水热法制备C3N4/CuGaO2 复合物及其气敏性能

采用简单水热法合成了一系列C₃N₄/CuGaO₂复合材料。采用XRD、SEM、TEM和XPS对制备的样品进行了表征。研究了一系列C₃N₄/CuGaO₂复合材料的气敏性能。结果表明,基于C₃N₄/CuGaO₂-0.3复合材料（C₃N₄与CuGaO₂的摩尔比为0.3:1）的气体传感器对甲苯的传感性能优于CuGaO₂传感器。相比较于CuGaO₂传感器的工作温度（140 ℃）,C₃N₄/CuGaO₂-0.3复合材料传感器的最佳工作温度仅为25 ℃,对100 μL/L甲苯气体的响应达到28,检出限低至0.01 μL/L。对100 μL/L甲苯气体的响应时间和恢复时间分别为114.2和27.4 s。此外,用于检测甲苯的C₃N₄/CuGaO₂-0.3复合材料传感器还具有优异的长期稳定性、良好的重复性和优异的抗湿性能。     

Ar/N2-Ar共溅射Ti掺杂对Ta2O5 涂层光学和力学性能的影响

为了探索Ar/N₂-Ar共溅射Ti掺杂对Ta₂O₅涂层光学性能和力学性能的影响,采用射频和直流磁控共溅射技术在玻璃基底表面制备了Ta₂O₅、N₂-Ta₂O₅、Ti-Ta₂O₅和N₂-Ti-Ta₂O₅涂层。利用X射线衍射仪（XRD）、扫描电子显微镜（SEM）、原子力显微镜（AFM）表征了Ta₂O₅、N₂-Ta₂O₅、Ti-Ta₂O₅和N₂-Ti-Ta₂O₅涂层的微观结构和表面形貌;通过紫外可见分光光度计测试了涂层的光学参数;采用纳米压痕仪测试了涂层的硬度和杨氏模量。XRD测试结果表明,Ta₂O₅、N₂-Ta₂O₅、Ti-Ta₂O₅和N₂-Ti-Ta₂O₅涂层主要以Ta₂O₅为主体的非晶相结构组成。SEM和AFM结果显示,沉积在玻璃基底上的涂层未出现大面积空隙,溅射粒子在基底表面均匀堆积生长,并且涂层沉积厚度基本一致,厚度误差在5%以内。分别引入N₂和Ti及N₂-Ti共掺杂,均可降低Ta₂O₅涂层的粗糙度。光学测试结果表明,分别引入N₂和Ti元素,可以提高Ta₂O₅涂层的平均透射率至81%以上,而N₂-Ti共掺杂制备的N₂-Ti-Ta₂O₅涂层平均透射率降低。力学测试结果显示,与Ta₂O₅涂层对比,N₂-Ta₂O₅和N₂-Ti-Ta₂O₅涂层的硬度显著增大,Ti-Ta₂O₅涂层硬度基本一致。弹性指数（H/E）和塑性指数（H³/E²）表明,N₂-Ta₂O₅涂层和N₂-Ti-Ta₂O₅涂层具备更好的断裂韧性和抗塑性变形能力。在玻璃表面制备Ta₂O₅掺杂N₂和Ti元素的涂层,可以实现以N₂-Ta₂O₅涂层和N₂-Ti-Ta₂O₅涂层为代表的、同时具备优异光学性能和力学性能的多功能涂层。     

TiZrNiCu钎焊Si3N4-MoSi2复合陶瓷与Nb接头组织与力学性能

采用高温活性钎料TiZrNiCu对Si₃N₄-MoSi₂复合陶瓷和金属Nb进行真空钎焊试验,研究了其典型界面组织组成及形成机理,分析了钎焊温度和保温时间对钎焊接头界面组织及力学性能的影响规律。结果表明,接头典型界面结构为Nb/β-Ti/(Ti. Zr)₂(Cu, Ni)+β-Ti+(Ti, Zr)₅Si₃/TiN+(Ti, Zr)₅Si₃+MoSi₂/Si₃N₄-MoSi₂。钎焊温度和保温时间主要通过控制Si₃N₄-MoSi₂复合陶瓷母材中Si原子向钎料中扩散程度,来影响钎缝中(Ti, Zr)₅Si₃化合物的数量及分布,进而影响钎焊接头的抗剪强度。在920 ℃/10 min的工艺参数下,Si₃N₄-MoSi₂/Nb接头的室温抗剪强度最高达到112 MPa,选择最优参数条件下的Nb/Si₃N₄-MoSi₂钎焊接头在500 ℃和600 ℃条件下进行高温剪切实验,其高温抗剪强度分别达到123 MPa和131 MPa。     

Li4SiO4 氚增殖陶瓷的制备及其与14Cr-ODS钢的腐蚀界面行为

Li₄SiO₄小球与ODS钢的化学相容性对聚变反应器的安全运行具有重要意义。研究了在500、600、700 ℃的氩气环境中保温300 h后ODS钢与小球接触界面组织和成分的变化。结果表明,在600~700 ℃时,Li₄SiO₄小球与ODS钢的界面发生了严重的元素互扩散和反应。在Li₄SiO₄小球表面,由于ODS钢中Fe和Cr的扩散,出现了一层薄薄的反应层,这也导致了密度的增加,破碎负荷从51 N （500 ℃）下降到32 N（700 ℃）。XRD图谱显示,ODS钢表面出现了LiCrO₂和LiFeO₂新相,说明Li₄SiO₄小球中的Li和O原子可以扩散到ODS中,与Fe、Cr元素在高温下发生反应形成腐蚀层。在700 ℃时,腐蚀层可分为2个氧化层。最外层是LiFeO₂和LiCrO₂的混合物,下一层主要是LiFeO₂。在ODS钢的表面,700 ℃/300 h条件下氧扩散系数为2.2×10^-14 cm²/s,这说明ODS钢作为一种包层结构材料,在未来的包层设计中需要一层耐腐蚀涂层。     

激光热喷涂Co30Cr8W1.6C3Ni1.4Si涂层在PAO+2.5%MoDTC油中摩擦学特性

为了提高TC4合金的耐磨性能,采用激光热喷涂技术在其表面制备了Co₃₀Cr₈W_1.6C₃Ni_1.4Si涂层。通过扫描电子显微镜（SEM）和X射线衍射（XRD）分析了涂层的形貌和物相,并通过摩擦磨损实验研究了涂层在PAO+2.5% MoDTC（质量分数）油中的磨损行为。结果表明,激光热喷涂的Co₃₀Cr₈W_1.6C₃Ni_1.4Si涂层主要由Ti、WC_1-x、CoO、Co₂Ti₄O和CoAl相组成,在涂层界面形成冶金结合。在激光功率为1000、1200和1400 W时所制备的涂层平均摩擦因数分别为0.151、0.120和0.171,其对应的磨损率分别为1.17×10^-6、1.33×10^-6和2.80×10^-6 mm³?N^-1?m^-1,磨损机理为磨粒磨损,其枝晶尺寸对降磨起主要作用。     

NiMoO4/g-C3N4的制备及电化学性能研究

超级电容器具有比电容高、循环寿命长和绿色无污染的特点,其优异的电化学性能备受关注。本文水热合成了NiMoO₄/g-C₃N₄复合粉体,并将粉体涂覆在泡沫镍上制备了NiMoO₄/g-C₃N₄电极材料。结果表明,NiMoO₄/g-C₃N₄粉体形貌主要为NiMoO₄纳米棒和团状g-C₃N₄,且NiMoO₄纳米棒生长在g-C₃N₄纳米片上。在NiMoO₄中加入30at%的g-C₃N₄能降低电容体系的等效串联电阻和扩散阻抗,有利于氧化还原反应的进行。相比于其他g-C₃N₄含量的电极材料,g-C₃N₄含量为30at%的NiMoO₄/g-C₃N₄电极材料具有更高的比电容(584.3F/g)和更好的倍率特性。     

激光辅助热喷涂NiCoCrAlYTa/ZrO2/BaF2·CaF2涂层的组织及性能∗

高温耐磨涂层是航空发动机关键摩擦副可靠使用的重要保障,鉴于其服役环境日益严苛复杂,进一步提高涂层的高温耐磨性能是十分必要的。利用激光辅助热喷涂技术制备 NiCoCrAlYTa / ZrO₂ / BaF₂·CaF₂ 高温耐磨涂层,利用 SEM、EDS 分析高温耐磨涂层的横截面微观组织及化学成分,研究 ZrO₂ / BaF₂·CaF₂质量分数、激光功率及扫描速度对耐磨涂层微观组织、力学性能及高温耐磨性能的影响。结果表明：激光辅助处理可以诱导耐磨涂层表面形成具有树枝状结构的 ZrO₂陶瓷层; 当激光功率为 80 W,扫描速度为 8 mm / s,喷涂粉末为 75 wt.% NiCoCrAlYTa+25 wt.% ZrO₂ / BaF₂·CaF₂时,制备涂层的微观组织、综合力学性能及高温耐磨性能达到最好;在此工艺参数下,涂层顶部的 ZrO₂ 陶瓷层最为致密均匀,其平均纳米硬度为 13.6 GPa,平均弹性模量为 182.5 GPa,800 ℃时的磨损率为 2.7×10^?5 mm³ ·N^?1 ·m^?1 。将高温耐磨涂层的组分设计与激光辅助热喷涂工艺相结合,可为提高涂层综合性能的提供解决途径。     

TiO2纳米粒子对铝锂合金微弧氧化膜结构及性能的影响

为改善微弧氧化膜层的耐蚀性及力学性能,向电解液中添加TiO₂纳米粒子后对2297铝锂合金进行了微弧氧化。利用SEM、XRD、EDS、辉光放电表征技术及电化学测试技术,分析了TiO₂纳米粒子对微弧氧化膜结构、力学性能及耐蚀性的影响。结果表明：添加TiO₂纳米粒子后,微弧氧化膜层变得平坦致密。随着TiO₂纳米粒子添加量的提高,膜层表面放电通道的孔径逐渐减小,数量逐渐增多。TiO₂纳米粒子会抑制熔融Al₂O₃与电解液中$ {\rm{SiO}}_{\rm{3}}^{{\rm{2 ^- }}}$的接触,所以膜层中Si元素的含量随TiO₂纳米粒子添加量的增加而逐渐下降(原子数分数从初始的10.27%下降到了3.10%)。显微硬度测试结果表明,TiO₂纳米粒子的引入增加了膜层的致密度及平整度,所以膜层的硬度得到了提升(添加1 g/L TiO₂纳米粒子后硬度提高了15%)。电化学测试结果显示,当微弧氧化的其它条件相同时,TiO₂纳米粒子的适量添加会提升膜层的耐蚀性,但过量添加时,由于膜层放电通道数量的增多等原因,其耐蚀性下降。     

H2S/CO2环境中L360钢点蚀行为研究

利用静态挂片失重法研究了含H₂S/CO₂模拟油田水溶液中, 温度及Cl^-浓度对L360管线钢点蚀的影响, 并利用Gumbel第一类近似函数分析了最深蚀孔概率. 结果表明, 在40℃~70℃之间, Cl^-浓度为10 g/L条件下, 点蚀的严重程度随温度增高而增大. 恒定温度下, Cl^-浓度对点蚀发生也有明显的影响, 当Cl^-在10×15 g/L范围时, 腐蚀试样发生明显的点蚀; 当Cl^-浓度大于20 g/L时, 试样主要发生均匀腐蚀, 随着Cl^-浓度的增大, 腐蚀产物膜变得更加疏松, 保护性能下降, 均匀腐蚀速率增大. 最深点蚀分布服从Gumbel第一类近似函数.     

超音速大气等离子喷涂TiB2-SiC涂层的抗氧化性及耐熔盐腐蚀性能

采用超音速大气等离子喷涂制备全包覆TiB₂-SiC涂层,研究了TiB₂-SiC涂层在400和800 ℃的氧化性能,并探究其氧化机理。对TiB₂-SiC涂层在900 ℃下的抗铝熔盐腐蚀性能进行研究,并探讨其耐熔盐腐蚀机理。结果表明,超音速大气等离子喷涂制备的TiB₂-SiC涂层具有良好的抗氧化性,在400 ℃的氧化速率常数为1.92×10^-5 mg²·cm^-4·s^-1,在800 ℃的氧化速率常数为1.82×10^-4 mg²·cm^-4·s^-1。超音速大气等离子喷涂制备的TiB₂-SiC涂层在900 ℃下具有良好的抗熔盐腐蚀性能,熔盐腐蚀后TiB₂-SiC涂层都保持致密结构,未发生涂层的开裂及剥落。     

Ce(SO4)2浓度对电喷镀Ni-W-Ce合金镀层性能影响

为了研究Ce(SO4)2浓度与合金镀层表面性能的关系,采用喷射电沉积法制备了一系列Ni-W-Ce合金镀层工件。用扫描电镜(SEM)观察了镀层的表面结构,并用能谱仪(EDS)检测镀层中的元素组成。XRD分析表明,镀层存在晶格畸变。LEXT4100激光共焦显微镜观察磨损痕迹,发现磨损机理发生了变化。结果表明,添加Ce(SO4)2改善了涂层的表面微观形貌,当浓度为0.5g/L时,涂层的表面质量最佳。同时,显微硬度、耐磨性和耐腐蚀性随浓度的增加呈现先好后坏的规律。当Ce(SO4)2浓度为0.5g/L时,显微硬度达到峰值519.69HV0.1。此时,镀层耐磨性最好,其耐磨性表征参数均取得最小值。且镀层的耐蚀性也最好,腐蚀电位为-0.5537V,电弧电抗半径最小。     

Influence of normal load and sliding speed on the tribological property of amorphous carbon nitride coatings sliding against Si3N4 balls in water

Amorphous carbon nitride (a-CN_x) coatings were deposited on Si₃N₄ disks by an ion beam assisted deposition system. The composition, structure and hardness of the a-CN_x coatings were characterized by Auger electronic spectroscopy, Raman spectroscopy and nano-indentation tester, respectively. The influences of normal load and sliding speed on the friction coefficients and the specific wear rates for the a-CN_x/Si₃N₄ tribo-pairs were investigated and analyzed synthetically by ball-on-disk tribometer. The worn surfaces were observed by optical microscope. The results showed that the a-CN_x coatings contained 12 at.% nitrogen, and their structure was a mixture of sp²and sp³ bonds. The a-CN_x coatings’ nanohardness was 29 GPa. The influence of sliding speed on the friction coefficients and the specific wear rate of the CN_x coatings was more obvious than that of normal load. The friction coefficients and the specific wear rate of the CN_x coatings decreased as the sliding speed increased. At a sliding speed higher than 0.1 m/s, the friction coefficients were less than 0.04. The specific wear rates of the a-CN_x coatings were higher than those of Si₃N₄ balls at a sliding speed below 0.1 m/s, while the specific wear rates of the a-CN_x coatings and the Si₃N₄ balls all fluctuated around a lower level of 10^− 8 mm³/Nm as the sliding speed increased beyond 0.2 m/s. To describe the wear behavior of a-CN_x coatings sliding against Si₃N₄ balls in water with normal loads of 3-15 N and sliding speeds of 0.05-0.5 m/s, the wear-mechanism map for the a-CN_x/Si₃N₄ tribo-pairs in water was developed.     

Structure and mechanical properties of TiAlSiN/Si3N4 multilayer coatings

TiAlSiN/Si₃N₄ multilayer coatings which have different separate layer thicknesses of TiAlSiN or Si₃N₄ were deposited onto glass sheets, single-crystal silicon wafers and polished WC-Co substrates by reactive magnetron co-sputtering. The morphology, crystalline structure and thickness of the as-prepared multilayer coatings were characterized by TEM, SEM, XRD and film thickness measuring instrument. The mechanical properties of the coatings were evaluated by a nanoindenter. The effects of monolayer thickness on the microstructure and properties of TiAlSiN/Si₃N₄ multilayer coatings were explored. The coatings showed the highest hardness when the thickness of Si₃N₄ and TiAlSiN monolayers was 0.33 nm and 5.8 nm, respectively. The oxidation characteristics of the coatings were studied at temperatures ranging from 700 °C to 900 °C for oxidation time up to 20 h in air. It was found that the coatings displayed good oxidation resistance.     

Deposition and characterization of CrN/Si3N4 and CrAlN/Si3N4 nanocomposite coatings prepared using reactive DC unbalanced magnetron sputtering

Nanocomposite coatings of CrN/Si₃N₄ and CrAlN/Si₃N₄ with varying silicon contents were synthesized using a reactive direct current (DC) unbalanced magnetron sputtering system. The Cr and CrAl targets were sputtered using a DC power supply and the Si target was sputtered using an asymmetric bipolar-pulsed DC power supply, in Ar + N₂ plasma. The coatings were approximately 1.5 μm thick and were characterized using X-ray diffraction (XRD), nanoindentation, X-ray photoelectron spectroscopy and atomic force microscopy. Both the CrN/Si₃N₄ and CrAlN/Si₃N₄ nanocomposite coatings exhibited cubic B1 NaCl structure in the XRD data, at low silicon contents (< 9 at.%). A maximum hardness and elastic modulus of 29 and 305 GPa, respectively were obtained from the nanoindentation data for CrN/Si₃N₄ nanocomposite coatings, at a silicon content of 7.5 at.%. (cf., 24 and 285 GPa, respectively for CrN). The hardness and elastic modulus decreased significantly with further increase in silicon content. CrAlN/Si₃N₄ nanocomposite coatings exhibited a hardness and elastic modulus of 32 and 305 GPa, respectively at a silicon content of 7.5 at.% (cf., 31 and 298 GPa, respectively for CrAlN). The thermal stability of the coatings was studied by heating the coatings in air for 30 min in the temperature range of 400-900 °C. The microstructural changes as a result of heating were studied using micro-Raman spectroscopy. The Raman data of the heat-treated coatings in air indicated that CrN/Si₃N₄ and CrAlN/Si₃N₄ nanocomposite coatings, with a silicon content of approximately 7.5 at.% were thermally stable up to 700 and 900 °C, respectively.     

Thermal shock behavior of Si3N4-TiN nano-composites

Si₃N₄-TiN nano-composites were fabricated by hot press sintering nano-sized Si₃N₄ and TiN powders. The microstructure, mechanical properties and thermal shock behavior of Si₃N₄-TiN nano-composites were investigated. The addition of proper amount TiN particles can significantly increase the flexural strength and the fracture toughness. Si₃N₄-TiN nano-composites showed both higher critical temperature difference and higher residual strength compared with those of monolithic silicon nitride nano-ceramic when the amount of TiN is less than 15 wt.%. But a further increase in the amount of TiN leaded to a decrease in the thermal shock resistance.     

Ni/Cu定向结构涂层在不同浓度H2SO4中的耐蚀性能

为了研究Cu元素对Ni基合金定向结构涂层耐腐蚀性能的影响,向Ni60合金粉末中添加了5%Cu(质量分数,下同),制备了定向结构Ni60/Cu复合涂层。采用电化学试验和浸泡试验,评估了涂层在不同浓度H₂SO₄溶液中的电化学腐蚀特性和浸泡腐蚀性能,探讨了涂层在不同浓度H₂SO₄溶液中的腐蚀行为。结果表明,涂层在不同浓度H₂SO₄溶液中的腐蚀均表现为活化-钝化-过钝化的过程,电化学阻抗谱在整个时间常数内具有典型的容抗特征,H₂SO₄溶液浓度从5%增至80%时,电荷转移电阻先减小后增大,涂层的耐腐蚀性呈现先降低后升高的趋势。随着H₂SO₄溶液浓度的增加,涂层表面的腐蚀程度先加剧后逐渐减缓,且在H₂SO₄溶液浓度为40%时,腐蚀电位移至最负,腐蚀电流密度增至最大。但在H₂SO₄溶液浓度达到80...     

原位生成 WC-B4C 增强镍基激光熔覆层及其性能研究

目的通过激光熔覆技术,在Q235钢表面原位生成WC-B4C增强镍基熔覆层。方法以WO3,B2O3,C和Ni60混合粉末为预涂原料,采用激光熔覆技术原位生成WC-B4C增强镍基熔覆层,对熔覆层的显微组织和物相构成进行分析,研究其摩擦磨损性能。结果采用合适的工艺参数,通过原位生成WC-B4C形成的增强镍基涂层形貌良好,与基材呈现较好的冶金结合。熔覆层平均硬度1200HV0.3,摩擦磨损失重仅为纯Ni60熔覆层的1/3。结论熔覆层硬度较高,耐磨性很好。大量原位生成的WC-B4C增强相及其均匀分布是熔覆层硬度和耐磨性提高的原因。     

The effects of nano-SiO2 additive on the zinc phosphating of carbon steel

In this paper, nano-SiO₂ was used as an accelerator for improving the microstructure and the corrosion resistance of phosphate coating on carbon steel. The chemical composition and microstructure of the coatings were analyzed by X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM). The effects of nano-SiO₂ on weight, roughness and corrosion resistance of the phosphate coatings were also investigated. Results show that the compositions of phosphate coating were Zn₃(PO₄)₂·4H₂O (hopeite), and Zn₂Fe(PO₄)₂·4H₂O (phosphophylite). The phosphate coatings became denser due to the addition of nano-SiO₂ which reduced the size of the crystal clusters. The average weight of phosphate coatings approximately linearly increased with the nano-SiO₂ content in the bath from 0 to 4 g/L, and the phosphate coatings formed in bath containing 2 g/L nano-SiO₂ showed the highest corrosion resistance in 5 wt.% sodium chloride solution at ambient temperature. Nano-SiO₂ would be widely utilized as a phosphating additive to replace the traditional nitrite, due to its less pollutant and its better quality of the coating.     

TC4钛合金表面沉积CrSiN/SiN纳米多层膜在3.5%NaCl溶液中的腐蚀磨损性能

为了研究纳米多层膜的耐腐蚀性能以及腐蚀磨损机理,采用离子源辅助磁控溅射在TC4钛合金表面制备不同调制周期的CrSiN/SiN纳米多层膜。使用扫描电子显微电镜、能谱仪表征涂层的微观结构、腐蚀形貌以及元素分布;使用划痕仪、纳米压痕仪、维氏硬度计测量涂层的膜基结合力、硬度、弹性模量及断裂韧性,采用电化学工作站以及销盘磨损仪测量涂层耐腐蚀性和腐蚀磨损性。结果表明:调制周期为90 nm与360 nm时涂层耐腐蚀性能较好,腐蚀电流密度分别为1.31×10~(-8)A·cm~(-2)和1.20×10~(-8)A·cm~(-2)。此外,调制周期为45nm时,涂层硬度及弹性模量最大,分别为(22.5±0.6)GPa和(226.4±6.3)GPa,且腐蚀磨损率最低,为9.67×10~(-7)mm~3·N~(-1)·m~(-1)。多层膜结构显著改善了TC4钛合金的耐腐蚀及腐蚀磨损性能。