Anodization

阳极氧化
  • 文章类型: Journal Article
    钛和钛合金具有低密度和接近自然骨的弹性模量的优点,可以降低应力屏蔽效应,成为人体硬组织置换和修复的首选方法之一。然而,植入部位感染仍是植入失败的主要原因之一。在本文中,将2.5wt%Ag元素添加到Ti-15Mo中以获得低模量,并应用表面阳极氧化来提高表面生物相容性。弹性模量,微观形态,表面元素化合价,耐腐蚀性,抗菌性能,和细胞相容性通过机械测试进行研究,扫描电子显微镜,X射线光电子能谱,电化学测试,电感耦合等离子体光谱,平板计数法,和细胞测试。实验结果表明,阳极氧化的Ti-15Mo-2.5Ag样品的弹性模量为79GPa,具有很强的耐腐蚀性,强抗菌能力≥99.99%,和良好的生物相容性。结果表明,Ag2O在表面的形成和Ag离子的释放提高了抗菌性能,银离子与微米和纳米结构的结构协同作用在促进细胞早期扩散和提高细胞相容性方面发挥了重要作用。
    Titanium and titanium alloys have the advantages of a low density and a close elastic modulus to natural bone, which can reduce the stress-shielding effect and become one of the first choices for human hard tissue replacement and repair. However, implant site infection is still one of the main reasons for implantation failure. In this paper, 2.5 wt % Ag element was added to Ti-15Mo to obtain a low modulus, and a surface anodization was applied to improve the surface biocompatibility. The elastic modulus, micromorphology, surface elemental valence, corrosion resistance, antimicrobial properties, and cytocompatibility were investigated by mechanical tests, scanning electron microscopy, X-ray photoelectron spectroscopy, electrochemical tests, inductively coupled plasma spectroscopy, plate counting method, and cellular tests. The experimental results showed that the anodized Ti-15Mo-2.5Ag sample exhibited an elastic modulus of 79 GPa, a strong corrosion resistance, a strong antimicrobial ability of ≥99.99%, and good biocompatibility. It was demonstrated that the formation of Ag2O on the surface and Ag ion release improved the antimicrobial properties and that the structural synergism of silver ions with micro- and nanostructures played an important role in promoting the early spreading of cells and improving the cytocompatibility.
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  • 文章类型: Journal Article
    用于骨科植入物的材料不仅应具有接近骨骼的物理性质,耐久性和生物相容性,但也应表现出足够程度的抗菌功能。由于其优异的性能,钛仍然是一种广泛用于生产骨科植入物的材料,但未改性的材料表现出较差的抗菌活性。在这项工作中,物理化学特征,如化学成分,结晶度润湿性,粗糙度,分析了用纳米管层修饰的钛表面的Ti离子的释放,并研究了其对负责假体关节感染的两种生物膜形成细菌菌株(金黄色葡萄球菌和铜绿假单胞菌)的抗菌活性。电化学阳极氧化(阳极氧化)用于制备两种类型的纳米管阵列,其纳米管的尺寸不同(直径为73和118nm,长度为572和343nm,分别)。这两种表面类型显示出相似的化学性质,结晶度表面能量。具有较小纳米管直径(TNT-73)但较大粗糙度参数值的表面对金黄色葡萄球菌更有效。对于铜绿假单胞菌,具有较大纳米管直径的样品(TNT-118)具有更好的抗菌效果,同时证实细胞裂解。钛纳米管表面的抗菌性能具有潜在的植入学,在我们之前的工作中证明了对人类牙龈成纤维细胞行为的积极影响,在表面参数方面进行了研究。纳米管直径和粗糙度之间的相互作用对于纳米管表面上的细菌命运至关重要。纳米管直径的关系,粗糙度参数值,以及其他表面特性对细菌行为的影响进行了详细讨论。该研究被认为可以进一步阐明纳米管状表面参数及其相互作用如何影响抗菌活性。
    Materials used for orthopedic implants should not only have physical properties close to those of bones, durability and biocompatibility, but should also exhibit a sufficient degree of antibacterial functionality. Due to its excellent properties, titanium is still a widely used material for production of orthopedic implants, but the unmodified material exhibits poor antibacterial activity. In this work, the physicochemical characteristics, such as chemical composition, crystallinity, wettability, roughness, and release of Ti ions of the titanium surface modified with nanotubular layers were analyzed and its antibacterial activity against two biofilm-forming bacterial strains responsible for prosthetic joint infection (Staphylococcus aureus and Pseudomonas aeruginosa) was investigated. Electrochemical anodization (anodic oxidation) was used to prepare two types of nanotubular arrays with nanotubes differing in dimensions (with diameters of 73 and 118 nm and lengths of 572 and 343 nm, respectively). These two surface types showed similar chemistry, crystallinity, and surface energy. The surface with smaller nanotube diameter (TNT-73) but larger values of roughness parameters was more effective against S. aureus. For P. aeruginosa the sample with a larger nanotube diameter (TNT-118) had better antibacterial effect with proven cell lysis. Antibacterial properties of titanium nanotubular surfaces with potential in implantology, which in our previous work demonstrated a positive effect on the behavior of human gingival fibroblasts, were investigated in terms of surface parameters. The interplay between nanotube diameter and roughness appeared critical for the bacterial fate on nanotubular surfaces. The relationship of nanotube diameter, values of roughness parameters, and other surface properties to bacterial behavior is discussed in detail. The study is believed to shed more light on how nanotubular surface parameters and their interplay affect antibacterial activity.
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  • 文章类型: Journal Article
    阳极化是一种制造可调纳米孔隙率和厚度的氧化铝涂层的方法。本研究致力于大面积硬质阳极氧化(HA),超硬阳极氧化(UHA),过渡模式。使用线性扫描伏安法在大面积样品上研究了UHA的现象和挑战以及从HA的转变。研究结果表明,通过使用预UHA模式可以实现均匀的大面积厚涂层。研究结果表明,UHA在大面积阳极氧化中只会导致厚度不均匀的涂层。在0.3M草酸电解质中,使用不同的温度(0、5、10和15°C)和处理时间(1、2、4、6和12h)研究了预UHA的特性。当前的研究表明,厚纳米多孔氧化铝仅需12小时即可快速生长至235±4µm。
    Anodization is a method to fabricate a tunable nanoporosity and thickness of alumina coating. This research is devoted to large-area hard anodization (HA), ultrahard anodization (UHA), and transitional modes. The phenomenon and challenges of UHA and the transition from HA are studied on large-area samples using linear-sweep voltammetry. The findings indicate that a uniform large-area thick coating can be achieved by utilizing pre-UHA modes. The study\'s results indicate that UHA leads only to coatings with non-uniform thickness in large-area anodization. The peculiarities of pre-UHA are studied using different temperatures (0, 5, 10, and 15 °C) and processing times (1, 2, 4, 6, and 12 h) in a 0.3 M oxalic acid electrolyte. The current study shows the possibility for the fast growth of thick nanoporous alumina up to 235 ± 4 µm for only 12 h.
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  • 文章类型: Journal Article
    生物材料是医学发展的基础,因为它们允许与生物体安全接触。这项工作的目的是在商业纯钛4级(CpTiG4)的表面上生产具有微孔结构的创新氧化物层,并表征其作为药物载体的性能。进行机械研磨和电化学抛光的CpTiG4的阳极氧化在1M乙二醇溶液中进行,其中加入40g氟化铵,在20V电压下在室温下持续2、18、24和48小时。发现阳极氧化时间越长,使用FE-SEM方法显示,CpTiG4表面形成的孔数量越多,并且在轮廓测量测试中确定的表面粗糙度越大。随着阳极氧化时间的增加,合并到所得孔中的硫酸庆大霉素形式的药物的量减少。对于CpTiG4阳极氧化2小时,发现了通过UV-VIS吸收光谱确定的最有利的药物释放动力学曲线。
    Biomaterials are the basis for the development of medicine because they allow safe contact with a living organism. The aim of this work was to produce innovative oxide layers with a microporous structure on the surface of commercially pure titanium Grade 4 (CpTi G4) and to characterize their properties as drug carriers. The anodization of the CpTi G4 subjected to mechanical grinding and electrochemical polishing was carried out in a solution of 1M ethylene glycol with the addition of 40 g of ammonium fluoride at a voltage of 20 V for 2, 18, 24, and 48 h at room temperature. It was found that the longer the anodization time, the greater the number of pores formed on the CpTi G4 surface as revealed using the FE-SEM method, and the greater the surface roughness determined in profilometric tests. As the anodizing time increases, the amount of the drug in the form of gentamicin sulfate incorporated into the resulting pores decreases. The most favorable drug release kinetics profile determined via UV-VIS absorption spectroscopy was found for the CpTi G4 anodized for 2 h.
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  • 文章类型: Journal Article
    本研究提出了一种通过单步电化学合成制造阳极Co-F-WO3层的新方法,利用氟化钴作为电解质中的掺杂剂源。提出的原位掺杂技术利用了氟的高电负性,确保CoF2在整个合成过程中的稳定性。纳米多孔层的形成,由于在氟离子存在下阳极氧化物溶解,有望促进钴化合物有效掺入到膜中。该研究探讨了电解质中掺杂剂浓度的影响,对所得材料进行全面表征,包括形态学,composition,光学,电化学,和光电化学性能。通过能量色散谱(EDS)证实了WO3的成功掺杂,X射线衍射(XRD)拉曼光谱,光致发光测量,X射线光电子能谱(XPS),和Mott-Schottky分析。光学研究表明,Co掺杂材料的吸收较低,带隙能量略有变化。光电化学(PEC)分析表明,共掺杂层的PEC活性得到改善,观察到的光电流起始电位的变化归因于钴和氟离子的催化作用。该研究包括对观察到的现象及其对太阳能水分解应用的影响的深入讨论,强调阳极Co-F-WO3层作为有效光电极的潜力。此外,该研究对阳极Co-F-WO3的电化学合成和表征进行了全面的探索,强调了它们对析氧反应(OER)的光催化性能。发现Co掺杂的WO3材料表现出更高的PEC活性,与原始材料相比,最大增强5倍。此外,研究表明,这些光阳极可以有效地重复使用PEC水分解实验。
    This study presents a novel approach to fabricating anodic Co-F-WO3 layers via a single-step electrochemical synthesis, utilizing cobalt fluoride as a dopant source in the electrolyte. The proposed in situ doping technique capitalizes on the high electronegativity of fluorine, ensuring the stability of CoF2 throughout the synthesis process. The nanoporous layer formation, resulting from anodic oxide dissolution in the presence of fluoride ions, is expected to facilitate the effective incorporation of cobalt compounds into the film. The research explores the impact of dopant concentration in the electrolyte, conducting a comprehensive characterization of the resulting materials, including morphology, composition, optical, electrochemical, and photoelectrochemical properties. The successful doping of WO3 was confirmed by energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), Raman spectroscopy, photoluminescence measurements, X-ray photoelectron spectroscopy (XPS), and Mott-Schottky analysis. Optical studies reveal lower absorption in Co-doped materials, with a slight shift in band gap energies. Photoelectrochemical (PEC) analysis demonstrates improved PEC activity for Co-doped layers, with the observed shift in photocurrent onset potential attributed to both cobalt and fluoride ions catalytic effects. The study includes an in-depth discussion of the observed phenomena and their implications for applications in solar water splitting, emphasizing the potential of the anodic Co-F-WO3 layers as efficient photoelectrodes. In addition, the research presents a comprehensive exploration of the electrochemical synthesis and characterization of anodic Co-F-WO3, emphasizing their photocatalytic properties for the oxygen evolution reaction (OER). It was found that Co-doped WO3 materials exhibited higher PEC activity, with a maximum 5-fold enhancement compared to pristine materials. Furthermore, the studies demonstrated that these photoanodes can be effectively reused for PEC water-splitting experiments.
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  • 文章类型: Journal Article
    在这项研究中,我们评估了通过各种施加电压序列通过阳极氧化制造的直径定制的TiO2纳米管层的药物释放行为:常规的恒定施加电位为20V(45nm)和60V(80nm),20/60V步进电位(50nm[两个直径]),和20-60V扫描电位(49nm[全锥形])(括号中的值表示纳米管层顶部的内管直径)。50nm(两个直径)和49nm(全锥形)样品的结构在纳米管层顶部的内径小于80nm样品的内径,而纳米管层底部的外径与80nm样品的尺寸几乎相同。80nm的样品,具有最大的纳米管直径和长度,展示了最大的爆发释放,其次是50nm(两个直径),49nm(全锥形),和45nm样品。较小的管顶部显著抑制了从50nm(两个直径)和49nm(全锥形)样品的初始突释药物量和释放速率。另一方面,对于50nm(两个直径)样品,观察到缓慢释放的药物量占总释放药物量的最大比例。因此,50nm(两个直径)实现了抑制的初始爆发释放和大的存储容量。因此,这项研究,第一次,应用具有调制直径(两个直径和全锥形)的TiO2纳米管层以实现具有定制药物释放特性的局部药物递送系统(LDDS)。
    In this study, we evaluated the drug release behavior of diameter customized TiO2 nanotube layers fabricated by anodization with various applied voltage sequences: conventional constant applied potentials of 20 V (45 nm) and 60 V (80 nm), a 20/60 V stepped potential (50 nm [two-diameter]), and a 20-60 V swept potential (49 nm [full-tapered]) (values in parentheses indicate the inner tube diameter at the top part of nanotube layers). The structures of the 50 nm (two-diameter) and 49 nm (full-tapered) samples had smaller inner diameters at the top part of nanotube layers than that of the 80 nm sample, while the outer diameters at the bottom part of nanotube layers were almost the same size as the 80 nm sample. The 80 nm sample, which had the largest nanotube diameter and length, exhibited the greatest burst release, followed by the 50 nm (two-diameter), 49 nm (full-tapered), and 45 nm samples. The initial burst released drug amounts and release rates from the 50 nm (two-diameter) and 49 nm (full-tapered) samples were significantly suppressed by the smaller tube top. On the other hand, the largest proportion of the slow released drug amount to the total released drug amount was observed for the 50 nm (two-diameter) sample. Thus, 50 nm (two-diameter) achieved suppressed initial burst release and large storage capacity. Therefore, this study has, for the first time, applied TiO2 nanotube layers with modulated diameters (two-diameter and full-tapered) to the realization of a localized drug delivery system (LDDS) with customized drug release properties.
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  • 文章类型: Journal Article
    钛的临床使用历史悠久,但是自然形成的氧化物对于细菌抗性并不理想。阳极氧化过程可以改变结晶度,表面形貌,和钛氧化物的表面化学。锐钛矿,金红石,已知和混合相氧化物在UVA辐照下表现出光催化活性(PCA)驱动的细菌抗性。据报道,银添加增强PCA并减少细菌附着。这项研究调查了银掺杂添加剂对三种已建立的阳极氧化过程的影响。银掺杂对氧化物结晶度没有显著影响,表面形貌,或表面润湿性。来自硫酸阳极氧化过程的氧化物在银掺杂后表现出显着增强的PCA,但是由含磷酸的电解质产生的银掺杂的氧化物没有。还在黑暗和UVA照射条件下对每种氧化物评估金黄色葡萄球菌的附着。与黑暗条件相比,每种氧化物均表现出光催化抗微生物作用,这表明在UVA辐射下细菌附着显着降低。然而,由于银掺杂,只有磷掺杂的混合锐钛矿和金红石相氧化物在UVA辐照下表现出细菌附着的显着减少。这种氧化物的抗微生物成功归因于混合相氧化物和更高的银掺杂吸收水平的组合。
    Titanium has a long history of clinical use, but the naturally forming oxide is not ideal for bacterial resistance. Anodization processes can modify the crystallinity, surface topography, and surface chemistry of titanium oxides. Anatase, rutile, and mixed phase oxides are known to exhibit photocatalytic activity (PCA)-driven bacterial resistance under UVA irradiation. Silver additions are reported to enhance PCA and reduce bacterial attachment. This study investigated the effects of silver-doping additions to three established anodization processes. Silver doping showed no significant influence on oxide crystallinity, surface topography, or surface wettability. Oxides from a sulfuric acid anodization process exhibited significantly enhanced PCA after silver doping, but silver-doped oxides produced from phosphoric-acid-containing electrolytes did not. Staphylococcus aureus attachment was also assessed under dark and UVA-irradiated conditions on each oxide. Each oxide exhibited a photocatalytic antimicrobial effect as indicated by significantly decreased bacterial attachment under UVA irradiation compared to dark conditions. However, only the phosphorus-doped mixed anatase and rutile phase oxide exhibited an additional significant reduction in bacteria attachment under UVA irradiation as a result of silver doping. The antimicrobial success of this oxide was attributed to the combination of the mixed phase oxide and higher silver-doping uptake levels.
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  • 文章类型: Journal Article
    利用单步阳极氧化技术开发纳米多孔结构被公认为是用于多种应用的成本有效且简单的方法。在目前的工作中,利用草酸作为电解质,在40V的连续电压下开发出具有纳米多孔结构的阳极氧化氧化铝。由于其对宽带太阳光谱能量的高吸收率,所形成的纳米多孔结构可用于脱盐应用。海水淡化装置由两个太阳能剧照组成,即常规和改良。将开发的结构放置在修改的静止中以检查其性能。观察到,该结构通过纳米孔吸收来自太阳的光子能量并为水蒸气提供有效的途径以发展有效的脱盐作用,从而将热量分配给周围的水。纳米多孔结构具有〜45nm的平均直径。此外,发现纳米多孔结构的带隙能量为〜2.5eV(吸收光谱拟合)和〜2.8eV(Tauc图)。纳米多孔结构具有太阳区域中的可见光光谱,这有助于纳米多孔结构的带隙提供额外的能量供应以产生更多的水蒸发。此外,该结构的Urbach能量为0.5eV,这表明改性后的缺陷较少。与常规相比,改性蒸馏物的总馏出物收率增加到21%。海水淡化实验前后也进行了水质分析,结果在世界卫生组织(WHO)设定的可接受范围内。
    Development of nanoporous structures utilizing a single step of anodization technique is well recognized as a cost-effective and straightforward approach for several applications. In the current work, anodized alumina was developed with nanoporous structure by utilizing oxalic acid as an electrolyte with a continuous voltage of 40 V. The formed nanoporous structure was subjected to desalination application because of its high absorbance of broadband solar spectrum energy. The desalination setup consists of two solar stills namely conventional and modified. The developed structure is placed in the modified still to examine its performance. It was observed that the structure distributing heat to surrounding water by absorbing photon energy from the sun through the nanopores and giving an efficient pathway to the water vapours for developing effective desalination. The nanoporous structure having ~ 45 nm average diameter. Furthermore, the band gap energy of nanoporous structure was found to be ~ 2.5 eV (absorption spectrum fitting) and ~ 2.8 eV (Tauc plot). The nanoporous structure possess the visible light spectra in solar region which helps the band gaps of nanoporous structure to provide an additional supply of energy for generating more water to evaporate. Moreover, the Urbach energy of the structure is 0.5 eV which reveals less defects in the modified still. The overall distillate yield of modified still was increased to 21% in contrast to conventional. Water quality analysis was also carried out before and after the desalination experiments, and the results were within acceptable limits set by World Health Organization (WHO).
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  • 文章类型: Journal Article
    分析药品是生产设施中的质量控制要求。这项研究提出了一种基于CuO电极的可重复使用的非酶传感器,作为快速分析葡萄糖输注中葡萄糖水平的替代方法。CuO被广泛用作非酶葡萄糖传感器中的电极材料。传统上,这些电极是使用CuO的化学合成然后固定到电极基底上制造的。相比之下,在这里,Cu金属被机械改性以产生沟槽表面,然后进行电化学阳极氧化和随后的退火工艺,以原位生长出具有增强的催化活性的无缝CuO层。使用扫描电子显微镜(SEM)和X射线衍射仪(XRD)对电极的形貌进行了表征。通过循环伏安法详细研究了开发的CuO修饰电极对碱性介质中葡萄糖氧化的直接电催化活性。CuO修饰的电极在0.10V左右开始氧化过程Ag伪参比电极,与裸Cu电极相比,葡萄糖氧化的过电压显着降低。该传感器能够在低氧化电位(如0.2V)下检测葡萄糖,灵敏度值为0.37µAppm-1,宽线性范围(80-2300ppm),定量限(LOQ)为1ppm,更大的可重复性,1%的精度,3%的偏差,响应时间短(80秒),良好的重现性和优异的可重用性(196次连续尝试)。增强的性能和成本效益使该传感器成为葡萄糖注射液中产品分析的有前途的替代方法。
    Analyzing pharmaceutical products is a quality control requirement in a production facility. This study presents a CuO electrode-based reusable non-enzymatic sensor as an alternative method for rapid analysis of glucose levels in glucose infusions. CuO is extensively employed as an electrode material in non-enzymatic glucose sensors. Conventionally, these electrodes are fabricated using chemical synthesis of CuO followed by immobilization to the electrode substrate. In contrast, here, Cu metal was mechanically modified to create a grooved surface, followed by electrochemical anodization and subsequent annealing process to grow a seamless CuO layer in situ with enhanced catalytic activity. The morphology of the electrodes was characterized using scanning electron microscopy (SEM) and X-ray diffractometry (XRD). The direct electrocatalytic activity of the developed CuO-modified electrode towards glucose oxidation in alkaline media was investigated by cyclic voltammetry in detail. The CuO-modified electrode commenced the oxidation process around 0.10 V vs. Ag pseudo-reference electrode, demonstrating a significant reduction in the overvoltage for glucose oxidation compared to the bare Cu electrode. The sensor is capable of detecting glucose at low oxidation potentials such as 0.2 V with a sensitivity value of 0.37 µA ppm-1, a wide linear range (80-2300 ppm), limit of quantification (LOQ) of 1 ppm, greater repeatability, 1% precision, 3% bias, a short response time (80 s), good reproducibility and excellent reusability (196 consecutive attempts). The enhanced performance and cost-effectiveness make this sensor a promising alternative method for product analysis in glucose injection solutions.
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  • 文章类型: Journal Article
    具有极大表面积的Ni纳米线阵列电极是通过电化学还原工艺,利用孔长为320μm的阳极氧化铝模板制成的,孔径为100nm,和孔径比3200。无论沉积电势如何,电沉积的Ni纳米线阵列都优先在(111)平面上取向,并且表现出单轴磁各向异性,并且在轴向方向上容易磁化。关于磁性,电沉积Ni纳米线阵列的矩形度和矫顽力提高到0.8和550Oe,分别。还证实,通过增加纵横比抑制了磁化反转,并且改善了硬磁性能。还研究了电沉积Ni纳米线阵列上析氢的电催化性能,并将氢过电压降低至〜0.1V,几乎比电沉积Ni膜低0.2V。此外,在-1.0V和-1.5V时析氢的电流密度与Ag/AgCl分别增加到约-580A/m2和-891A/m2,由于电沉积Ni纳米线阵列的极大表面积。
    Ni nanowire array electrodes with an extremely large surface area were made through an electrochemical reduction process utilizing an anodized alumina template with a pore length of 320 µm, pore diameter of 100 nm, and pore aspect ratio of 3200. The electrodeposited Ni nanowire arrays were preferentially oriented in the (111) plane regardless of the deposition potential and exhibited uniaxial magnetic anisotropy with easy magnetization in the axial direction. With respect to the magnetic properties, the squareness and coercivity of the electrodeposited Ni nanowire arrays improved up to 0.8 and 550 Oe, respectively. It was also confirmed that the magnetization reversal was suppressed by increasing the aspect ratio and the hard magnetic performance was improved. The electrocatalytic performance for hydrogen evolution on the electrodeposited Ni nanowire arrays was also investigated and the hydrogen overvoltage was reduced down to ~0.1 V, which was almost 0.2 V lower than that on the electrodeposited Ni films. Additionally, the current density for hydrogen evolution at -1.0 V and -1.5 V vs. Ag/AgCl increased up to approximately -580 A/m2 and -891 A/m2, respectively, due to the extremely large surface area of the electrodeposited Ni nanowire arrays.
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