℃ again with pH value.
(4) drying is good powder was calcined 2 hours in 1200 ℃, obtained pure akermanite powder.
The XRD of prepared akermanite and SEM as depicted in figs. 1 and 2, soak after 5 days SEM as shown in Figure 4.
Claims (2)
1, the method for the synthetic akermanite powder of a kind of two-step precipitation is characterized in that concrete steps are:
(a) ca nitrate soln of elder generation's preparation 0.05-0.1M, dropping ammonia is regulated pH value 12.0-13.0; Prepare the sodium silicate solution of 0.05-0.1M again, it is 13.0 that dropping ammonia is regulated the pH value;
(b) then sodium silicate solution slowly is added drop-wise in the ca nitrate soln, stirred 12-24 hour, generate Calucium Silicate powder suspension;
(c) prepare the magnesium nitrate solution of 0.05-0.1M again, slowly be added drop-wise in the Calucium Silicate powder suspension that step (b) generates, dropping ammonia makes the pH value of whole system maintain 12.0 in suspension in the time of stirring;
(d) drip after, sealed vessel stirred 6-12 hour, made it to generate the uniform mixing throw out of magnesium hydroxide and Calucium Silicate powder;
(e) throw out of filtration step (d) gained, and be that 12.0 ammonia soln cleans three times with the pH value, ethanol dehydration three times, in 60-80 ℃ dry 20-24 hour again;
(f) drying back powder was 1200 ℃ of calcinings 2 hours;
Described nitrocalcite is analytical pure Ca (NO
3)
24H
2O;
Described SODIUMNITRATE is analytical pure Na
2SiO
39H
2O;
Described magnesium nitrate is analytical pure Mg (NO
3)
26H
2O.
2, by the method for the synthetic akermanite powder of the described two-step precipitation of claim 1, it is characterized in that synthetic akermanite particle diameter is 0.5-5 μ m.
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Families Citing this family (2)
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|---|---|---|---|---|
| CN100360191C (en) * | 2005-05-13 | 2008-01-09 | 中国科学院上海硅酸盐研究所 | Material of porous akermanite for support and its preparation process and application |
| CN103656747A (en) * | 2012-09-07 | 2014-03-26 | 中国科学院上海硅酸盐研究所 | Medical implant as well as preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5344456A (en) * | 1989-06-06 | 1994-09-06 | Tdk Corporation | Materials for living hard tissue replacements |
-
2004
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5344456A (en) * | 1989-06-06 | 1994-09-06 | Tdk Corporation | Materials for living hard tissue replacements |
| US5356436A (en) * | 1989-06-06 | 1994-10-18 | Tdk Corporation | Materials for living hard tissue replacements |
Non-Patent Citations (1)
| Title |
|---|
| 燃烧法快速合成新型蓝色硅酸盐长余辉材料 镠春燕等，中国陶瓷，第39卷第6期 2003 * |
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Owner name: KUNSHAN CHINESE TECHNOLOGY NEW MATERIALS CO., LTD. Free format text: FORMER OWNER: SHANGHAI SILICATES INSTITUTE, THE CHINESE ACADEMY OF SCIENCES Effective date: 20101122 |
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Free format text: CORRECT: ADDRESS; FROM: 200050 NO. 1295, DINGXI ROAD, SHANGHAI TO: 215311 NO. 311, SUHANG ROAD, BACHENG TOWN, KUNSHAN CITY, JIANGSU PROVINCE |
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Effective date of registration: 20101122 Address after: 215311 Jiangsu Province town Kunshan city Suzhou Road No. 311 Patentee after: KUNSHAN CHINESE TECHNOLOGY NEW MATERIALS Co.,Ltd. Address before: 1295 Dingxi Road, Shanghai, No. 200050 Patentee before: SHANGHAI INSTITUTE OF CERAMICS, CHINESE ACADEMY OF SCIENCES |
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