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Crack resistance, strength and dynamic fatigue of quartz fibers with copper coatings 铜涂层石英纤维的抗裂性、强度和动态疲劳性能
Pub Date : 2022-03-24 DOI: 10.17073/1997-308x-2022-1-57-65
M. I. Bulatov, A. Shatsov, N. S. Grigoryev, N. Malkov
Metallized coatings can significantly improve the operational properties of quartz fibers. The research was conducted to determine the crack resistance, strength and dynamic fatigue of optical fibers without any coating and with copper coatings. The microhardness of quartz fibers was measured by the diamond indentation of end surfaces. The stress intensity parameter K1c was found from the A. Niihara semi-empirical dependence. The geometry of indentation and radial cracks was studied using a scanning electron microscope. The crack resistance of uncoated quartz turned out to be almost 3 times less as compared to the copper coating fiber, which is presumably due to the additive contribution of compressive stresses on fiber surfaces and quartz wetting with copper. Copper-coated optical fiber drawing increases the tensile strength, crack resistance and dynamic fatigue parameter, and it is the main resource for maintaining operation in the conditions of a statistical approach to structural strength. Comparative tests were conducted to check the optical fiber strength by two-point bending and axial tension methods. Experimental tests conducted to check the ultimate mechanical strength of quartz optical fibers showed a significant spread of data, which indicates the presence of cracks of various sizes in a brittle solid and is a characteristic feature of brittle fracture as suggested by the A. Griffiths theory. In addition, it was assumed that the chaotic distribution of defects and microcracks extends along the entire length of a brittle solid, a quartz optical fiber in this case. A statistical model based on the Weibull distribution was used to describe surface microcracks depending on the fiber length. As a result, Weibull graphs were plotted in coordinates connecting the probability of failure with the strength, fiber length and parameter describing the ultimate strength.
金属化涂层可以显著改善石英纤维的使用性能。对无涂层光纤和镀铜光纤的抗裂性能、强度和动态疲劳性能进行了研究。采用端面金刚石压痕法测定了石英纤维的显微硬度。应力强度参数K1c由A. Niihara半经验依赖得到。用扫描电镜研究了压痕和径向裂纹的几何形状。结果表明,未包覆石英纤维的抗裂性能比包覆铜纤维低近3倍,这可能是由于纤维表面压应力的附加作用和石英被铜润湿所致。镀铜光纤拉伸提高了光纤的抗拉强度、抗裂性能和动态疲劳参数,是在结构强度统计方法的条件下维持运行的主要资源。采用两点弯曲法和轴向拉伸法对光纤的强度进行了对比试验。为检验石英光纤的极限机械强度而进行的实验测试显示,数据分布明显,这表明脆性固体中存在不同大小的裂纹,这是a . Griffiths理论提出的脆性断裂的特征。此外,假设缺陷和微裂纹的混沌分布沿着脆性固体的整个长度延伸,在这种情况下是石英光纤。采用基于威布尔分布的统计模型来描述随纤维长度变化的表面微裂纹。因此,将破坏概率与强度、纤维长度和描述极限强度的参数在坐标中绘制威布尔图。
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引用次数: 0
Production of finely dispersed titanium powder by volumetric reduction of its ions with sodium dissolved in the BaCl2–CaCl2–NaCl melt 用溶解在BaCl2-CaCl2-NaCl熔体中的钠对钛离子进行体积还原法制备细分散钛粉
Pub Date : 2022-03-24 DOI: 10.17073/1997-308x-2022-1-4-16
V. A. Lebedev, V. Polyakov
The research is intended to develop a technology for the production of finely dispersed (10 to 100 μm) powders of titanium and its alloys suitable for use in additive technologies after classification and spheroidization. A eutectic mixture was used as electrolyte, mole fractions: BaCl2 – 0.16, CaCl2 – 0.47, NaCl – 0.37, melting point of 452 °C. Electrolytes with a similar composition are used in industry for the electrolytic production of sodium with high current efficiency. No titanium salts were added to electrolyte. Sodium losses due to evaporation, corrosion, and ion recharge were replenished by a periodic increase in electrolysis current. A VT1-0 titanium plate was used as an anode. The walls of a steel crucible served as a cathode. Sodium was released on these walls and dissolved in electrolyte. Titanium ions were reduced in the bulk of electrolyte and in the anode layer. It is the first time that the results obtained were interpreted using the data on the electrode potentials of Ti3+/Ti, Ti2+/Ti, Ti3+/Ti2+ systems. It was shown that the concentration of slowly moving complex Ti3+ ions increases in the anode layer, and sodium dissolved in electrolyte reduces mainly Ti2+ ions in the electrolyte volume in the first 12 min of electrolysis. Starting from the 20th min, the concentration of Ti2+ ions in the anode layer begins to increase rapidly according to the reaction: 2Ti3+ + Ti = 3Ti2+ as titanium powder accumulates in the electrolyte volume. At the same time, the proportion of sodium consumed for the reduction of Ti3+ ions to Ti2+ decreases, which contributes to an increase in current efficiency and cathode potential stabilization for 30 minutes at –2.963 V. After the 50th min, the reactivity of the salt melt begins to decrease, the concentration of Ti3+ ions increases steadily until it levels off with the concentration of Ti2+ ions at the 85th min. This sharply increased the current consumption for ion recharge and made it necessary to stop electrolysis after switching on a current of 12 A for a short time (for 40 s). After 10 s, judging by the change in the cathode potential, sodium dissolved in electrolyte was almost completely consumed for titanium ion reduction. After 6 min, the potentials of electrodes returned to the initial anode potential value indicating that the system returned to its original state with the near-zero content of titanium salts and dissolved sodium. 95 % of powder was obtained in the electrolyte volume. Current efficiency was 84.0 % and turned out to be close to the value calculated from the average valence of titanium ions and the loss of anode weight (87.0 %). After ultrasonic dispersion, more than 80 % of powder was in the 10–100 μm range with a maximum at 36 μm. X-ray phase analysis showed that this is practically pure α-titanium (93.06 %) and oxygenated α-titanium (5.45 %). The originality of the research consists in the use of a volumetric, intensive, electrolytic method for producing finely dispersed titan
该研究旨在开发一种技术,用于生产精细分散(10 ~ 100 μm)的钛及其合金粉末,适合在分级和球化后用于添加剂技术。电解质为共晶混合物,摩尔分数为:BaCl2 - 0.16, CaCl2 - 0.47, NaCl - 0.37,熔点为452℃。具有类似成分的电解质在工业上用于电解生产具有高电流效率的钠。电解液中不添加钛盐。电解电流的周期性增加弥补了由于蒸发、腐蚀和离子补给而造成的钠损失。采用VT1-0钛板作为阳极。钢坩埚的壁用作阴极。钠被释放到这些壁上,溶解在电解质中。电解液和阳极层中钛离子均被还原。这是第一次用Ti3+/Ti、Ti2+/Ti、Ti3+/Ti2+体系的电极电位数据来解释所得结果。结果表明,阳极层中缓慢移动的络合Ti3+离子浓度增加,电解前12 min电解液中钠的溶解主要使电解液体积中的Ti2+离子减少。从第20分钟开始,随着钛粉在电解液体积内的积累,阳极层中Ti2+离子浓度根据2Ti3+ + Ti = 3Ti2+的反应开始快速增加。同时,减少了将Ti3+离子还原为Ti2+所消耗的钠的比例,这有助于提高电流效率和阴极电位在-2.963 V下稳定30分钟。50min后,盐液的反应性开始下降,Ti3+离子浓度稳步上升,直到85min时随Ti2+离子浓度趋于平稳。这使得离子充电消耗的电流急剧增加,需要在短时间内(40s)接通12a电流后停止电解。电解液中溶解的钠几乎被完全消耗,用于钛离子还原。6 min后,电极电位恢复到初始阳极电位值,表明体系恢复到初始状态,钛盐和溶解钠含量接近于零。95%的粉末是在电解液中得到的。电流效率为84.0%,接近由钛离子平均价和阳极重量损失计算的值(87.0%)。超声分散后,80%以上的粉末分布在10 ~ 100 μm范围内,最大分布在36 μm。x射线物相分析表明,该物质为纯α-钛(93.06%)和氧合α-钛(5.45%)。该研究的独创性在于使用体积,密集,电解方法来生产精细分散的钛粉,在初始和最终电解质中没有溶解的钠和氯化钛,在电流和电位的过程控制中逐步增加。该研究的独特之处在于所获得的钛粉,其主要部分以共生体的形式存在于熔体中,这些共生体很容易被超声波分散成单个晶体。超过80%的这些晶体在平均尺寸为36 μm的增材技术所需的10-100 μm范围内。
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引用次数: 0
Effect of chromium addition on the copper binder structure, properties and adhesion to diamond 添加铬对铜粘结剂结构、性能及与金刚石结合力的影响
Pub Date : 2022-03-24 DOI: 10.17073/1997-308x-2022-1-43-48
P. Loginov, G. M. Markov, S. Rupasov
The study covers the effect of chromium on the structure, mechanical properties, and adhesion of alloys used as a binder for metal-diamond composites. Cu–Cr powder mixtures were obtained by high-energy ball milling in a planetary centrifugal mill. This process was used to obtain two-phase Cu–Cr powders with uniformly distributed submicron Cr particles. Cu–Х%Cr compact samples (where Х = 10, 30 and 50 %) were obtained by hot pressing. It was found that Cu–30%Cr compact samples showed the best mechanical properties (9 times higher as compared to pure copper). These alloys feature a hardening mechanism based on the Hall–Petch law. The resulting alloys have a homogenous ultrafine structure, which results in high ultimate bending strength (2330 MPa). Chromium addition to the copper binder considerably increases its adhesion to diamond in metal-diamond composites due to chemical interaction between chromium included into the binder and diamond carbon with Cr3C2 carbide formation.
研究了铬对金属-金刚石复合材料的结构、机械性能和附着力的影响。采用行星离心磨高能球磨法制备了铜铬混合粉末。采用该工艺制备了具有均匀分布的亚微米级Cr颗粒的两相Cu-Cr粉末。通过热压得到Cu -Х %Cr压实样品(其中Х = 10,30和50%)。结果表明,Cu-30%Cr致密试样的力学性能最好,是纯铜的9倍。这些合金具有基于霍尔-佩奇定律的硬化机制。所得合金具有均匀的超细组织,具有较高的极限抗弯强度(2330 MPa)。在金属-金刚石复合材料中,铜结合剂中加入铬可显著提高其与金刚石的附着力,这是由于结合剂中的铬与金刚石碳发生化学作用,形成Cr3C2碳化物。
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引用次数: 0
Production of fibers based on polyacrylonitrile with magnetite nanoparticles 磁性纳米颗粒聚丙烯腈纤维的制备
Pub Date : 2021-12-10 DOI: 10.17073/1997-308x-2021-4-68-76
Z. Mansurov, G. Smagulova, B. Kaidar, A. Lesbayev, A. Imash
The paper presents the results of experiments on the production of composite fibers based on polyacrylonitrile (PAN) and magnetite. For this, magnetite nanoparticles were synthesized by the method of chemical condensation from iron (III) chloride solutions with a concentration of 0.32 mol/l and iron sulfate with a concentration of 0.2 mol/l by gradually adding a 25 % aqueous ammonia solution. It was shown that a simple deposition method can be used to synthesize homogeneous nanoparticles of Fe3O4 magnetite with a particle size of 8–25 nm. This is confirmed by the results of X-ray phase analysis and transmission electron microscopy. Magnetite nanoparticles were then used to obtain PAN/Fe3O4 composite fibers by adding magnetite in a 7 wt.% PAN solution in dimethylformamide. Fibers were obtained from the PAN/Fe3O4 suspension in dimethylformamide by electrospinning. Scanning electron microscopy showed that magnetite nanoparticles are uniformly distributed throughout the fiber surface, and the fiber size is 288–658 nm. The comparison of PAN fibers without the magnetite additive and PAN/Fe3O4 fibers showed that the addition of magnetite leads to a decrease in the fiber diameter at the same polymer concentrations and electrospinning conditions. XRD and elemental analysis of PAN/Fe3O4 fibers showed that magnetite particles in the fibers did not change their chemical composition and represent single-phase magnetite in a polymer matrix. The results obtained in the studies showed the possibility of obtaining composite fibers based on magnetite by the electrospinning method. Resulting composite fibers may be useful in practical scientific and engineering applications.
本文介绍了以聚丙烯腈(PAN)和磁铁矿为原料制备复合纤维的试验结果。为此,以浓度为0.32 mol/l的氯化铁(III)溶液和浓度为0.2 mol/l的硫酸铁溶液为原料,逐步加入25%的氨水溶液,采用化学缩合法制备了纳米磁铁矿。结果表明,采用简单的沉积方法可以制备出粒径为8 ~ 25 nm的Fe3O4磁铁矿纳米颗粒。x射线相分析和透射电子显微镜的结果证实了这一点。然后将磁铁矿纳米颗粒添加到7 wt.%的PAN -二甲酰胺溶液中,得到PAN/Fe3O4复合纤维。采用静电纺丝法将PAN/Fe3O4悬浮液置于二甲基甲酰胺中制备成纤维。扫描电镜显示,磁性纳米颗粒均匀分布在纤维表面,纤维尺寸为288 ~ 658 nm。通过对未添加磁铁矿的PAN纤维和PAN/Fe3O4纤维的比较发现,在相同聚合物浓度和静电纺丝条件下,添加磁铁矿导致纤维直径减小。对PAN/Fe3O4纤维的XRD和元素分析表明,纤维中的磁铁矿颗粒没有改变其化学组成,表现为聚合物基体中的单相磁铁矿。研究结果表明,静电纺丝法制备磁铁矿基复合纤维是可行的。由此产生的复合纤维可用于实际的科学和工程应用。
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引用次数: 0
Effect of the structure and morphology of Ni-based porous deposits on their electrocatalytic activity towards hydrogen evolution reaction 镍基多孔镀层结构和形貌对析氢反应电催化活性的影响
Pub Date : 2021-12-10 DOI: 10.17073/1997-308x-2021-4-57-67
T. S. Trofimova, A. B. Darintseva, T. N. Ostanina, V. M. Rudoi, I. E. Il’ina
Porous nickel and nickel-cobalt alloy deposits were obtained by electrodeposition on a dynamic hydrogen bubble template. Deposition was carried out from chloride electrolytes in a galvanostatic mode at a current density of 0.3 A/cm2. The porosity of the obtained deposits is associated with the macro- and micropores. It was found that the nickel and nickel-cobalt alloy deposits feature by different porous layer structures. In case of nickel, a typical foam structure is formed, while the Ni–Co alloy deposit morphology is more like loose (powder) metals. The total porosity of the obtained structures calculated based on experimental data decreased with the deposit thickness: from 0.4 to 0.1 for nickel foams, and from 0.9 to 0.8 for the Ni–Co deposit. It was shown that the dependences of the macropore number and the fraction of the surface occupied by them can be approximated by lognormal distribution. The agreement between the experimental values and values calculated by approximating equations indicates the stochastic nature of the macropore system formation. The catalytic properties of the obtained porous deposits toward the hydrogen evolution reaction in alkali were investigated. It was found that the decrease in the hydrogen evolution potential in comparison with a smooth electrode reaches 370 mV for nickel foams, and 440 mV for porous Ni–Co alloy deposits. However, the high porosity of the Ni–Co alloy caused poor adhesion of the deposit to the substrate; therefore, the porous Ni–Co deposit cannot be used without further strengthening. The dependences of the depolarization value during hydrogen evolution on the average diameter of pores, their number, and the macropore fraction were analyzed. Optimal properties of foams that reduce the potential of hydrogen evolution in alkali are as follows: pore diameters from 30 to 50 μm and their quantity from 50 to 100 pcs/mm2.
在动态氢泡模板上电沉积多孔镍和镍钴合金镀层。氯化物电解质在电流密度为0.3 a /cm2的恒流模式下进行沉积。所得矿床的孔隙度与宏观和微观孔隙有关。发现镍和镍钴合金镀层具有不同的多孔层结构。以镍为例,形成典型的泡沫结构,而镍钴合金的沉积形态更像松散(粉末)金属。根据实验数据计算所得结构的总孔隙度随镀层厚度的增加而减小:泡沫镍镀层的孔隙度从0.4降至0.1,镍钴镀层的孔隙度从0.9降至0.8。结果表明,大孔数与大孔所占表面积的关系可以近似为对数正态分布。实验值与近似方程计算值吻合,表明大孔系统形成的随机性。研究了制备的多孔沉积材料对碱中析氢反应的催化性能。结果表明,与光滑电极相比,泡沫镍的析氢电位降低了370 mV,多孔镍钴合金的析氢电位降低了440 mV。然而,Ni-Co合金的高孔隙率导致镀层与基体的附着力较差;因此,多孔镍钴镀层必须进一步强化才能使用。分析了析氢过程中脱极化值与孔平均直径、孔数和大孔分数的关系。降低碱中析氢电位的泡沫的最佳性能为:孔径在30 ~ 50 μm之间,数量在50 ~ 100 pcs/mm2之间。
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引用次数: 1
Structure and wear resistance of coatings produced by the short-pulse laser alloying of titanium carbohydride-based mechanocomposites 短脉冲激光合金化碳化钛基机械复合材料涂层的组织和耐磨性
Pub Date : 2021-12-10 DOI: 10.17073/1997-308x-2021-4-46-56
M. Eryomina, S. Lomayeva, E. Kharanzhevskiy
The study covers the phase composition, morphology and properties of coatings deposited on steel by means of short pulse selective laser alloying of titanium carbohydride-based mechanocomposites. Mechanocomposites were fabricated by milling of Ti and Ti–Cu powders in a liquid hydrocarbon environment. The synthesized mechanocomposites and fabricated coatings are investigated by X-ray diffraction, scanning electron microscopy and optical microscopy. The phase composition of mechanocomposites is represented by titanium carbohydride phase with a size of powder particles ranging from 2 to 30 μm for powders without copper, and from 1 to 10 μm for copper-containing powders. Coatings fabricated from powder mechanocomposites have a gradient structure. The Ti(C,H) powder coating contains 48 vol.% of the titanium carbide phase in a shell of Fe–Ti intermetallic compounds. The Ti(C,H)–Cu powder coating contains 85 vol.% of titanium carbide inclusions surrounded by Ti(Fe,Cu) and CuTi2 phases. Round-shaped carbide inclusions formed have a size of 50 to 200 nm, and dendritic ones are up to 5 μm. Coatings have a microhardness of 10 GPa and 8 GPa for compositions without and with copper, respectively. Coatings were tested for wear resistance under the conditions of dry friction in pairs with the balls made of steel and VK6 tungsten carbide alloy. Coefficients of friction for both coating types are 0.16–0.3 with the ball made of VK6 tungsten carbide alloy and 0.2–0.4 with the ball made of hardened steel. Coatings almost do not wear out under the counterbody load of 10 N and testing time of 20 min.
研究了短脉冲选择性激光合金化碳化钛基机械复合材料在钢表面沉积涂层的相组成、形貌和性能。在液态烃环境下,采用Ti和Ti - cu粉末的铣削工艺制备了力学复合材料。采用x射线衍射、扫描电镜和光学显微镜对合成的机械复合材料和涂层进行了研究。力学复合材料的相组成以碳化钛相为代表,无铜粉末颗粒尺寸为2 ~ 30 μm,含铜粉末颗粒尺寸为1 ~ 10 μm。粉末力学复合材料制备的涂层具有梯度结构。Ti(C,H)粉末涂层在Fe-Ti金属间化合物的外壳中含有48 vol.%的碳化钛相。Ti(C,H) -Cu粉末涂层含有85%的碳化钛夹杂物,包裹着Ti(Fe,Cu)和CuTi2相。形成的碳化物包裹体呈圆形,尺寸为50 ~ 200 nm,树枝晶包裹体的尺寸可达5 μm。不含铜和含铜镀层的显微硬度分别为10gpa和8gpa。在干摩擦条件下,对涂层与由钢和VK6碳化钨合金制成的球对进行了耐磨性试验。两种涂层的摩擦系数分别为:VK6碳化钨合金涂层的摩擦系数为0.16 ~ 0.3,淬火钢涂层的摩擦系数为0.2 ~ 0.4。在10 N的反体载荷和20 min的试验时间下,涂层几乎不发生磨损。
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引用次数: 1
Obtaining Ti–Cu–C system composite materials by SHS process SHS法制备Ti-Cu-C系复合材料
Pub Date : 2021-12-09 DOI: 10.17073/1997-308x-2021-4-11
V. G. Tsikarev, A. A. Filippenkov, M. Filippov, A. Alabushev, V. Sharapova
 The aim of the research is to obtain wear-resistant products from composite materials of a new type using the SHS technology. The Ti–Cu–C system was selected taking into account the data available in the scientific and technical literature. Various SHS charge compositions consisting of titanium powder, copper powder, and carbon black were experimentally burned to determine compositions that can burn during the SHS process and provide a melt containing titanium carbide and titanium cuprides as a binder featuring higher mechanical properties and lower melting points than pure copper. Model samples of products in the form of bushings with an outer diameter of 70 and 110 mm were produced by burning the SHS charge with selected compositions in a reactor followed by the compaction of the resulting melt with a force of 50–60 t. After the rough workpiece electrical discharge machining, samples were cut out for phase analysis, X-ray spectral analysis, and wear tests. With an optimal ratio of SHS charge components, titanium carbide and a binder in the form of titanium cuprides of different compositions were revealed in the model sample material. Using the method of testing for wear when sliding on a fixed abrasive under a specific pressure of 1 MPa, it was determined that the relative abrasive resistance of the new material at a hardness of 50–52 HRC is 1.8–2.0 units in comparison with the hardened tool and die steel Kh12MFL. In order to implement the technology in practice, an algorithm was developed for calculating the compositions of the newly formulated SHS charge, while its principle is such a ratio of components where the introduced carbon forms titanium carbide with titanium, and the added excess titanium forms titanium cuprides with copper. The developed material can be considered as promising for use as elements of equipment operating under abrasive wear conditions. This development is patented, Patent No. 2691656 (Russian Federation).
研究的目的是利用SHS技术从新型复合材料中获得耐磨产品。Ti-Cu-C系统的选择考虑了科学和技术文献中的现有数据。实验燃烧了由钛粉、铜粉和炭黑组成的各种SHS装药组合物,以确定在SHS过程中可以燃烧的组合物,并提供了含有碳化钛和铜化钛作为粘合剂的熔体,该熔体具有比纯铜更高的机械性能和更低的熔点。通过在反应器中燃烧选定成分的SHS装药,然后用50-60 t的力压实所产生的熔体,生产外径为70和110 mm的产品模型样品。在粗工件电火花加工后,样品被切割出来进行相分析、x射线光谱分析和磨损测试。在最佳SHS电荷组分配比下,模型样品材料中出现了碳化钛和不同成分的铜化钛形式的粘结剂。采用比压为1 MPa的固定磨料滑动磨损试验方法,确定新材料在硬度为50-52 HRC时的相对耐磨性与淬硬的工具模具钢Kh12MFL相比为1.8-2.0个单位。为了在实践中实现该技术,开发了一种计算新配制的SHS电荷组成的算法,其原理是引入的碳与钛形成碳化钛,而添加的过量钛与铜形成铜化钛的组分比例。所开发的材料可以被认为是在磨料磨损条件下作为设备元件使用的有前途的材料。该开发已获得专利,专利号2691656(俄罗斯联邦)。
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引用次数: 0
Exothermic synthesis of binary solid solutions based on hafnium and zirconium carbides 基于碳化铪和氧化锆的二元固溶体的放热合成
Pub Date : 2021-12-09 DOI: 10.17073/1997-308x-2021-4-30-37
V. Shcherbakov, A. Gryadunov, M. Alymov
The paper presents the results of an experimental study into the possibility of producing ultra-high temperature ceramics  constituting solid solutions of HfC and ZrC carbides by the single-stage electro-thermal explosion (ETE) method under pressure.  Adiabatic flame temperature and phase composition of the equilibrium final product were calculated based on thermodynamic  data. It was shown that when the ZrC content in the final product is less than 20 wt.%, adiabatic flame temperature reaches 3800– 3900 K, and the combustion product contains hafnium and zirconium carbides. The effect of mechanical activation modes in an  AGO-2 planetary centrifugal mill used for a reaction mixture containing Hf, Zr and C powders on its properties, phase composition  formation and the microstructure of carbide solid solutions was studied. It was shown that high-energy mixing in hexane leads to  the destruction of the crystal structure of Hf and Zr particles and the formation of amorphous composite particles. The synthesized  samples of ultra-high temperature ceramics were studied by X-ray phase and microstructure analyzes. It was shown that exothermic  synthesis leads to the formation of single-phase solid solutions of HfC and ZrC carbides with the average particle size of 0.2–1.5 μm.  The residual porosity of the binary carbides obtained is 10–12 %. It was found that, despite the high temperature of sample heating  during ETE under pressure, the particle size of the resulting solid solutions is significantly (by an order of magnitude) smaller than  the particle size of similar complex carbides (20–50 μm) obtained by other methods (SPS and hot pressing). This is associated with  the rapidity of the exothermic interaction of the reagents (10–50 ms) during ETE.
本文对高压下单级电热爆炸法制备HfC和ZrC碳化物固溶体超高温陶瓷的可能性进行了实验研究。根据热力学数据计算了绝热火焰温度和平衡终产物的相组成。结果表明,当最终产物中ZrC含量小于20wt .%时,绝热火焰温度达到3800 ~ 3900 K,燃烧产物中含有碳化铪和碳化锆。研究了AGO-2型行星离心机中机械活化方式对Hf、Zr和C粉末反应混合物性能、相组成形成和碳化物固溶体微观结构的影响。结果表明,在正己烷中进行高能混合会破坏Hf和Zr粒子的晶体结构,形成非晶复合粒子。对合成的超高温陶瓷样品进行了x射线物相分析和显微结构分析。结果表明,放热合成可形成平均粒径为0.2 ~ 1.5 μm的HfC和ZrC碳化物单相固溶体。所得二元碳化物的残余孔隙率为10 ~ 12%。研究发现,尽管在压力下加热时样品温度很高,但所得固溶体的粒径明显小于其他方法(SPS和热压)获得的类似复合碳化物(20-50 μm)的粒径(一个数量级)。这与电激放电过程中试剂的放热相互作用的速度(10-50 ms)有关。
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引用次数: 0
Thermally coupled SHS processes in (Ni + Al)/(Co + Ti)/(Ni + Al) layered system: experimental and theoretical study (Ni + Al)/(Co + Ti)/(Ni + Al)层状体系热耦合SHS过程的实验与理论研究
Pub Date : 2021-12-09 DOI: 10.17073/1997-308x-2021-4-20-29
R. Gabbasov, V. Kitler, V. Prokof'ev, A. M. Shul’pekov
The paper focuses on the theoretical and experimental study of the mechanisms of reaction mixture combustion in the ≪chemical oven≫ mode in a three-layer Ni–Al/Ti–Co/Ni–Al sample. Experimental studies were carried out in a reactor in an argon atmosphere at atmospheric pressure and an ambient temperature of 298 K on rectangular samples pressed from Ni–Al and Ti–Co powder mixtures in the form of a three-layer package. The Ti–Co acceptor layer was in the middle of the sample, and the Ni–Al donor layer was outside. The acceptor layer thickness was varied from 4.3 to 13 mm, while the donor layer thickness (4.7 mm) remained constant. It was found that as the acceptor layer thickness increases, the combustion wave front propagation velocity and reaction initiation temperature decrease, and the maximum temperature in the front remains constant and equal to the melting point of the final product. The time of acceptor layer heating before the reaction increases. The acceptor mixture reaction proceeds in the thermal explosion mode when the thickness of the acceptor layer exceeds that of the donor one. Maximum temperature in this case is higher than the melting point of the final product. The inner layer synthesis modes change with an increase in the acceptor layer thickness: stationary – pulsating – extinction. The mathematical model of the three-layer sample high-temperature synthesis in dimensional variables is constructed taking into account heat transfer with the environment. As a result of experimental studies and numerical calculations, the critical thickness of the inner layer was found to be 15 mm, at which the inner layer combustion becomes impossible at fixed sizes of donor layers. Critical conditions for the combustion wave propagation along the acceptor layer are weakly dependent on the external heating source. The experimental technique and mathematical model of the layered system combustion can be used to assess the critical conditions for the metal composite synthesis in the frontal combustion mode.
本文着重对Ni-Al / Ti-Co / Ni-Al三层样品在“化学烘箱”模式下反应混合物燃烧机理进行了理论和实验研究。在常压和298 K环境温度的氩气反应器中,对镍铝和钛钴粉末混合物压制成三层包体的矩形样品进行了实验研究。Ti-Co受体层位于样品的中间,Ni-Al给体层位于样品的外侧。受体层厚度变化范围为4.3 ~ 13 mm,而供体层厚度保持不变(4.7 mm)。研究发现,随着受体层厚度的增加,燃烧波前传播速度和反应起始温度降低,燃烧波前的最高温度保持不变,且等于最终产物的熔点。反应前受体层加热的时间增加。当受体层厚度超过供体层厚度时,受体混合反应以热爆炸模式进行。在这种情况下,最高温度高于最终产品的熔点。内层合成模式随受体层厚度的增加而变化:平稳-脉动-消光。建立了考虑环境传热的三层样品高温合成的量纲变量数学模型。通过实验研究和数值计算,得出了内层的临界厚度为15mm,在固定尺寸的供层下,内层燃烧是不可能的。燃烧波沿受热层传播的临界条件对外部热源的依赖性较弱。层状体系燃烧的实验技术和数学模型可用于评估金属复合材料在正面燃烧模式下合成的临界条件。
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引用次数: 0
SHS compaction of TiC cermets using mechanically activated mixtures 用机械活化混合物对TiC陶瓷进行SHS压实
Pub Date : 2021-12-09 DOI: 10.17073/1997-308x-2021-4-12-19
Yu. V. Bogatov, V. Shcherbakov
This paper focuses on obtaining cermet composite materials by SHS compaction. The study covers the effect of mechanical activation of metal components contained in reaction mixtures based on the Ti + C + Cr + Ni system when treated with grinding media in a ball mill. Two mechanical activation methods were used for Ti, Cr and Ni metal powders. In the first method, Cr and Ni powders were activated with grinding media separately from other reaction mixture components, and then mixed with titanium and carbon black powders. It is shown that the preliminary mechanical activation of inert components reduces the temperature and rate of combustion and increases the average size of carbide grains. In the second method, Ti + + Cr, Ti + Ni, and Ti + Cr + Ni powder mixtures were jointly processed in a ball mill, and then mixed with carbon black. This method provided mechanical activation of titanium particles with a minimum effect of grinding media on Cr and Ni powders. This led to an increase in the combustion rate and temperature, a decrease in the average size of carbide grains, and an increase in the composite structure homogeneity. A mechanism is proposed for the interaction of reagents (Ti + C) with the participation of activated Cr and Ni particles in combustion and structure formation zones, according to which the mechanical activation of inert components leads to their direct participation in the reaction interaction of titanium with carbon, which determines a decrease in the combustion rate and temperature and affects the fineness and structural homogeneity of compact composites. The results obtained were used to increase the structural homogeneity and fineness of the STIM-3B composite (Grade 3B synthetic hard tool material).
本文主要研究了用SHS压实法制备陶瓷复合材料。研究了Ti + C + Cr + Ni体系反应混合物中金属组分在球磨机研磨介质处理下的机械活化效应。采用两种机械活化方法对Ti、Cr和Ni金属粉末进行了活化。在第一种方法中,Cr和Ni粉末与其他反应混合物组分分别用研磨介质活化,然后与钛和炭黑粉末混合。结果表明,惰性成分的初步机械活化降低了燃烧温度和燃烧速率,增大了碳化物晶粒的平均尺寸。第二种方法是将Ti + + Cr、Ti + Ni和Ti + Cr + Ni粉末混合物在球磨机中共同加工,然后与炭黑混合。该方法提供了钛颗粒的机械活化,研磨介质对Cr和Ni粉末的影响最小。这导致燃烧速率和温度升高,碳化物晶粒的平均尺寸减小,复合材料的组织均匀性提高。提出了反应物(Ti + C)与活化的Cr和Ni颗粒在燃烧区和结构形成区相互作用的机理,认为惰性组分的机械活化导致其直接参与钛与碳的反应相互作用,从而决定了燃烧速率和温度的降低,影响了致密复合材料的细度和结构均匀性。将所得结果用于提高STIM-3B复合材料(3B级合成硬刀具材料)的结构均匀性和细度。
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引用次数: 0
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Izvestiya vuzov. Poroshkovaya metallurgiya i funktsional’nye pokrytiya
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