光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2014年
11期
3011-3014
,共4页
廖建国%李艳群%段星泽%刘琼
廖建國%李豔群%段星澤%劉瓊
료건국%리염군%단성택%류경
CO2 -3 替代%掺杂%拉曼光谱%碳羟基磷灰石
CO2 -3 替代%摻雜%拉曼光譜%碳羥基燐灰石
CO2 -3 체대%참잡%랍만광보%탄간기린회석
CO2 -3 -substituted%Doping%Raman spectrum%Carbonate hydroxylapatite
CO2-3掺杂是提高纳米羟基磷灰石(n-HA)生物活性的有效方法之一。以 Ca(NO3)2·4H2O 和Na3PO4·12H2O为主要原料,Na2CO3作为CO2-3来源,合成纳米碳羟基磷灰石(n-CHA)晶体。采用TEM , XRD ,FTIR ,RS对合成晶体形貌和结构进行表征。结果表明:合成的n-HA晶体长度约为60~80 nm ,宽度在20~30 nm之间,形状为针状,具有良好的结晶度,与自然骨磷灰石形貌相似;n-CHA晶体随CO2-3掺入量的增加,结晶度降低;合成的 n-CHA晶体的晶胞参数 a值随着CO2-3加入量的增大不断收缩,但 c值增大,参数比c/a值增大,符合B型取代(取代PO3-4)的晶胞参数变化规律。红外谱图中,872 cm -1附近出现AB混合型取代(同时取代O H -,PO3-4)的CO2-3面外弯曲振动特征红外峰,同时CO2-3的不对称伸缩振动红外峰在1454和1420 cm -1附近出现分裂峰,1540 cm -1附近出现弱CO2-3峰;1122 cm -1附近出现CO2-3对称伸缩振动拉曼峰,1071 cm -1附近出现CO2-3的B型替代特征拉曼峰,通过计算PO3-4,CO2-3,O H -拉曼峰的积分面积比PO3-4/CO2-3,O H -/CO23,PO3-4/O H -,表明CO2-3在替换时,先以B型为主,随着CO2-3掺入量的增加,发生A型替代(取代O H -)。实验结果表明,合成的磷灰石晶体为B型取代(取代PO3-4)为主的AB混合型取代的 n-CHA。与人骨磷灰石晶体在形态、尺寸、晶体结构和生长方式上具有相似性,可称为类骨磷灰石。
CO2-3摻雜是提高納米羥基燐灰石(n-HA)生物活性的有效方法之一。以 Ca(NO3)2·4H2O 和Na3PO4·12H2O為主要原料,Na2CO3作為CO2-3來源,閤成納米碳羥基燐灰石(n-CHA)晶體。採用TEM , XRD ,FTIR ,RS對閤成晶體形貌和結構進行錶徵。結果錶明:閤成的n-HA晶體長度約為60~80 nm ,寬度在20~30 nm之間,形狀為針狀,具有良好的結晶度,與自然骨燐灰石形貌相似;n-CHA晶體隨CO2-3摻入量的增加,結晶度降低;閤成的 n-CHA晶體的晶胞參數 a值隨著CO2-3加入量的增大不斷收縮,但 c值增大,參數比c/a值增大,符閤B型取代(取代PO3-4)的晶胞參數變化規律。紅外譜圖中,872 cm -1附近齣現AB混閤型取代(同時取代O H -,PO3-4)的CO2-3麵外彎麯振動特徵紅外峰,同時CO2-3的不對稱伸縮振動紅外峰在1454和1420 cm -1附近齣現分裂峰,1540 cm -1附近齣現弱CO2-3峰;1122 cm -1附近齣現CO2-3對稱伸縮振動拉曼峰,1071 cm -1附近齣現CO2-3的B型替代特徵拉曼峰,通過計算PO3-4,CO2-3,O H -拉曼峰的積分麵積比PO3-4/CO2-3,O H -/CO23,PO3-4/O H -,錶明CO2-3在替換時,先以B型為主,隨著CO2-3摻入量的增加,髮生A型替代(取代O H -)。實驗結果錶明,閤成的燐灰石晶體為B型取代(取代PO3-4)為主的AB混閤型取代的 n-CHA。與人骨燐灰石晶體在形態、呎吋、晶體結構和生長方式上具有相似性,可稱為類骨燐灰石。
CO2-3참잡시제고납미간기린회석(n-HA)생물활성적유효방법지일。이 Ca(NO3)2·4H2O 화Na3PO4·12H2O위주요원료,Na2CO3작위CO2-3래원,합성납미탄간기린회석(n-CHA)정체。채용TEM , XRD ,FTIR ,RS대합성정체형모화결구진행표정。결과표명:합성적n-HA정체장도약위60~80 nm ,관도재20~30 nm지간,형상위침상,구유량호적결정도,여자연골린회석형모상사;n-CHA정체수CO2-3참입량적증가,결정도강저;합성적 n-CHA정체적정포삼수 a치수착CO2-3가입량적증대불단수축,단 c치증대,삼수비c/a치증대,부합B형취대(취대PO3-4)적정포삼수변화규률。홍외보도중,872 cm -1부근출현AB혼합형취대(동시취대O H -,PO3-4)적CO2-3면외만곡진동특정홍외봉,동시CO2-3적불대칭신축진동홍외봉재1454화1420 cm -1부근출현분렬봉,1540 cm -1부근출현약CO2-3봉;1122 cm -1부근출현CO2-3대칭신축진동랍만봉,1071 cm -1부근출현CO2-3적B형체대특정랍만봉,통과계산PO3-4,CO2-3,O H -랍만봉적적분면적비PO3-4/CO2-3,O H -/CO23,PO3-4/O H -,표명CO2-3재체환시,선이B형위주,수착CO2-3참입량적증가,발생A형체대(취대O H -)。실험결과표명,합성적린회석정체위B형취대(취대PO3-4)위주적AB혼합형취대적 n-CHA。여인골린회석정체재형태、척촌、정체결구화생장방식상구유상사성,가칭위류골린회석。
CO2 -3 doping is an effective method to increase the biological activity of nano-hydroxyapatite (n-HA) .In the present study ,calcium nitrate and trisodium phosphate were chosen as raw materials ,with a certain amount of Na2 CO3 as a source of CO2 -3 ions ,to synthesize nano-carbonate hydroxyapatite (n-CHA) slurry by solution precipitation method .The structure and mi-cro-morphology of n-CHA were characterized by transmission electron microscope (TEM ) ,X-ray diffraction (XRD) ,Fourier transform-infrared spectroscopy (FTIR) and Raman spectroscopy (RS) .The results revealed that the synthetic n-HA crystals are acicular in nanometer scale and have a crystal size of 20~30 nm in diameter and 60~80 nm in length ,which are similar to natural bone apatite .And the crystallinity of n-CHA crystals decreases to the increment of CO2 -3 .Samples with more CO23 have composition and structure more similar to the bone apatite .The value of lattice parameters a decreases ,value of c increases ,and c/a value increases with the increase in the amount of CO2 -3 ,in accordance with crystal cell parameters change rule of type B re-placement .In the AB mixed type (substitution OH - and PO3 -4 ) CHA ,IR characteristic peak of CO2 -3 out-of-plane bending vi-bration appears at 872 cm -1 ,meanwhile ,the asymmetry flexible vibration band is split into band at 1 454 cm -1 and band at 1 420 cm -1 ,while weak CO23-peak appears at 1 540 cm -1 .CO2 -3 Raman peak of symmetric stretching vibration appears at 1 122 cm -1 .CO2 -3 B-type (substitution PO3 -4 ) peak appeared at 1 071 cm -1 .Through the calculation of integral area ratio of PO3 -4 /CO2 -3 ,OH - /CO2 -3 ,and PO3 -4 /OH - ,low quantity CO2 -3 is B-type and high quantity CO2 -3 is A-type (substitution OH -) .The results show that the synthesized apatite crystals are AB hybrid substitued nano-carbonate hydroxyapatite ,however B-type re-placement is the main substitute mode .Due to similarity in the shape ,size ,crystal structure and grow th mode ,the synthesized apatite crystals can be called a kind of bone-like apatite .