[1]巫剑波,秦草坪,袁秋华,等.湿化学法合成羟基磷灰石晶体及其表征[J].深圳大学学报理工版,2015,32(No.5(441-550)):465-472.[doi:10.3724/SP.J.1249.2015.05465]
 Wu Jianbo,Qin Caoping,Yuan Qiuhua,et al.Synthesis and characterization of hydroxyapatite crystals using wet chemistry methods[J].Journal of Shenzhen University Science and Engineering,2015,32(No.5(441-550)):465-472.[doi:10.3724/SP.J.1249.2015.05465]
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湿化学法合成羟基磷灰石晶体及其表征()
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《深圳大学学报理工版》[ISSN:1000-2618/CN:44-1401/N]

卷:
第32卷
期数:
2015年No.5(441-550)
页码:
465-472
栏目:
化学与化工
出版日期:
2015-09-18

文章信息/Info

Title:
Synthesis and characterization of hydroxyapatite crystals using wet chemistry methods
文章编号:
201505004
作者:
巫剑波秦草坪袁秋华郭志威刘家裕邓庆威张培新
深圳大学化学与环境工程学院,深圳 518060
Author(s):
Wu Jianbo Qin Caoping Yuan Qiuhua Guo Zhiwei Liu Jiayu Deng Qingwei and Zhang Peixin
College of Chemistry and Environmental Engineering, Shenzhen University, Shenzhen 518060, P.R.China
关键词:
无机仿生材料羟基磷灰石湿化学法水浴合成常温合成高结晶度和纯度晶体表征
Keywords:
inorganic biomimetic materials hydroxyapatite wet chemistry method water bath synthesis room temperature synthesis high crystallinity and purity crystal characterization
分类号:
R 318.08
DOI:
10.3724/SP.J.1249.2015.05465
文献标志码:
A
摘要:
采用湿化学法通过两种方案合成羟基磷灰石(hydroxyapatite,HA)晶体,一种方案是以Ca(NO3)2·4H2O和Na2HPO4作为原料,加入NaOH溶液调节pH值在10.5~11.0之间,不添加分散剂,在40 ℃水浴条件下合成羟基磷灰石;另一方案是在室温下(25 ℃)进行,在其他条件不变的情况下,以CaCl2·2H2O为钙源、乙醇胺作为分散剂合成羟基磷灰石.将两种方案合成的样品分别通过X射线衍射(X-ray diffraction, XRD)、傅里叶变换红外光谱(Fourier transform infrared spectroscopy, FTIR)、扫描电子显微镜(scanning electron microscopy, SEM)、X射线能量色散仪(energy-dispersive X-ray spectroscopy, EDX)、热重-差热分析和X射线光电子能谱(X-ray photoelectron spectroscopy, XPS)进行表征.XRD和FTIR结果显示,合成的两种HA粉末都具有较高结晶度和纯度.SEM分析表明,第1种方案可合成直径为30~50 nm,长50~150 nm的棒状晶体;第2种方案则可制备粒径约100~150 nm的球状(或椭球状)晶体.热分析表明,所制备的HA在1 000 ℃范围内有显著的热稳定性.XPS和EDX分析则证实HA由Ca、P和O等元素组成,两种方案中钙和磷的摩尔比分别是1.60和1.63.
Abstract:
Hydroxyapatite (HA) crystals were synthesized by two new wet chemistry methods. The first method was carried out by using calcium nitrate tetrahydrate and disodium hydrogen phosphate as starting materials and adding sodium hydroxide to ensure the pH value ranging from 10.5 to 11.0 under 40 ℃ water bath with no dispersant. For the other method, hydroxyapatite was synthesized at room temperature (25 ℃) with calcium chloride dehydrate as calcium source and ethanolamine as dispersing agent, while other conditions remained the same as those in the first method. The obtained samples were characterized by X-ray diffraction (XRD), fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDX), thermogravimetric analysis-differential thermal analysis (TG-DTA), and X-ray photoelectron spectroscopy (XPS), respectively. The XRD and FTIR results exhibit that the synthesized HA has a high crystallinity and purity. The SEM images reveal that rod-like HA crystals with a diameter of 30-50 nm and a length of 50-150 nm are formed by using the first method, while spherical or ellipsoidal HA crystals with a diameter of 100-150 nm around can be obtained through the second method. The thermal analysis shows that the synthesized HA has a remarkable heat stability up to 1 000 ℃,and the XPS and EDX studies indicate that HA samples are predominantly composed of elements including calcium (Ca), phosphorous (P), oxygen (O), etc. The ratios of Ca and P of HA samples in the first and the second methods are equal to 1.60 and 1.63, respectively.

参考文献/References:

[1] Dhand V, Rhee K Y, Park S J. The facile and low temperature synthesis of nanophase hydroxyapatite crystals using wet chemistry[J]. Materials Science and Engineering C,2014,36:152-159.
[2] Wang Fei, Zhou Hong, Guo Yucheng, et al. Biocompatibility and osteoinductive activity of nano-hydroxyapatite/chitosan/poly(lactide-co-glycolide)scaffolds in vitro [J]. Chinese Journal of Tissue Engineering Research, 2014, 18(8):1198-1204.(in Chinese)
王菲,周洪,郭昱成,等. 纳米羟基磷灰石/壳聚糖/聚丙交酯支架的体外生物相容性和成骨活性[J].中国组织工程研究,2014,18(8):1198-1204.
[3] Bazargan-Lari R,Zafarani H R,Bahrololoom M E,et al. Removal of Cu(II)ions from aqueous solutions by low-cost natural hydroxyapatite/chitosan composite: equilibrium, kinetic and thermodynamic studies[J]. Journal of the Taiwan Institiue of Chemical Engineers, 2014, 45(4): 1642-1648.
[4] Sadat-Shojai M,Khorasani M T,Dinpanah-Khoshdargi E,et al. Synthesis methods for nanosized hydroxyapatite with diverse structures[J]. Acta Biomaterialia, 2013, 9(8):7591-7621.
[5] Chou Mande,Wang Xiaoyan,Li Xu,et al. Microanalysis of hydroxyapatite synthesized by hydrothermal method[J],Journal of Synthetic Crystals,2013,42(9): 1965-1971.(in Chinese)
仇满德,王晓燕,李旭,等. 水热法合成羟基磷灰石的微分析研究[J]. 人工晶体学报,2013,42(9):1965-1971.
[6] Xu Xiaohong,Wu Jianfeng,Hua Quan,et al. Synthesis of nano-sized hydroxyapatite by powder sol-gels method[J]. Journal of The Chinese Ceramic Society,2012,40(2): 266-270.(in Chinese)
徐晓虹,吴建锋,华全,等. 溶胶-凝胶法制备纳米羟基磷灰石粉体[J]. 硅酸盐通报, 2012,40(2):266-270.
[7] Hossein E H,Mohammad R H,Mohammad C. Effects of parameters of sol-gel process on the phase evolution of sol-gel-derived hydroxyapatite[J]. Materials Chemistry & Physics, 2007, 106(2/3):310-316.
[8] Zhang Xiaoli,Zhang Zhaojun,Liu Ying,et al. The purity of hydroxyapatite(HAP)prepared by different method of precipitation[J]. Journal of Zhongyuan University of Technology,2014,24(1):56-58.(in Chinese)
张小立,张照君,刘英,等. 不同配方下沉淀法制备羟基磷灰石的纯度[J]. 中原工学院学报, 2013,24(1):56-58.
[9] Abidi S S A,Murtaza Q. Synthesis and characterization of nano-hydroxyapatite powder using wet chemical precipitation reaction[J]. Journal of Materials Science and Technology,2014,30(4):307-310.
[10] Amin S, Bekhit A El-Din A, Ali A, et al. Synthesis of nano-hydroxyapatite(nHA)from waste mussel shells using a rapid microwave method[J]. Materials Chemistry and Physics,2015,149/150:607-616.
[11] Wang Cai,Wang Shaohong,Hou Zhaoxia,et al. Advances in preparation of hydroxyapatite nano-particles by inverse micro-emulsions[J]. Ordnance Material Science and Engineering,2011,34(6): 102-106.(in Chinese)
王彩,王少洪,侯朝霞,等. 反相微乳液法制备纳米羟基磷灰石的研究进展[J]. 兵器材料科学与工程,2011,34(6):102-106.
[12] Guo Xiaojun,Yan Hudong,Wang Aiping,et al. Preparation of hydroxyapatite powders by solid-state reaction at room temperature[J]. Bulletin of the Chinese Ceramic Society,2012,31(6): 1453-1456.(in Chinese)
郭效军,严虎东,王爱平,等. 室温固相法制备羟基磷灰石粉体[J]. 硅酸盐通报,2012,31(6):1453-1456.
[13] Wang Pingping,Li Caihong,Gong Haiyan,et al. Effects of synthesis conditions on the morphology of hydroxyapatite nanoparticles produced by wet chemical process[J]. Powder Technology,2010,203(2):315-321.
[14] Hu Y Y, Liu X P, Ma X, et al. Biomimetic self-assembling copolymer hydroxyapatite nanocomposites with the nanocrystal size controlled by citrate[J]. Chemistry of Material,2011,23(9):2481-2490.
[15] Zhang Yanjie,Lu Jinjun. A mild and efficient biomimetic synthesis of rodlike hydroxyapatite particles with a high aspect ratio using polyvinylpyrrolidone as capping agent[J]. Crystal Growth and Design,2008,8(7): 2101-2107.
[16] Sadasivan S,Khushalani D,Mann A S. Synthesis of calcium phosphate nanofilaments in reverse micelles[J]. Chemistry of Materials,2005,17:2765-2770.
[17] Cai Yurong,Mei Danping,Jiang Tian,et al. Synthesis of oriented hydroxyapatite crystals: effect of reaction conditions in the presence or absence of silk sericin[J]. Materials Letters, 2010,64(24):2676-2678.
[18] Sadat-Shojai M,Khorasani M T,Jamshidi A, Hydrothermal processing of hydroxyapatite nanoparticles-a Taguchi experimental design approach[J]. Journal of Crystal Growth,2012,361:73-84.
[19] Suchanek W L,Shuk P,Byrappa K,et al. Mechanochemical-hydrothermal synthesis of carbonated apatite powders at room temperature[J]. Biomaterials, 2002,23:699-710.
[20] Li Ming’ou,Xiao Xiufeng,Liu Rongfang,et al. Structural characterization of zinc-substituted hydroxyapatite prepared by hydrothermal method[J]. Journal of Mate-rials Science Letters,2008,19(2):797-803.
[21] Koutsoukos P G,Nancollas G H. The morphology of hydroxyapatite crystals grown in aqueous solution at 37 ℃[J]. Journal of Crystal Growth,1981,55:369-375.
[22] Zhou Shaobing,Zheng Xiaotong,Yu Xiongjun,et al. Hydrogen bonding interaction of poly(D,L-Lactide)/hydroxyapatite nanocomposites[J]. Chemistry of Materials,2007,19(2):247-253.
[23] Yuan Qiuhua,Sahu L K,D’Souza N A, Sastry T P, et al. Synthesis of hydroxyapatite coatings on metal substrates using a spincasting technique[J]. Materials Chemistry and Physics,2009,116(2/3):523-526.
[24] Sobhana S S L,Sundaraseelan J,et al. Growth of hydroxyapatite crystals on gelatin-chitosan capped silver nanoparticles[J]. Advanced Porous Materials,2013,1(3):304-309.
[25] Song Yunjing,Wen Shulin,Li Musen,et al. Preparation and physicochemical process of nanosized hydroxyapatite powders with high purity[J]. Journal of Inorganic Materials,2002,17(5):985-991.( in Chinese)
宋云京,温树林,李木森,等,高品质羟基磷灰石纳米粉体的制备及物理化学过程研究[J]. 无机材料学报,2002,17(5): 985-991.

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备注/Memo

备注/Memo:
Received:2015-06-16;Accepted:2015-07-18
Foundation:National Natural Science Foundation of China(21471102, 20971088)
Corresponding author:Associate professor Yuan Qiuhua.E-mail: yuanqiuh@szu.edu.cn
Citation:Wu Jianbo,Qin Caoping,Yuan Qiuhua,et al.Synthesis and characterization of hydroxyapatite crystals using wet chemistry methods[J]. Journal of Shenzhen University Science and Engineering, 2015, 32(5): 465-472.(in Chinese)
基金项目:国家自然科学基金资助项目(21471102,20971088)
作者简介:巫剑波(1991—),男(汉族),广东省河源市人,深圳大学硕士研究生. E-mail:wj_boo@163.com
引文:巫剑波,秦草坪,袁秋华,等.湿化学法合成羟基磷灰石晶体及其表征[J]. 深圳大学学报理工版,2015,32(5):465-472.
更新日期/Last Update: 2015-09-15