定向碳纳米管薄膜的热化学气相沉积法制备及其血液相容性研究
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摘要
碳纳米管是一维新型纳米材料,具有低密度、高强度和极大的长径比。定向碳纳米管是它们沿着轴向生长的有序结构,具有优异的性能和广阔的应用前景,成为世界范围内的研究热点之一。
本论文首先利用K575X磁控溅射镀膜仪在硅基体上沉积一层镍催化剂薄膜,通过高温氨气对催化剂薄膜进行预处理,使催化剂由连续薄膜转变为纳米颗粒,探讨了刻蚀时间、温度和催化剂薄膜原始厚度等工艺参数对纳米颗粒显微结构的调控作用,寻找镍催化剂薄膜的刻蚀规律,获得具有良好形态的催化剂颗粒的基底,并初步分析氨气在其变化过程中的作用机制;其次,采用热化学气相沉积法在经氨刻蚀后获得的镍催化剂颗粒上制备定向碳纳米管薄膜,通过SEM、TEM、XRD和Raman等测试手段,对其进行表征与分析,研究制备工艺条件与碳纳米管薄膜的表面形貌和微观结构间的关系,并对工艺参数进行优化;在此基础上,通过对催化剂结构形貌和碳纳米管成核过程的的研究,提出了一种定向竹节型结构碳纳米管的生长机制,并构建了适合此类碳纳米管的生长模型;此外,本文还利用接触角测量仪测量了标准液在不同工艺条件下制备的碳纳米管薄膜表面上的接触角,并深入研究了制备工艺参数对碳纳米管薄膜表面界面特性的影响;最后探索了碳纳米管薄膜作为生物医用材料在血液相容性方面的潜在应用,采用体外法对碳纳米管薄膜的血液相容性进行了实验评价和对比研究,包括血小板粘附实验测定碳纳米管薄膜抗血小板黏附性能、动态凝血实验测定碳纳米管薄膜抗凝血性以及溶血实验评价碳纳米管薄膜对红细胞膜的破坏程度。通过对碳纳米管薄膜的表面界面特性表征和血液相容性评价,寻找影响碳纳米管薄膜血液相容性的主要因素,并对碳纳米管薄膜表面界面特性对其血液相容性的影响机理进行了初步探讨。获得的主要结论如下:
1、高温氨刻蚀可以调控硅基体表面镍催化剂颗粒的尺寸、密度和均匀性;只有恰当的刻蚀时间、温度和催化剂薄膜原始厚度才可以在硅基表面获得高密度、直径均匀细小的镍催化剂颗粒;实验中较理想的高温氨刻蚀工艺条件是刻蚀时间、温度和催化剂薄膜原始厚度分别为12min、800℃和10nm。
2、通过热化学气相沉积法成功制备出了定向碳纳米管薄膜;通过调控不同的制备工艺参数,实现了碳纳米管薄膜的可控性生长;并获得制备定向碳纳米管薄膜的优化工艺参数:生长温度850℃,反应时间10min,乙炔浓度16.7%,催化剂薄膜厚度10nm左右。
3、研究发现:D峰和G峰的强度比值I_D/I_G能够定量表征所研究的碳纳米管的纯度和有序度,I_D/I_G越低,说明该定向碳纳米管薄膜的非晶态碳成分越少,石墨化程度越高。
4、提出了一种基于生长-停止相间隔的动力学和空间位阻效应的定向竹节型结构碳纳米管的生长模型;利用EDX无损检测方式可以快速地推测出此类碳纳米管遵循顶端生长方式;通过XRD分析判断出在生长碳纳米管的过程中起催化作用的是金属镍颗粒而不是碳化镍。
5、通过采用接触角测量仪研究了不同工艺参数制备的碳纳米管薄膜的表面界面特性。结果表明:仅仅通过升高生长温度就可以使得其表面润湿性能大幅度提高——从亲水79.9°到超疏水155.4°;随着生长时间的增加其接触角先增加然后趋向稳定;随着乙炔浓度的增大其接触角先增大,然后骤然减小:通过调节催化剂厚度,碳纳米管薄膜表面的接触角可以从一般疏水95.7°到超疏水160.2°。此外,还发现随着碳纳米管薄膜表面接触角的提高,色散极性比γ_s~d/γ_s~p减少、界面自由能γ_(sl)增加、粘附功W_a降低。
6、碳纳米管血液相容性体外评价实验表明:碳纳米管薄膜的介入确实改善了基体的血液相容性,显著抑制了基体表面血小板黏附数量和激活百分数,有利于增强其抗血小板黏附性能;延长了动态凝血时间,有利于提高其抗凝血性能;降低了溶血率,大大改善了外环境,减少了异体材料对红细胞的毒害,这对维持红细胞的结构和功能的完整起了重要的作用;并且可以通过调整制备工艺参数来获得具有良好血液相容性的碳纳米管薄膜。
7、通过考察碳纳米管薄膜表面界面特性与其血液相容性的关系表明:碳纳米管薄膜表面的强疏水性、低色散极性比γ_s~d/γ_s~p和黏附功W_a、高界面自由能γ_(sl),有利于碳纳米管薄膜血液相容性的改善。此外,碳纳米管的血液相容性还与其表面微纳结构有关。
Carbon nanotubes(CNTs) are novel one-dimensional nano-materials with low density, high intensity and large aspect ratio.Aligned CNTs films are ordered groups of these nano-structures,which are all arranged along an identical direction,and are expected to have excellent properties implying promising applications,becoming one of the research hotspots in the world.
Nickel catalyst thin films were deposited firstly on silicon substrates by K575X magnetron sputtering coater.The effects of ammonia pretreatment on the change of catalyst films from continuous one to the one with nanoscale particles were investigated. The nanostructures of the Ni thin films as a function of etching time,temperature and initial thickness of the catalyst film were discussed.The etching rules of the nickel catalyst film were summarized.Good-shape catalyst particles were obtained on the substrates.And the functional mechanism of ammonia was primarily analyzed.Aligned CNTs films were prepared secondly on nickel particles which derived from ammonia etching through thermal CVD method.Modern measuring and testing techniques such as SEM,TEM,XRD and Raman spectrum were employed to characterize the sample properties.The relationship between surface morphologies of CNTs and technological conditions were investigated to optimize the preparation parameters.Based on the morphology of catalyst and the nucleation of CNTs,the growth mechanism of aligned bamboo-shaped CNTs was studied and growth model was proposed.Contact angles(CA) of standard solution on CNTs films prepared in different conditions were measured.Then the relationship between surface-interface properties of CNTs and technological parameters was studied.Potential applications of CNTs films for blood compatibility in biomedicine were investigated.The property of prevention of platelet adhesion, anticoagulant property and damage degree to erythrocytes of CNTs films were investigated by platelet adhesion test,dynamic clotting time test and hemolysis assessment in vitro,respectively.The main factors influencing the blood compatibility of CNTs films were analyzed according to the characterization of surface-interface properties and the evaluation of blood compatibility of CNTs films in vitro.The relationship between surface-interface properties and blood compatibility of CNTs films were preliminary discussed.The principal results of this thesis were listed as follows.
1、The size,density and homogenization of Ni nanoparticles on Si were adjusted through high temperature NH_3 etching.The appropriate processing time of ammonia, the processing temperature and initial film thickness are the key factors to obtain high dense.The better conditions for the fabrication of the uniform,small and high density transition metal catalyst nanoparticles on Si substrates are as follows:the etching duration of about 12min,the temperature of 800℃and initial film thickness of 10nm.
2、Aligned CNTs films were prepared successfully by thermal CVD on etched Ni films. Controllable growth of CNTs films was implemented by adjusting different technogical parameters.Optimum preparation parameters of aligned CNTs films is obtained as follows:the growth temperature of 850℃,the growth time of 10min, C_2H_2 concentration of 16.7%and film thickness of 10nm.
3、The results suggest that the intensity ratio I_D/I_G indicates the purity and degree of order in aligned CNTs.A lower I_D/I_G means less amorphous carbon and higher graphitization in aligned CNTs.
4、A new growth mechanism based on dynamics alternation between growth-stop and steric hindrance was proposed,and it can give a qualitative explaination for the experiment results.EDX spectroscopy with non-destructive testing quickly indicated that the growth of CNTs conformed to tip-growth model,and XRD testing confirmed that Ni nanoparticles acted as the catalyst,not nickel carbide compound occurred during the CNTs growth period.
5、The results obtained from surface-interface properties of CNTs films prepared in different conditions indicated that increasing the temperature could improve the wettability of CNTs surface with the contact angle ranging form 79.9°to 155.4°; contact angle increase of the time and ultimately kept steady;contact angle increased firstly and sharply decreased with the rising concentration of acetylene;contact angle changed from 95.7°to 160.2°by means of adjusting the thickness of nickel films. With the increase of contact angle for CNTs films,γ_s~d /γ_s~p and work of adhesion W_a decreased,while interfacial free energyγ_(sl) increased.
6、Blood compatibility test for CNTs films in vitro indicated that CNTs films could improve the blood compatibility of substrate.Due to the interposition of CNTs,the number of platelets adhered and activated decreased,dynamic clotting time extended, haemolysis ratio decreased.It also improved the external environment,reduced the toxicity to erythrocyte and played an important role in maintaining the normal morphology and function of erythrocyte.In addition,CNTs films with excellent blood compatibility could be prepared via optimizing the technological parameters.
7、Through investigation of the relation between surface-interface properties of CNTs and its blood compatibility,it indicated that several factors can be used to improve its blood compatibility such as strong hydrophobicity,low ratio of dispersive/polar component of the surface energyγ_s~d /γ_s~p and work of adhesion W_a,high interfacial free energyγ_(sl).Moreover,the micro-nano structure is also closely related to its blood compatibility.
本论文首先利用K575X磁控溅射镀膜仪在硅基体上沉积一层镍催化剂薄膜,通过高温氨气对催化剂薄膜进行预处理,使催化剂由连续薄膜转变为纳米颗粒,探讨了刻蚀时间、温度和催化剂薄膜原始厚度等工艺参数对纳米颗粒显微结构的调控作用,寻找镍催化剂薄膜的刻蚀规律,获得具有良好形态的催化剂颗粒的基底,并初步分析氨气在其变化过程中的作用机制;其次,采用热化学气相沉积法在经氨刻蚀后获得的镍催化剂颗粒上制备定向碳纳米管薄膜,通过SEM、TEM、XRD和Raman等测试手段,对其进行表征与分析,研究制备工艺条件与碳纳米管薄膜的表面形貌和微观结构间的关系,并对工艺参数进行优化;在此基础上,通过对催化剂结构形貌和碳纳米管成核过程的的研究,提出了一种定向竹节型结构碳纳米管的生长机制,并构建了适合此类碳纳米管的生长模型;此外,本文还利用接触角测量仪测量了标准液在不同工艺条件下制备的碳纳米管薄膜表面上的接触角,并深入研究了制备工艺参数对碳纳米管薄膜表面界面特性的影响;最后探索了碳纳米管薄膜作为生物医用材料在血液相容性方面的潜在应用,采用体外法对碳纳米管薄膜的血液相容性进行了实验评价和对比研究,包括血小板粘附实验测定碳纳米管薄膜抗血小板黏附性能、动态凝血实验测定碳纳米管薄膜抗凝血性以及溶血实验评价碳纳米管薄膜对红细胞膜的破坏程度。通过对碳纳米管薄膜的表面界面特性表征和血液相容性评价,寻找影响碳纳米管薄膜血液相容性的主要因素,并对碳纳米管薄膜表面界面特性对其血液相容性的影响机理进行了初步探讨。获得的主要结论如下:
1、高温氨刻蚀可以调控硅基体表面镍催化剂颗粒的尺寸、密度和均匀性;只有恰当的刻蚀时间、温度和催化剂薄膜原始厚度才可以在硅基表面获得高密度、直径均匀细小的镍催化剂颗粒;实验中较理想的高温氨刻蚀工艺条件是刻蚀时间、温度和催化剂薄膜原始厚度分别为12min、800℃和10nm。
2、通过热化学气相沉积法成功制备出了定向碳纳米管薄膜;通过调控不同的制备工艺参数,实现了碳纳米管薄膜的可控性生长;并获得制备定向碳纳米管薄膜的优化工艺参数:生长温度850℃,反应时间10min,乙炔浓度16.7%,催化剂薄膜厚度10nm左右。
3、研究发现:D峰和G峰的强度比值I_D/I_G能够定量表征所研究的碳纳米管的纯度和有序度,I_D/I_G越低,说明该定向碳纳米管薄膜的非晶态碳成分越少,石墨化程度越高。
4、提出了一种基于生长-停止相间隔的动力学和空间位阻效应的定向竹节型结构碳纳米管的生长模型;利用EDX无损检测方式可以快速地推测出此类碳纳米管遵循顶端生长方式;通过XRD分析判断出在生长碳纳米管的过程中起催化作用的是金属镍颗粒而不是碳化镍。
5、通过采用接触角测量仪研究了不同工艺参数制备的碳纳米管薄膜的表面界面特性。结果表明:仅仅通过升高生长温度就可以使得其表面润湿性能大幅度提高——从亲水79.9°到超疏水155.4°;随着生长时间的增加其接触角先增加然后趋向稳定;随着乙炔浓度的增大其接触角先增大,然后骤然减小:通过调节催化剂厚度,碳纳米管薄膜表面的接触角可以从一般疏水95.7°到超疏水160.2°。此外,还发现随着碳纳米管薄膜表面接触角的提高,色散极性比γ_s~d/γ_s~p减少、界面自由能γ_(sl)增加、粘附功W_a降低。
6、碳纳米管血液相容性体外评价实验表明:碳纳米管薄膜的介入确实改善了基体的血液相容性,显著抑制了基体表面血小板黏附数量和激活百分数,有利于增强其抗血小板黏附性能;延长了动态凝血时间,有利于提高其抗凝血性能;降低了溶血率,大大改善了外环境,减少了异体材料对红细胞的毒害,这对维持红细胞的结构和功能的完整起了重要的作用;并且可以通过调整制备工艺参数来获得具有良好血液相容性的碳纳米管薄膜。
7、通过考察碳纳米管薄膜表面界面特性与其血液相容性的关系表明:碳纳米管薄膜表面的强疏水性、低色散极性比γ_s~d/γ_s~p和黏附功W_a、高界面自由能γ_(sl),有利于碳纳米管薄膜血液相容性的改善。此外,碳纳米管的血液相容性还与其表面微纳结构有关。
Carbon nanotubes(CNTs) are novel one-dimensional nano-materials with low density, high intensity and large aspect ratio.Aligned CNTs films are ordered groups of these nano-structures,which are all arranged along an identical direction,and are expected to have excellent properties implying promising applications,becoming one of the research hotspots in the world.
Nickel catalyst thin films were deposited firstly on silicon substrates by K575X magnetron sputtering coater.The effects of ammonia pretreatment on the change of catalyst films from continuous one to the one with nanoscale particles were investigated. The nanostructures of the Ni thin films as a function of etching time,temperature and initial thickness of the catalyst film were discussed.The etching rules of the nickel catalyst film were summarized.Good-shape catalyst particles were obtained on the substrates.And the functional mechanism of ammonia was primarily analyzed.Aligned CNTs films were prepared secondly on nickel particles which derived from ammonia etching through thermal CVD method.Modern measuring and testing techniques such as SEM,TEM,XRD and Raman spectrum were employed to characterize the sample properties.The relationship between surface morphologies of CNTs and technological conditions were investigated to optimize the preparation parameters.Based on the morphology of catalyst and the nucleation of CNTs,the growth mechanism of aligned bamboo-shaped CNTs was studied and growth model was proposed.Contact angles(CA) of standard solution on CNTs films prepared in different conditions were measured.Then the relationship between surface-interface properties of CNTs and technological parameters was studied.Potential applications of CNTs films for blood compatibility in biomedicine were investigated.The property of prevention of platelet adhesion, anticoagulant property and damage degree to erythrocytes of CNTs films were investigated by platelet adhesion test,dynamic clotting time test and hemolysis assessment in vitro,respectively.The main factors influencing the blood compatibility of CNTs films were analyzed according to the characterization of surface-interface properties and the evaluation of blood compatibility of CNTs films in vitro.The relationship between surface-interface properties and blood compatibility of CNTs films were preliminary discussed.The principal results of this thesis were listed as follows.
1、The size,density and homogenization of Ni nanoparticles on Si were adjusted through high temperature NH_3 etching.The appropriate processing time of ammonia, the processing temperature and initial film thickness are the key factors to obtain high dense.The better conditions for the fabrication of the uniform,small and high density transition metal catalyst nanoparticles on Si substrates are as follows:the etching duration of about 12min,the temperature of 800℃and initial film thickness of 10nm.
2、Aligned CNTs films were prepared successfully by thermal CVD on etched Ni films. Controllable growth of CNTs films was implemented by adjusting different technogical parameters.Optimum preparation parameters of aligned CNTs films is obtained as follows:the growth temperature of 850℃,the growth time of 10min, C_2H_2 concentration of 16.7%and film thickness of 10nm.
3、The results suggest that the intensity ratio I_D/I_G indicates the purity and degree of order in aligned CNTs.A lower I_D/I_G means less amorphous carbon and higher graphitization in aligned CNTs.
4、A new growth mechanism based on dynamics alternation between growth-stop and steric hindrance was proposed,and it can give a qualitative explaination for the experiment results.EDX spectroscopy with non-destructive testing quickly indicated that the growth of CNTs conformed to tip-growth model,and XRD testing confirmed that Ni nanoparticles acted as the catalyst,not nickel carbide compound occurred during the CNTs growth period.
5、The results obtained from surface-interface properties of CNTs films prepared in different conditions indicated that increasing the temperature could improve the wettability of CNTs surface with the contact angle ranging form 79.9°to 155.4°; contact angle increase of the time and ultimately kept steady;contact angle increased firstly and sharply decreased with the rising concentration of acetylene;contact angle changed from 95.7°to 160.2°by means of adjusting the thickness of nickel films. With the increase of contact angle for CNTs films,γ_s~d /γ_s~p and work of adhesion W_a decreased,while interfacial free energyγ_(sl) increased.
6、Blood compatibility test for CNTs films in vitro indicated that CNTs films could improve the blood compatibility of substrate.Due to the interposition of CNTs,the number of platelets adhered and activated decreased,dynamic clotting time extended, haemolysis ratio decreased.It also improved the external environment,reduced the toxicity to erythrocyte and played an important role in maintaining the normal morphology and function of erythrocyte.In addition,CNTs films with excellent blood compatibility could be prepared via optimizing the technological parameters.
7、Through investigation of the relation between surface-interface properties of CNTs and its blood compatibility,it indicated that several factors can be used to improve its blood compatibility such as strong hydrophobicity,low ratio of dispersive/polar component of the surface energyγ_s~d /γ_s~p and work of adhesion W_a,high interfacial free energyγ_(sl).Moreover,the micro-nano structure is also closely related to its blood compatibility.
引文
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