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Secondary micro- and nanostructures on the surface of microwave carbonized cotton fibers 微波碳化棉纤维表面的二次微结构和纳米结构
Pub Date : 2024-06-01 DOI: 10.30791/0015-3214-2023-6-57-74
E. V. Matveev, A. Gaidar, B. Lapshinov, V. V. Berestov
The method of scanning electron microscopy and X-ray microanalysis was used to study the morphology and surface composition of cotton lint fibers carbonized by microwave radiation and secondary micro- and nanostructures formed on the surface of the fibers in the process of carbonization. The mass of 3 g of cotton lint treated with 5 at. % H3PO4 solution and having a cylindrical form with transverse notches was used as samples for microwave carbonization. It was shown that impurity elements contained in the initial fibers move during microwave carbonization from the central region of the sample to the marginal zones, where they are deposited on the fibers both as continuous phosphorus-containing coatings and as micro- and nanostructures with different morphology and composition. It was found that the most difficult to remove impurities are P and Ca. On the surfaces of notches of microwave carbonized samples, mainly in the central part, there are areas of deep black color characteristic of activated carbon. It is shown that the carbonized fibers of these areas do not contain impurity elements. Significant differences in the morphology of the fiber surface in this area were found. Four characteristic types of fiber surface structure were revealed. In similar areas of samples without notches, carbonized earlier, the fiber surface always contained a small amount of impurity elements (phosphorus ~ 3 – 6 at. %, calcium ~ 1 – 3 at. %), and the fiber structure was fairly uniform. Secondary carbon structures of various morphologies were found on the surfaces of the cuts: monolithic carbon deposits with a hummocky and platelet structure, thin transparent films (presumably, graphene-like structures), carbon nanofibers and nanotubes (straight and curved, diameter 70 – 150 nm and several microns long). A large variety of structures of carbon products and the absence of impurities in them is due to the high heterogeneity of the process conditions in the slit gap, within which microplasma spots, spark and arc discharges arise.
采用扫描电子显微镜和 X 射线显微分析方法研究了经微波辐射碳化的棉绒纤维的形态和表面成分,以及碳化过程中在纤维表面形成的次生微结构和纳米结构。微波碳化的样品是用 5 % H3PO4 溶液处理过的棉绒,质量为 3 克,呈带横向缺口的圆柱形。结果表明,在微波碳化过程中,初始纤维中所含的杂质元素会从样品的中心区域移动到边缘区域,并以连续含磷涂层和具有不同形态和成分的微纳米结构的形式沉积在纤维上。研究发现,最难去除的杂质是 P 和 Ca。在微波碳化样品的凹口表面,主要是中央部分,有活性炭特有的深黑色区域。结果表明,这些区域的碳化纤维不含杂质元素。该区域的纤维表面形态存在显著差异。纤维表面结构有四种特征类型。在没有缺口、碳化较早的类似样品区域,纤维表面总是含有少量杂质元素(磷 ~ 3 - 6 at.在切口表面发现了形态各异的次生碳结构:具有驼峰状和板状结构的整体碳沉积、透明薄膜(推测为类似石墨烯的结构)、纳米碳纤维和纳米管(直的和弯的,直径 70 - 150 纳米,长几微米)。碳产品的结构种类繁多且不含杂质,这是因为狭缝间隙中的工艺条件具有高度异质性,在狭缝间隙中会产生微等离子点、火花放电和电弧放电。
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引用次数: 0
W – C – Co composite nanopowder treatment in microwave electromagnetic field 在微波电磁场中处理 W - C - Co 复合纳米粉体
Pub Date : 2024-06-01 DOI: 10.30791/0015-3214-2023-5-47-57
A. Samokhin, N. Alekseev, M. Sinayskiy, A. Astashov, A. Vodopyanov, A. A. Sorokin, S. Sintsov
Experiments were carried out on the treatment of the W – C – Co system nanopowders obtained by plasma chemical synthesis in a microwave electromagnetic field with a frequency of 2.45 and 24 GHz in different gas media. The effect of treatment time, power input and carbon content in the treated nanopowder on the yield of tungsten monocarbide WC was investigated.
在频率为 2.45 和 24 千兆赫的微波电磁场中,在不同的气体介质中对等离子化学合成得到的 W - C - Co 系纳米粉体进行了处理实验。研究了处理时间、输入功率和处理纳米粉体中碳含量对碳化钨产量的影响。
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引用次数: 0
Structure and properties of bioinert Mo – Nb coating formed on Titanium Grade 5 medical alloy by electroexplosive method 用电爆法在 5 级医用钛合金上形成的生物惰性钼-铌涂层的结构和性能
Pub Date : 2024-06-01 DOI: 10.30791/0015-3214-2023-4-47-64
D. Romanov, K. V. Sosnin, S. Pronin, V. Pochetukha, Yu.F. Ivanov, V. E. Gromov
In this article, an attempt was made to solve the problem of creating a coating for an implant that has better biological compatibility than the medical titanium alloy Titanium Grade 5. A Mo – Nb coating of the composition Mo – Nb is formed on the titanium grade 5 medical alloy by the electroexplosive method. The coating is formed as a result of the simultaneous electric explosion of molybdenum and niobium foils. A set of studies has been carried out to establish the structure, phase composition, and properties of the formed coatings. The coatings were studied by scanning and transmission electron microscopy. It is shown that the hardness of the surface layer of the coating by 60 % and Young’s modulus by 43 % exceed the corresponding characteristics of the Titanium Grade 5 alloy. The thickness of the layer with high (relative to the substrate) values of hardness and Young’s modulus reaches 80 µm. It was found that the wear parameter of the coating is 1.8 times, and the friction coefficient of the coating is 1.6 times higher than the wear parameter and the friction coefficient of the substrate. It has been established that in the surface layer, along with the coating atoms, there are Al, Ti, V atoms, which indicates that the coating is doped with substrate atoms, as well as oxygen and carbon atoms. The layering of the coating by elemental composition was revealed, namely, the top of the coating is enriched with niobium atoms, the lower part of the coating is enriched with molybdenum atoms. It is shown that the coating has a polycrystalline structure formed by a solid solution based on molybdenum. In the bulk and along the grain boundaries, there are inclusions of the second phase of the composition a-Ti, Nb, Mo9Ti4, and NbTi4 of various shapes and sizes. The studies of the phase composition did not reveal compounds based on vanadium and aluminum, which reduce the biocompatibility of the coatings. The identified phases contain only molybdenum, niobium and titanium, which are bioinert. This fact suggests that, as in studies of the phase composition of the surface of the coatings and its change in thickness, the biocompatibility of the obtained coatings will be higher compared to the Titanium Grade 5 titanium alloy. The conducted complex of studies makes it possible to recommend the resulting coatings for further clinical trials. These coatings are expected to be used in the future for better survival of titanium implants in the human body.
本文试图解决为植入物制造一种生物相容性优于医用钛合金 5 级钛的涂层的问题。通过电爆法在 5 级医用钛合金上形成了钼-铌涂层。该涂层是钼箔和铌箔同时电爆的结果。为确定所形成涂层的结构、相组成和性能,进行了一系列研究。通过扫描和透射电子显微镜对涂层进行了研究。结果表明,涂层表层的硬度比 5 级钛合金的相应特性高出 60%,杨氏模量高出 43%。硬度和杨氏模量值较高(相对于基体)的涂层厚度达到 80 µm。研究发现,涂层的磨损参数是基体的 1.8 倍,摩擦系数是基体的 1.6 倍。研究证实,在表层中,除了涂层原子外,还有 Al、Ti、V 原子,这表明涂层中掺杂了基体原子以及氧原子和碳原子。揭示了涂层按元素组成的分层情况,即涂层顶部富含铌原子,涂层下部富含钼原子。研究表明,涂层具有以钼为基础的固溶体形成的多晶结构。在基体和沿晶界处,存在不同形状和大小的第二相 a-Ti、Nb、Mo9Ti4 和 NbTi4 杂质。对相组成的研究没有发现基于钒和铝的化合物,这些化合物会降低涂层的生物相容性。已确定的相只含有钼、铌和钛,它们是生物惰性的。这一事实表明,通过对涂层表面相组成及其厚度变化的研究,所获得涂层的生物相容性将高于 5 级钛合金。通过这些综合研究,我们可以建议对所获得的涂层进行进一步的临床试验。这些涂层有望在未来用于提高钛植入物在人体内的存活率。
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引用次数: 0
Structural and morphological peculiarities of montmorillonite treated with microwave radiation 微波处理蒙脱土的结构和形态特性
Pub Date : 1900-01-01 DOI: 10.30791/0015-3214-2019-3-5-12
A. G. Chetverikova, O. N. Kanygina, M. Filyak, S. A. Ogerchuk
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引用次数: 0
Oxidation of zirconium alloyed with chromium atoms by means of compression plasma flows impact 用压缩等离子体流冲击氧化铬原子锆合金
Pub Date : 1900-01-01 DOI: 10.30791/0015-3214-2023-3-18-32
V. Shymanski, V. V. Sheveleva, V. Uglov, V. Astashynski, A. Kuzmitski
The results of investigation of the zirconium structure on the first stage of oxidation at temperature 700 °C in the air atmosphere after 15 minutes are presented. The commercial pure zirconium alloy as well as zirconium alloyed with chromium atoms by means of compression plasma flows impact are investigated. The results showed the possibility to form the top layer in zirconium alloyed with chromium when a thin chromium coating (1 mm) was deposited on the surface and the compression plasma flow with the absorbed energy density 25 – 43 J/cm2 influenced. Due to alloying with chromium, the high-temperature β-phase of zirconium is stabilized at room temperature as β-Zr(Cr) solid solution and martensite α′-Zr phase is formed. The oxidation at temperature 700 °C demonstrated the higher oxidation resistance of the zirconium samples treated with compression plasma flows at the highest absorbed energy density 43 J/cm2. This regime modified the top layer of the zirconium sample without β-Zr(Cr) solid solution formation which enhances the oxygen diffusion.
本文介绍了在700℃空气气氛中氧化15分钟后第一阶段锆结构的研究结果。用压缩等离子体流冲击的方法对工业纯锆合金和铬原子锆合金进行了研究。结果表明,在铬锆合金表面沉积1 mm的薄铬层,影响吸收能量密度为25 ~ 43 J/cm2的压缩等离子体流,有可能形成顶层。由于与铬的合金化作用,锆的高温β相在室温下稳定为β-Zr(Cr)固溶体,形成马氏体α′-Zr相。在700℃的氧化条件下,压缩等离子体流处理的锆样品具有较高的抗氧化性,吸收能量密度最高为43 J/cm2。这一机制修饰了锆样品的顶层,没有形成β-Zr(Cr)固溶体,增强了氧的扩散。
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引用次数: 0
Degradation of spacecraft’s thermo control coatings during deposition of thin Au films 航天器热控制涂层在金薄膜沉积过程中的退化
Pub Date : 1900-01-01 DOI: 10.30791/0015-3214-2019-1-35-42
A. Nadiradze, G. V. Panasova, R. R. Rakhmatullin, V. A. Smirnov
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引用次数: 0
Changes in the composition and corrosion-electrochemical properties of the chromium-nickel steel 03Cr18Ni11 during implantation of argon, oxygen and nitrogen ions 氩、氧、氮离子注入对铬镍钢03Cr18Ni11组成及腐蚀电化学性能的影响
Pub Date : 1900-01-01 DOI: 10.30791/0015-3214-2023-3-5-17
S. G. Bystrov, S. Reshetnikov, A. Kolotov, V. Bayankin
The effect of implantation of argon, oxygen and nitrogen ions on the physicochemical structure of the surface and the corrosion-electrochemical behavior of chromium-nickel steel 03Cr18Ni11has been studied. Methods of electrochemical polarization (EP), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS) were used. Ion implantation of argon, oxygen and nitrogen leads to an increase in the corrosion resistance of steel 03Cr18Ni11 both in a neutral environment and in the presence of a corrosion activator (chloride anions), while irradiation with argon ions is most effective. It was found that after implantation of argon ions, a partial etching of the steel surface occurs, i.e. an increase in the true surface. This, in turn, facilitates the onset of the passive state. At the same time, the use of oxygen and nitrogen ions leads to smoothing of the surface. AFM data indicate that the studied steel treated with argon ions exhibits the greatest resistance to local corrosion. The implantation of oxygen and argon ions reduces the overall corrosion to the greatest extent. It is important to note that deep craters and traces of pitting corrosion do not form on the surface of the steel. The XPS data show that after ion implantation, there was a change in the concentration of the elements that make up the steel in the near-surface layers of the material in the depth of the implanted layer compared with the non-irradiated sample. It is established that the surface layers of steel are enriched with chromium atoms during ion implantation. This process occurs most intensively when samples are treated with argon ions. In this case, mixed chromium and iron oxides are formed, contributing to the passivation of the steel surface. Also, the process of ion implantation is accompanied by oxidation of the surface of the steel under study. This is confirmed by an increase in the oxygen content in the surface layers. To the greatest extent, this process occurs during implantation of oxygen ions. After corrosion tests, an increased chromium content is also observed on the surface of steel treated with Ar+ ions, which confirms the formation in this case of strong chromium oxides that remain on the surface during the corrosion of steel. The analysis of the fine structure of the XPS spectra showed that under the action of argon ions, the oxygen of surface oxides is redistributed in favor of chromium atoms and the formation of strong mixed iron and chromium oxides of the spinel type, including Fe2+, Fe3+, Cr3+ and Cr6+ compounds. It is important to note that although chromium oxides are also formed during oxygen implantation and in the same quantities as during argon implantation, the protective properties of the resulting compounds are noticeably lower. Therefore, not only the chemical composition is important, but also the structure of the resulting layers. It can be assumed that the high kinetic energy of heavy argon ions affects both the formation of a de
研究了氩、氧、氮离子注入对铬镍钢03cr18ni11表面物理化学结构和腐蚀电化学行为的影响。采用电化学极化(EP)、原子力显微镜(AFM)和x射线光电子能谱(XPS)等方法进行分析。在中性环境和有腐蚀活化剂(氯离子)存在的情况下,注入氩、氧和氮离子均能提高03Cr18Ni11钢的耐蚀性,其中氩离子辐照最有效。结果表明,氩离子注入后,钢的表面发生了局部腐蚀,即真实表面增大。这反过来又促进了被动状态的开始。同时,氧和氮离子的使用导致表面光滑。原子力显微镜数据表明,经氩离子处理的钢具有最佳的抗局部腐蚀性能。氧离子和氩离子的注入最大程度地降低了整体腐蚀。值得注意的是,深坑和点蚀痕迹不会在钢的表面形成。XPS数据表明,离子注入后,与未辐照样品相比,注入层深处材料近表层中组成钢的元素浓度发生了变化。结果表明,在离子注入过程中,钢的表层富集了铬原子。当样品用氩离子处理时,这一过程发生得最强烈。在这种情况下,形成混合的铬和铁的氧化物,有助于钢表面的钝化。同时,离子注入过程伴随着钢的表面氧化。表层氧含量的增加证实了这一点。在最大程度上,这个过程发生在氧离子的注入过程中。在腐蚀试验之后,在经Ar+离子处理的钢的表面上还观察到铬含量增加,这证实在这种情况下,在钢腐蚀过程中,在表面上形成了强铬氧化物。XPS光谱的精细结构分析表明,在氩离子的作用下,表面氧化物中的氧被重新分配到有利于铬原子的位置,形成尖晶石型强铁铬混合氧化物,包括Fe2+、Fe3+、Cr3+和Cr6+化合物。值得注意的是,虽然在氧气注入过程中也会形成氧化铬,其数量与氩气注入过程中相同,但所产生的化合物的保护性能明显较低。因此,不仅化学成分很重要,所产生的层的结构也很重要。可以认为,重氩离子的高动能既影响了发育的表面浮雕的形成,也影响了尖晶石型强铁铬混合氧化物的形成。
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引用次数: 0
Waterjet cutting of permanent magnets from Fe – Co – Ni – Cu – Al – Ti alloys
Pub Date : 1900-01-01 DOI: 10.30791/0015-3214-2022-6-76-80
I. Belyaev, N. M. Zaytsev, Yu. V. Rudnitsky
The possibility of waterjet cutting of permanent magnets of the Fe – Co – Ni – Cu – Al – Ti system was investigated. The OMAX 555 JetMachining Center XX waterjet cutting machine was used. Permanent magnet blanks intended for cutting had a thickness of 2 and 5 mm. The cutting process was carried out in air. The cutting speed varied between 50 – 250 mm/min. The magnetic properties of the studied workpieces were measured before and after waterjet cutting by recording demagnetization curves. Changes in the chemical and phase composition of the studied alloys were evaluated by X-ray fluorescence and X-ray phase analysis. It was found that permanent magnets 2 – 5 mm thick can be cut without causing any mechanical damage to their surface. At the same time, the chemical and phase composition of the permanent magnet material practically does not change. The magnetic properties of permanent magnets do not decrease or even increase. The thickness of the cut is not more than 0.5 mm. Cutting modes can be optimized for workpieces of different thicknesses.
研究了水射流切割Fe - Co - Ni - Cu - Al - Ti系永磁体的可能性。采用OMAX 555 JetMachining Center XX型水射流切割机。用于切割的永磁体坯的厚度为2和5毫米。切割过程在空气中进行。切割速度在50 - 250mm /min之间变化。通过记录消磁曲线,测量了水射流切割前后工件的磁性能。通过x射线荧光和x射线相分析,评价了所研究合金的化学成分和相组成的变化。研究发现,2 - 5mm厚的永磁体可以切割而不会对其表面造成任何机械损伤。同时,永磁材料的化学成分和相组成几乎没有变化。永磁体的磁性能不降低,甚至不增加。切割厚度不大于0.5 mm。可针对不同厚度的工件优化切削方式。
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引用次数: 0
The effect of argon and oxygen ion implantation on the physicochemical and corrosion-electrochemical properties of 14Cr17Ni2 chromium-nickel steel 氩离子和氧离子注入对14Cr17Ni2铬镍钢物理化学和腐蚀电化学性能的影响
Pub Date : 1900-01-01 DOI: 10.30791/0015-3214-2021-4-5-14
S. G. Bystrov, S. Reshetnikov, E. Borisova, I. N. Klimova, A. Kolotov, A. V. Zhikharev, V. Bayankin
The effect of argon and oxygen ion implantation both in separate and joint was carried out. Physical and chemical structure of the surface and corrosion-electrochemical behavior of 14Cr17Ni2 chromium-nickel steel was studied. Methods of potentiometry, atomic force microscopy, X-ray photoelectron spectroscopy, and microhardness measurement were used. It was found that the initial chromium-nickel steel exhibits high corrosion resistance in the medium of a borate buffer solution with the addition of a local corrosion initiator — potassium sulfate. However, steel was found to be susceptible to local (pitting) corrosion in this environment. It is shown that the implantation of argon and oxygen ions changes the nature of the corrosion-electrochemical behavior of chromium-nickel steel. Treatment with Ar+ ions enriched the sample surface with Cr atoms and reduces the overall corrosion losses of steel, but is characterized by the maximum value of local corrosion. Treatment with O+ ions provide optimal results in terms of reducing local and general corrosion. It was found that in this case, the sample surface is intensively oxidized to a depth of more than 20 nm, resulting in the formation of mixed oxides that are resistant to corrosion. There is a process similar to electropolishing of the sample surface due to partial dissolution of steel. Defects in the structure of the sample surface, on which pitting corrosion began, are “healed”. Joint treatment with Ar+ ions and O+ ions does not give noticeable advantages compared to separate implantation with these ions. Corrosion losses for samples treated only with O+ ions and Ar+ ions together with O+ ions did not exceed those for the original sample, although there are practically no passivation regions on the potentiodynamic curves. Microhardness of the samples after ion implantation coincides with the microhardness of the original sample. Result of ion implantation is no significant for change in the structural and phase structure of the surface layers of chromium-nickel steel. Ion implantation will not negatively affect the physical and mechanical properties of studied steel. The research shows that it is advisable to choose the type of implantable ions and the optimal process parameters depending on the steel grade and its application. For these purposes, the research methodology proposed in this article will be useful.
研究了氩离子和氧离子分别注入和联合注入的效果。研究了14Cr17Ni2铬镍钢的表面物理化学结构和腐蚀电化学行为。采用电位法、原子力显微镜、x射线光电子能谱、显微硬度测定等方法。结果表明,在硼酸盐缓冲溶液中加入局部腐蚀引发剂硫酸钾后,初始铬镍钢具有较高的耐腐蚀性。然而,人们发现钢在这种环境下容易受到局部(点蚀)腐蚀。结果表明,氩离子和氧离子的注入改变了铬镍钢腐蚀电化学行为的性质。Ar+离子处理使试样表面富集了Cr原子,降低了钢的整体腐蚀损失,但其特点是局部腐蚀值最大。用O+离子处理在减少局部和整体腐蚀方面提供了最佳结果。结果发现,在这种情况下,样品表面被强烈氧化,深度超过20nm,形成了耐腐蚀的混合氧化物。由于钢的部分溶解,样品表面有一个类似电抛光的过程。在试样表面的结构中,开始点蚀的缺陷被“愈合”。与单独注入Ar+离子和O+离子相比,Ar+离子和O+离子联合处理没有明显的优势。虽然在动电位曲线上几乎没有钝化区,但仅用O+离子、Ar+离子和O+离子处理的样品的腐蚀损失没有超过原始样品。离子注入后样品的显微硬度与原样品的显微硬度一致。离子注入对铬镍钢表层组织和相结构的影响不显著。离子注入不会对所研究钢的物理力学性能产生负面影响。研究表明,可根据不同的钢种和不同的应用场合选择注入离子的种类和最佳工艺参数。对于这些目的,本文提出的研究方法将是有用的。
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引用次数: 0
Structural modification of fine powders of overburden rocks of saponite-containing bentonite clay 含皂石膨润土覆岩细粉的结构改性
Pub Date : 1900-01-01 DOI: 10.30791/0015-3214-2023-1-56-63
A. Ayzenshtadt, E. Korolev, M. Malygina, T. Drozdyuk, M. Frolova
The kinetic regularities of the process of structural modification of highly dispersed powders of saponite-containing material after mechanical dispersion have been studied. As information criteria characterizing the restructuring of the crystal lattice of minerals, changes are used that occur with the specific surface of powders at different grinding times and the exothermic thermal effect (enthalpy change) in the temperature range of 810 – 820 °С. It has been determined that during mechanical grinding of a saponite-containing material for more than 20 minutes, intensive modification of saponite occurs, associated with its structural changes, leading to the formation of serpentine. It has been established that the traditionally used criterion for evaluating the process of mechanical grinding of raw materials by the specific surface of the powder in this case is not a sufficient information parameter when optimizing structural changes in experimental samples. The dominant parameter of this process is the enthalpy factor, which characterizes the thermal effect of the structural modification.
研究了高分散皂矿粉体机械分散后结构改性过程的动力学规律。作为表征矿物晶格重构的信息标准,采用了粉体在不同磨矿时间比表面的变化以及在810 ~ 820°С温度范围内的放热热效应(焓变)。经测定,含皂石物料在机械研磨超过20分钟的过程中,皂石发生强烈的改性,其结构发生变化,导致蛇纹石的形成。在优化实验样品的结构变化时,传统的用粉体比表面来评价原料机械研磨过程的准则并不是一个足够的信息参数。这一过程的主要参数是焓因子,它表征了结构改性的热效应。
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引用次数: 0
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Physics and Chemistry of Materials Treatment
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