羟基磷灰石晶粒/粒子的水热控制合成
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摘要
羟基磷灰石,由于其独特的生物活性和生物相容性,使其成为一种重要的生物材料。为了拓广羟基磷灰石的研究价值和应用范围,制备具有多种形貌和不同空间结构的羟基磷灰石微纳米颗粒,成为生物材料领域研究的热点。论文通过对水热合成羟基磷灰石过程中的水热物化条件的控制、反应添加剂的添加以及聚合物模板的介入的研究,获得了不同形貌粒径的羟基磷灰石晶粒/粒子,以及空心结构的羟基磷灰石微球,同时探讨了水热合成过程中能有效控制晶体/粒子形貌及结构的机理及模型。主要内容及结果归纳如下：
首先,通过对反应温度、压力、初始pH值以及不同pH调节剂、钙离子的浓度和释放方式等水热物化条件的研究,得出了获得结晶程度高及晶形完整的反应参数,以及各种参数条件对晶体形貌的影响程度。通过构晶离子相对浓度的调节,可制备出具有纤维状和六方棱柱状的大颗粒羟基磷灰石晶体,同时可控制晶粒大小尺寸。结合负离子配位体晶体生长模型,获得了水热环境中各种物化条件对羟基磷灰石的生长基元的形成及结合的影响规律。
研究了十二烷基溴化铵(CTAB)、十二烷基硫酸钠(SDS)以及聚乙烯醇(PVA)三种不同类型的表面活性剂在水热反应过程中对HA晶体生长及形貌的影响。研究结果表明：阳离子表面活性剂-CTAB的加入可以控制获得短棒状的羟基磷灰石纳米颗粒,而阴离子表面活性剂-SDS的加入可得到片状形貌的羟基磷灰石粒子,非离子表面活性剂-PVA的加入使得羟基磷灰石粒子的长径比减小。其原理在于：带有不同电性的阴、阳离子表面活性剂基团,能够影响负离子配位体生长基元Ca-P6O24的形成,在一定程度上阻止了羟基磷灰石生长基元进入羟基磷灰石晶体,使得各个晶面的相对生长速率受影响,从而形成不同结晶形貌的羟基磷灰粒子。
采用碱性的精氨酸、酸性的谷氨酸和复合氨基酸作为反应添加剂,在水热反应过程中制备出不同形貌的羟基磷灰石粒子。研究发现：带有正电荷胍基基团的碱性精氨酸加入到水热溶液中,易于吸附到羟基磷灰石晶体的(100)面的P位置,而且这种吸附引起的抑制作用会因浓度的增加而增强,从而得到长径比小的短棒状的羟基磷灰石颗粒；加入带有负离子羧基团的酸性谷氨酸,易于吸附晶体的(100)面或(010)面,得到片状羟基磷灰石晶体；而复合氨基酸加入到水热溶液中,它对晶面的影响将随pH的变化而发生改变,最后将得到粒径较大的球柱状的羟基磷灰石晶体。其机理在于：不同的氨基酸根离子对羟基磷灰石的晶体的吸附位置不一样,从而对各个晶面的产生不同的影响,得到不同形貌的羟基磷灰石晶体。
研究了聚电解质六偏磷酸钠(STPP)和三聚磷酸钠(SHMP)在水热反应过程中对羟基磷灰石形貌的影响。研究发现：聚电解质在水溶液中形成的聚阴离子更易于吸附在羟基磷灰石晶体(100)面,阻碍羟基磷灰石在(100)面的活性位置的生长,使得羟基磷灰石晶体(100)面受到抑制成为较大的显露面。研究表明,直线性的分子链状聚阴离子比环状的聚阴离子的吸附力更强,从而对羟基磷灰石晶体形貌的影响更明显。另外,研究了三聚磷酸钠的浓度对羟基磷灰石晶体形貌的影响,发现聚电解质浓度越高越容易获得扁平状的羟基磷灰石晶体。
尝试采用壳聚糖与聚丙烯酸(CS-PAA)聚合物微球为模板,使羟基磷灰石颗粒在聚合物空心微球表面形核生长,经煅烧,去除聚合物模板,从而得到空心结构的羟基磷灰石微球。研究表明：聚电解质之间的静电引力斥力是复合空心球形成的关键,通过改变壳聚糖和丙烯酸的初始浓度,以及壳聚糖与丙烯酸的原始比例(AA/CS)可以调节聚合物空心球的尺寸；利用明胶作为聚合物与无机物的羟基磷灰石之间的粘结剂,使得羟基磷灰石粒子能够在聚合物微球表面成核、生长。研究表明,明胶具有联结羟基磷灰石微粒与聚合物微球的作用。通过煅烧,除掉聚合物模板CS-PAA,最后得到空心结构羟基磷灰石微球。此种空心结构羟基磷灰石微球合成的方法和原理,提供了一条无机物空心微球合成的有效途径。
Hydroxyapatite (HA) has been a very important biomaterial due to its excellent bioactivity and biocompatibility. In order to develop its research merits and application scope, the preparation of hydroxyapatite nanoparticle/microparticle with various morphology and different spacial structure become one hotspot of biomaterials research. This paper focuses on synthesis of crystal/particles with various morphology or hollow structure microspheres by controlling reaction conditions, introducing different kinds of reaction additives and adopting polymer templates.This paper also investigated the mechanism and model, which is adopted to control the morphology and structure of hydroxyapatite crystal/particles effectively in the hydrothermal conditions. The main content and results are summed up as following:
Firstly, the hydrothermal parameters of high crystallization degree and complete crystal shape are achieved by studying on the impact of hydrothermal conditions, such as reaction temperature, pressure, initial pH value, different pH regulator, calcium ion concentration and calcium ion releasing channel and so on, also including the affected degree of these hydrothermal parameters. Fibre-like and big size hexagonal prism-like hydroxyapatite crystal, and controllable crystal size particles are available by adjusting the relative ion concentration of hydroxyapatite components. The function mechanism that hydrothermal conditions impact hydroxyapatite growth unit formation and combination, is elaborated by introducing growth unit model of anion coordination polyhedron.
CTAB (Cetyl trimethyl ammonium bromide), SDS (sodium dodecyl sulfate) and PVA (polyvinyl alcohol), three kinds of surfactants are introduced to hydrothermal process to adjust the hydroxyapatite crystal growth habits and crystal morphology. The results indicate that short rod-like hydroxyapatite nanoparticles are achieved by adding positive surfactant-CTAB, while plate-like hydroxyapatite nanoparticle are obtained by introducing negative surfacetant-SDS, and low aspect ratio hydroxylapatite nanoparticles are prepared by introducing nonionic surfacetant-PVA. The mechanism bases on:the formation of Ca-P6O24growth unit of anionic coordination polyhedra is influenced by different surfactant groups with electric charge blocks, which disturbs hydroxyapatite growth unit to join hydroxyapatite crystal and retards the combination velocity of growth unit, and those effects lead to different morphology crystals.
The basic amino acid of arginine, acidic amino acid of glutamic acid, and compound amino acid are used as additives to prepare HA nanoparticle with various morphology. The research shows that the Arginine with positive guanidine group is apt to adhere to the P site of (100) face of HA crystal, and the adsorption interaction become stonger with higher concentration, which leads to short rod-like HA nanoparticle with lower aspect ratio. The Glutamic acid with negative carboxy groups prefer to bind on the (100) or (010) face of HA crystal, which leads to plate-like hydroxyapatite crystals. The compound amino acid affects different crystal facet in different pH value, which result in spherical HA particle as the growth speed is almost uniform.The main reaction mechanism lies in:different amino acid groups may absord on different sites of hydroxyapatite crystal, and have different effect on crystal facets, which changed the HA crystal structure and produced various crystal morphology.
The effect of STPP (sodium tripolyphosphate) and SHMP (Sodium hexametaphosphate) on hydroxyapatite crystal morphology are studied in hydrothermal preparation. The investigation shows that polyanions, the ions of polyelectrolyte in solution, are easy to adhere to (100) facet of hydroxyapatite crystal, which blocks active sites growth of (100) plane and make (100) facet to be obvious facet. The research also demonstrates that the polyanions with linear type molecular chain have stronger absorption force, and show more obvious effect on crystal morphology than the polyanions with circular type moleculear chain. In addition, the concentration of STPP impacts the morphology of hydroxyapatite crystal. It is preferable to get plate-like hydroxyapatite crystal with higher concentration of polyelectrolyte.
The hydroxyapatite microspheres with hollow structure are prepared by adopting template of CS-PAA polymer complex, hydroxyapatite particles nucleating and growing on the hollow CS-PAA polymer microspheres, and the polymer template is removed by calcination. The experiment shows that electrostatic attractive force and repulsive force have played crucial role in the formation of the CS-PAA sphere, and the size of CS-PAA spheres could be tuned by adjust the ratio and concentration of CS-AA in the reaction system. Gelatin, acted as binder to connect the spheres of CS-PAA with hydroxyapatite particles, help hydroxyapatite crystals to nucleate and grow on the polymer microsphere. Finally, the hollow structure hydroxyapatite microspheres are achieved by calcining the CS-PAA polymer template. This preparation method and mechanism of hollow structure hydroxyapatite microspheres, provides an effective approach to produce hollow inorganic microsphere.
首先,通过对反应温度、压力、初始pH值以及不同pH调节剂、钙离子的浓度和释放方式等水热物化条件的研究,得出了获得结晶程度高及晶形完整的反应参数,以及各种参数条件对晶体形貌的影响程度。通过构晶离子相对浓度的调节,可制备出具有纤维状和六方棱柱状的大颗粒羟基磷灰石晶体,同时可控制晶粒大小尺寸。结合负离子配位体晶体生长模型,获得了水热环境中各种物化条件对羟基磷灰石的生长基元的形成及结合的影响规律。
研究了十二烷基溴化铵(CTAB)、十二烷基硫酸钠(SDS)以及聚乙烯醇(PVA)三种不同类型的表面活性剂在水热反应过程中对HA晶体生长及形貌的影响。研究结果表明：阳离子表面活性剂-CTAB的加入可以控制获得短棒状的羟基磷灰石纳米颗粒,而阴离子表面活性剂-SDS的加入可得到片状形貌的羟基磷灰石粒子,非离子表面活性剂-PVA的加入使得羟基磷灰石粒子的长径比减小。其原理在于：带有不同电性的阴、阳离子表面活性剂基团,能够影响负离子配位体生长基元Ca-P6O24的形成,在一定程度上阻止了羟基磷灰石生长基元进入羟基磷灰石晶体,使得各个晶面的相对生长速率受影响,从而形成不同结晶形貌的羟基磷灰粒子。
采用碱性的精氨酸、酸性的谷氨酸和复合氨基酸作为反应添加剂,在水热反应过程中制备出不同形貌的羟基磷灰石粒子。研究发现：带有正电荷胍基基团的碱性精氨酸加入到水热溶液中,易于吸附到羟基磷灰石晶体的(100)面的P位置,而且这种吸附引起的抑制作用会因浓度的增加而增强,从而得到长径比小的短棒状的羟基磷灰石颗粒；加入带有负离子羧基团的酸性谷氨酸,易于吸附晶体的(100)面或(010)面,得到片状羟基磷灰石晶体；而复合氨基酸加入到水热溶液中,它对晶面的影响将随pH的变化而发生改变,最后将得到粒径较大的球柱状的羟基磷灰石晶体。其机理在于：不同的氨基酸根离子对羟基磷灰石的晶体的吸附位置不一样,从而对各个晶面的产生不同的影响,得到不同形貌的羟基磷灰石晶体。
研究了聚电解质六偏磷酸钠(STPP)和三聚磷酸钠(SHMP)在水热反应过程中对羟基磷灰石形貌的影响。研究发现：聚电解质在水溶液中形成的聚阴离子更易于吸附在羟基磷灰石晶体(100)面,阻碍羟基磷灰石在(100)面的活性位置的生长,使得羟基磷灰石晶体(100)面受到抑制成为较大的显露面。研究表明,直线性的分子链状聚阴离子比环状的聚阴离子的吸附力更强,从而对羟基磷灰石晶体形貌的影响更明显。另外,研究了三聚磷酸钠的浓度对羟基磷灰石晶体形貌的影响,发现聚电解质浓度越高越容易获得扁平状的羟基磷灰石晶体。
尝试采用壳聚糖与聚丙烯酸(CS-PAA)聚合物微球为模板,使羟基磷灰石颗粒在聚合物空心微球表面形核生长,经煅烧,去除聚合物模板,从而得到空心结构的羟基磷灰石微球。研究表明：聚电解质之间的静电引力斥力是复合空心球形成的关键,通过改变壳聚糖和丙烯酸的初始浓度,以及壳聚糖与丙烯酸的原始比例(AA/CS)可以调节聚合物空心球的尺寸；利用明胶作为聚合物与无机物的羟基磷灰石之间的粘结剂,使得羟基磷灰石粒子能够在聚合物微球表面成核、生长。研究表明,明胶具有联结羟基磷灰石微粒与聚合物微球的作用。通过煅烧,除掉聚合物模板CS-PAA,最后得到空心结构羟基磷灰石微球。此种空心结构羟基磷灰石微球合成的方法和原理,提供了一条无机物空心微球合成的有效途径。
Hydroxyapatite (HA) has been a very important biomaterial due to its excellent bioactivity and biocompatibility. In order to develop its research merits and application scope, the preparation of hydroxyapatite nanoparticle/microparticle with various morphology and different spacial structure become one hotspot of biomaterials research. This paper focuses on synthesis of crystal/particles with various morphology or hollow structure microspheres by controlling reaction conditions, introducing different kinds of reaction additives and adopting polymer templates.This paper also investigated the mechanism and model, which is adopted to control the morphology and structure of hydroxyapatite crystal/particles effectively in the hydrothermal conditions. The main content and results are summed up as following:
Firstly, the hydrothermal parameters of high crystallization degree and complete crystal shape are achieved by studying on the impact of hydrothermal conditions, such as reaction temperature, pressure, initial pH value, different pH regulator, calcium ion concentration and calcium ion releasing channel and so on, also including the affected degree of these hydrothermal parameters. Fibre-like and big size hexagonal prism-like hydroxyapatite crystal, and controllable crystal size particles are available by adjusting the relative ion concentration of hydroxyapatite components. The function mechanism that hydrothermal conditions impact hydroxyapatite growth unit formation and combination, is elaborated by introducing growth unit model of anion coordination polyhedron.
CTAB (Cetyl trimethyl ammonium bromide), SDS (sodium dodecyl sulfate) and PVA (polyvinyl alcohol), three kinds of surfactants are introduced to hydrothermal process to adjust the hydroxyapatite crystal growth habits and crystal morphology. The results indicate that short rod-like hydroxyapatite nanoparticles are achieved by adding positive surfactant-CTAB, while plate-like hydroxyapatite nanoparticle are obtained by introducing negative surfacetant-SDS, and low aspect ratio hydroxylapatite nanoparticles are prepared by introducing nonionic surfacetant-PVA. The mechanism bases on:the formation of Ca-P6O24growth unit of anionic coordination polyhedra is influenced by different surfactant groups with electric charge blocks, which disturbs hydroxyapatite growth unit to join hydroxyapatite crystal and retards the combination velocity of growth unit, and those effects lead to different morphology crystals.
The basic amino acid of arginine, acidic amino acid of glutamic acid, and compound amino acid are used as additives to prepare HA nanoparticle with various morphology. The research shows that the Arginine with positive guanidine group is apt to adhere to the P site of (100) face of HA crystal, and the adsorption interaction become stonger with higher concentration, which leads to short rod-like HA nanoparticle with lower aspect ratio. The Glutamic acid with negative carboxy groups prefer to bind on the (100) or (010) face of HA crystal, which leads to plate-like hydroxyapatite crystals. The compound amino acid affects different crystal facet in different pH value, which result in spherical HA particle as the growth speed is almost uniform.The main reaction mechanism lies in:different amino acid groups may absord on different sites of hydroxyapatite crystal, and have different effect on crystal facets, which changed the HA crystal structure and produced various crystal morphology.
The effect of STPP (sodium tripolyphosphate) and SHMP (Sodium hexametaphosphate) on hydroxyapatite crystal morphology are studied in hydrothermal preparation. The investigation shows that polyanions, the ions of polyelectrolyte in solution, are easy to adhere to (100) facet of hydroxyapatite crystal, which blocks active sites growth of (100) plane and make (100) facet to be obvious facet. The research also demonstrates that the polyanions with linear type molecular chain have stronger absorption force, and show more obvious effect on crystal morphology than the polyanions with circular type moleculear chain. In addition, the concentration of STPP impacts the morphology of hydroxyapatite crystal. It is preferable to get plate-like hydroxyapatite crystal with higher concentration of polyelectrolyte.
The hydroxyapatite microspheres with hollow structure are prepared by adopting template of CS-PAA polymer complex, hydroxyapatite particles nucleating and growing on the hollow CS-PAA polymer microspheres, and the polymer template is removed by calcination. The experiment shows that electrostatic attractive force and repulsive force have played crucial role in the formation of the CS-PAA sphere, and the size of CS-PAA spheres could be tuned by adjust the ratio and concentration of CS-AA in the reaction system. Gelatin, acted as binder to connect the spheres of CS-PAA with hydroxyapatite particles, help hydroxyapatite crystals to nucleate and grow on the polymer microsphere. Finally, the hollow structure hydroxyapatite microspheres are achieved by calcining the CS-PAA polymer template. This preparation method and mechanism of hollow structure hydroxyapatite microspheres, provides an effective approach to produce hollow inorganic microsphere.
引文
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