不同氧化剂对6H-SiC化学机械抛光的影响

选用胶体SiO₂纳米颗粒为磨粒,研究不同pH值条件下高锰酸钾和双氧水两种氧化剂对6H-SiC晶片化学机械抛光的影响,并使用原子力显微镜观察抛光后表面质量。采用Zeta电位分析仪分析溶液中胶体SiO₂颗粒的Zeta电位,采用X射线光电子能谱分析SiC抛光表面元素及其化学状态。结果表明：SiC晶片的材料去除率随pH值变化而变化,采用高猛酸钾抛光液抛光时,材料去除率在pH 6时达到峰值185 nm/h,R_a为0.25 nm;采用双氧水抛光液抛光时,材料去除率在pH 8时达到峰值110 nm/h,R_a为0.32 nm。pH值低于5时,电负性的SiO₂颗粒会通过静电作用吸附在带正电的SiC表面,抑制SiC晶片表面原子的氧化及去除,降低材料去除率;pH值高于5时,SiO₂颗粒在双氧水抛光液中的静电排斥力弱于高锰酸钾抛光液中静电排斥力,从而影响了SiO₂颗粒的分散性能,降低了抛光效果。采用高锰酸钾抛光液抛光后,SiC晶片表面的Si-C氧化产物含量（Si-C-O、Si₄C_4-xO₂和Si₄C₄O₄）较高,高锰酸钾抛光液的氧化能力较强。     

单晶SiC化学机械抛光液化学反应参数研究

选择影响化学机械抛光化学反应速率的参数:催化剂浓度、氧化剂浓度、抛光液的pH值、抛光液温度等进行了试验,研究了它们对基于芬顿反应的单晶SiC化学机械抛光效果的影响规律。发现只有当H_2O_2浓度高于20%、Fe_3O_4浓度高于1.25%时,增大H_2O_2、Fe_3O_4浓度,材料去除率才会显著越高,此时材料去除速率由化学液腐蚀速度与磨料机械去除速度共同决定;低于此范围时由磨料的机械作用决定。温度升高会加速H_2O_2分解,抑制羟基自由基·OH的生成,减缓化学腐蚀,降低材料去除率。当Fe_3O_4浓度、H_2O_2浓度、pH值、抛光液温度分别为1.25%、15%、7、41℃时,化学腐蚀与机械去除的协调性及磨料的分散性较好,表面粗糙度最低;当它们分别为5%、25%、9.3、15℃时,材料去除率最高。     

放电等离子烧结温度对Fe-Si/MnZn(Fe2O4)2软磁复合材料组织与磁性能的影响

采用球磨法制备了Fe-Si/MnZn（Fe₂O₄）₂核壳结构粉末,并采用放电等离子烧结制备Fe-Si/MnZn（Fe₂O₄）₂软磁复合材料,研究了烧结温度（600～1 000℃）对该复合材料显微组织与磁性能的影响。结果表明：不同温度烧结Fe-Si/MnZn（Fe₂O₄）₂复合材料均由Fe-Si合金颗粒和颗粒间MnZn（Fe₂O₄）₂相组成;在600～700℃烧结时复合材料通过机械结合实现致密化,属于欠烧,800～900℃烧结可实现良好冶金结合,属于完全烧结,1 000℃烧结时颗粒间MnZn（Fe₂O₄）₂铁氧体层遭到破坏,属于过烧;复合材料磁性能随烧结温度升高而先提高后下降,在900℃烧结时磁性能最好,饱和磁化强度最高,为1 476 kA·m^-1     

光助芬顿反应对6H-SiC化学机械抛光的影响

为提高6H-SiC晶片化学机械抛光的材料去除率(MRR)并改善其表面质量,采用光助芬顿反应体系对6H-SiC晶片进行化学机械抛光,研究紫外光功率、抛光液pH值、H2O2质量分数和Fe2+浓度对6H-SiC晶片抛光效果的影响。使用原子力显微镜观察6H-SiC晶片表面质量,采用纳米粒度电位仪测量抛光液中SiO2磨粒的粒径分布及Zeta电位,利用可见分光光度法检测溶液中羟基自由基(·OH)的浓度并通过紫外-可见光谱分析紫外光的作用机制。结果表明:引入紫外光提高了6H-SiC的MRR,增大紫外光功率,MRR也随之增加;随pH值、H2O2质量分数和Fe2+浓度的升高,MRR先增大后减小;pH值影响磨粒间的静电排斥力及磨粒的分散稳定性,从而影响6H-SiC的MRR;与采用芬顿反应体系的抛光液相比,采用光助芬顿反应体系的抛光液中产生的·OH数量较多,说明紫外光能够增加反应体系中·OH的数量,从而促进6H-SiC晶片的表面氧化,提高6H-SiC晶片的MRR,并改善其表面质量。     

同步辐射光电离质谱检测氟原子在二氧化硅表面反应产物

采用微波放电等离子体源产生高密度F原子,结合同步辐射真空紫外光电离质谱全面检测F原子在二氧化硅表面刻蚀反应的产物,并探究其反应机理。通过扫描同步辐射光子能量,获得具有特定质量选择的离子光电离效率谱,测量了反应产物的电离能及碎片离子的出现势等基本参数;同时结合量子化学理论计算质谱中离子的来源,即对光电离和光解离过程进行了区分。结果表明,F原子在二氧化硅表面会反应生成一系列的氟氧硅化合物 (Si_xO_yF_z),主要包括SiF₄、SiF₃OSiF₃和SiFOSiF₂OF等,质谱中观察到的SiF₃⁺、SiF₃OSiF₂⁺等离子信号来源于其对应母体离子的解离碎片。实验测得SiF₄的电离能为15.85 eV,SiF₃⁺和SiF₃OSiF₂⁺碎片离子的出现势分别为16.20、16.40 eV。该方法实现了高效检测F原子刻蚀反应的产物,由于F原子具有较高的化学反应活性,该实验装置也可用于开展气相自由基反应研究,模拟大气化学和燃烧火焰等体系中的化学反应过程。     

Pd-MOX(Mn,Mo,Sn)催化剂在电化学甲醛传感器中的应用

文中合成了金属氧化物(Mn₃O₄、MoO₃和SnO)掺杂的Pd基催化剂,研究了其催化甲醛氧化(formaldehyde oxidation reaction,FOR)的能力。结果表明,Pd-Mn₃O₄展示出最高的FOR活性(3.5 mA/cm²),是纯Pd催化剂的2.6倍。以Pd-Mn₃O₄为工作电极敏感材料的甲醛传感器对甲醛的响应是干扰气体的20倍,显示出良好的气体选择性。Pd-Mn₃O₄传感器在甲醛检测方面显示出巨大应用潜力。     

锌电解整流变压器循环冷却水软化净化方案的研究

将锌冶炼厂的锌电解车间的整流变压器的冷却方式改为“油-水”循环方式,可提高产能。在水循环换热的过程中,由于水中含有Ca²⁺和Mg²⁺等,加之敞开式的冷却塔形式,循环水存在蒸发和风吹等现象,使得Ca²⁺和Mg²⁺等离子浓度增大。当增大的离子浓度超过其溶解度时,容易析出形成水垢。文章对冷却水循环系统进行改造设计,在循环系统加入旁路软化系统,首先利用Ca(OH)₂与Ca²⁺和Mg²⁺等离子发生化学反应生成Ca CO₃和Mg(OH)₂,其次利用Na₂CO₃与永硬度和负硬度盐发生反应生成Ca CO₃和Mg CO₃等难溶于水的化合物,再次经过析出、沉淀和过滤去除Ca²⁺和Mg²⁺,最后用活性炭吸附进一步净化,滤除微小悬浮颗粒。旁路软化系统的加入,使循环水充分软化和洁净,减少...     

Y2O3改性石墨/CaF2/TiC/镍基合金复合涂层微观组织与摩擦学性能研究

为提高石墨/CaF₂/TiC/镍基合金（GCTN）复合涂层的力学性能和摩擦学性能,运用等离子喷涂技术在45钢表面制备了Y₂O₃改性GCTN复合涂层,研究了Y₂O₃对复合涂层的微观组织、显微硬度、断裂韧性和摩擦磨损性能的影响。结果表明：Y₂O₃改性GCTN复合涂层主要由γ-Ni、CrB、Cr7C₃、TiC、CaF₂和石墨等物相组成。Y₂O₃在等离子火焰加热作用下与C元素反应生成活性元素Y,Y净化了复合涂层的微观组织,并细化了CrB、Cr₃C7等硬质相晶粒,提高了其致密性。当Y₂O₃质量分数为0.5%时,复合涂层的显微硬度和断裂韧性分别为593.3MPa和6.82MPa·m^1/2,比不含Y₂O₃的复合涂层分别增大了8%和22%,其机理主要是Y₂O₃细化了CrB、Cr₃C₇等硬质相晶粒,起到了细化强化作用。由于GCTN-0.5Y₂O₃复合涂层的显微硬度和断裂韧性显著提高,减少了其黏着磨损和微观断裂磨损,因而GCTN-0.5Y₂O₃复合涂层的摩擦因数和磨损率最小,分别为0.085和0.39×10-3mm3/m。     

热压烧结制备碳化硅增韧氧化铝刀具复合材料及其力学性能评价研究

氧化铝陶瓷作为制造切削刀具的优良材料,较低的韧性限制了其应用。选用不同含量的碳化硅(2%,5%和10%)加入氧化铝颗粒中,经球磨后,利用真空热压烧结法(1400℃,20MPa)制备Al₂O₃/SiC复合材料。从X射线衍射(XRD)、致密度、硬度、弯曲强度以及断裂韧性等方面对材料性能进行了分析。结果发现,随着SiC的加入,Al₂O₃/SiC复合陶瓷硬度和抗弯强度增大。当SiC质量分数为5%时,其硬度和弯曲强度最大,最大值分别为1071.98HV和379.83MPa,此时断裂韧性也最大,为6.39MPa·m^1/2。     

(Sm0.5Nd0.5)3Ce7Ta2O23.5和(Yb0.5Dy0.5)3Ce7Ta2O23.5氧化物的热物理性能

以高纯度Sm₂O₃、Nd O₃、Dy₂O₃、Yb₂O₃、Ce O₂和Ta₂O₅为原材料,采用多步高温固相烧结法制备了(Sm_0.5Nd⁾_0.53Ce₇Ta₂O_23.5和(Yb_0.5Dy⁾_0.53Ce₇Ta₂O_23.5氧化物,研究了其晶体结构、微观形貌、热物理性能等。结果表明:制备的氧化物均具有单一的萤石结构,其结构致密,晶界清晰,元素种类和原子比与化学式基本一致;这2种氧化物的热导率明显低于7YSZ,且(Yb_0.5Dy⁾_0.53Ce₇     

LED蓝宝石衬底抛光表面原子台阶形貌及其周期性研究

LED蓝宝石衬底的表面质量会极大影响到后续外延质量,进而影响到LED器件性能。蓝宝石研磨片经Al2O3磨粒粗抛液、SiO2磨粒精抛液下进行化学机械抛光(CMP),最终表面经原子力显微镜(AFM)所测表面粗糙度达到0.101nm,获得亚纳米级粗糙度超光滑表面,并呈现出原子台阶形貌。同时,通过使用Zygo表面形貌仪、AFM观察蓝宝石从研磨片经Al2O3粗抛液、SiO2精抛液抛光后的表面变化,阐述蓝宝石表面原子台阶形貌的形成原因,提出蓝宝石原子级超光滑表面形成的CMP去除机理。通过控制蓝宝石抛光中的工艺条件,获得a-a型、a-b型两种不同周期规律性的台阶形貌表面,并探讨不同周期规律性台阶形貌的形成机理。     

剪切增稠抛光磨料液的制备及其抛光特性

为了实现对工件的剪切增稠抛光(STP),采用机械混合与超声波分散法制备了一种Al2O3基STP磨料液,并研究了它们的抛光特性。利用应力控制流变仪考察其流变性能,通过扫描电镜和光学轮廓仪研究了单晶硅加工后表面显微组织的变化,并测量其表面粗糙度。结果表明:STP磨料液具有剪切变稀和可逆的剪切增稠特性,达到临界剪切速率后,会形成Al2O3"粒子簇";当剪切速率增大至1000s-1,储能模量,耗能模量和耗散因子都增至最大值,此时主要表现为类似固体的弹性行为,有利于形成类似"柔性固着磨具"。在STP加工单晶硅过程中,采用塑性去除的材料去除方式。随着抛光时间的延长,硅片去除速率先增大后减小;表面粗糙度不断减小并趋于稳定。实验显示,磨粒浓度不宜过高,否则会因剪切增稠效应造成黏度过大,导致流动性差而影响抛光质量。当Al2O3质量分数为23%时,抛光25min后,硅片表面粗糙度Ra由422.62nm降至2.46nm,去除速率达0.88μm/min,表明其能实现单晶硅片的高效精密抛光。     

Prediction of the surface roughness and material removal rate in chemical mechanical polishing of single-crystal SiC via a back-propagation neural network

Chemical mechanical polishing (CMP) is a common method for realising the global planarisation and polishing of single-crystal SiC and other semiconductor substrates. The strong oxidant hydroxyl radicals (·OH) generated by the Fenton reaction can effectively oxidise and corrode the SiC substrate, and are thus used to improve the material removal rate (MRR) and surface roughness (Ra) after polishing of SiC during CMP. Therefore, it is necessary to study the material removal mechanism in detail. Based on the modified Preston equation, the effects of the CMP process parameters on the MRR and Ra after polishing of SiC and their relationship were studied, and a prediction model of the CMP process parameters, MRR, and Ra after polishing was also established based on a back-propagation neural network. The MRR initially increased and then decreased, and the Ra after polishing initially decreased and then increased, with increasing FeSO₄ concentration, H₂O₂ concentration, and pH value. The MRR continuously increased with increasing abrasive particle size, abrasive concentration, polishing pressure, and polishing speed. However, the Ra continuously decreased with increasing abrasive particle size and abrasive concentration, increased with increasing polishing pressure, and initially decreased and then increased with increasing polishing speed. The established prediction model could accurately predict the relationship between the process parameters, MRR and Ra after polishing in CMP (relative prediction error of less than 10%), which could provide a theoretical basis for CMP of SiC.     

The wear behaviour of high-chromium white cast irons as a function of silicon and Mischmetal content

The sliding wear behaviour of high-chromium white cast iron (16.8% Cr) has been examined as a function of silicon and Mischmetal alloy additions (1, 2, 3 and 5% Si and 0.1 and 0.3% Mischmetal). Such additions are known to modify the structure, but there is considerable controversy as to the exact effect. Silicon was found to refine the dendritic structure and increased the eutectic carbide volume fraction. However, for contents above 3%, transformation of the austenitic matrix to pearlite occurred in preference to martensite. Mischmetal additions reduced the austenite dendrite arm spacing, but did not have a significant effect on the carbide structure. The wear behaviour was investigated for each alloy in the as-cast (austenitic matrix) and hardened (martensitic) conditions using a block on ring configuration in pure sliding in the load range 42–238 N for a distance of 70 km against a hardened M2 steel counterface. For low loads (42 and 91 N), all the alloys showed a similar wear rate (3×10⁻⁴ to 4×10⁻⁴ mm³/m), associated with the formation of a thin (3 μm) oxide film of Fe₂O₃, the formation of very fine debris and a small depth of deformation below the worn surface (7 μm). For higher loads, wear was a strong function of microstructure, and was associated with a thicker film of the oxides Fe₂O₃ and Fe₃O₄ and greater depths of deformation. The iron with 2% silicon exhibited the best performance with a wear rate of 7×10⁻⁴ mm³/m and this was attributed to its finer structure and the formation of a thicker oxide film. In contrast, the iron with 5% silicon exhibited the worst performance, with a wear rate of 14×10⁻⁴ mm³/m, attributed to the pearlitic matrix. A linear relationship was observed between the depth of carbide fracture and the wear rate. The relationship between microstructure and wear mechanism is discussed.     

宋代黑釉茶盏油滴的飞行时间二次离子质谱表征

本研究利用飞行时间二次离子质谱(TOF-SIMS)表征典型黑釉茶盏釉面上银色反光斑纹,即华北油滴。高分辨质谱测定油滴的主要成分是氧化铁,由显微拉曼光谱确定其矿物形式是赤铁矿(α-Fe₂O₃)。二次离子质谱(SIMS)离子成像进一步揭示：该赤铁矿呈六方柱晶体(约2～10μm);近百余枚这样的晶体自组织分散排列构成类似雨滴状的斑纹(约120μm);与其形貌互补的是含硅、铝、钙、钠等元素的碱性石灰质釉质。SIMS深度剖析发现,α-Fe₂O₃晶体的连续深度不小于5μm。基于SIMS表征结果,还探讨了赤铁矿沉积薄膜状镜铁矿(α-Fe₂O₃)引起华北油滴呈银色与镜面反射现象的原理,以及TOF-SIMS在表征和研究古瓷方面的潜力和局限。     

电化学机械复合抛光薄膜太阳能电池柔性不锈钢衬底

设计了针对薄膜太阳能电池柔性不锈钢衬底的电化学机械复合抛光法以满足其对表面粗糙度、光反射率和有害物质扩散的要求。首先,设计并制造了一种用于平面加工的复合阴极刀具,理论分析了它的材料去除机理。然后,结合法拉第原理和黏着摩擦理论分析了电化学腐蚀行为和摩擦力作用行为,解决了电化学腐蚀和机械去除钝化膜的匹配一致性问题。最后,以50mm×50mm×0.3mm规格的304不锈钢为阳极工件,对提出的方法进行了实验验证。结果显示:对衬底加工20min后,其表面粗糙度Ra从124nm降到10nm;表面反射率从加工前的56.8%提高到62.4%;表面金属氧化层的形成(氧化铁和氧化铬),有效阻挡了Fe和Cr离子的扩散。实验显示,提出的方法是处理柔性不锈钢表面的有效方法,成本低、效率高。     

The effects of iron particles on the friction and wear mechanisms of ceramics in ethanol

For the combinations of an Si₃N₄ pin and five kinds of ceramic disk (SiC, Si₃N₄, Al₂O₃, ZrO₂, TiC), a friction and wear test was carried out in ethanol and in ethanol containing iron particles (1 wt.%, average diameter d = 200 nm, D = 12 μm under cohered condition) under a load in the range 5.88–11.50 N, at a sliding velocity of 0.138–0.196 m s⁻¹. A topographical analysis was also performed on the microasperities of the wear surfaces to estimate the behavior of the iron particles, and the degree of surface damage. As a result, the following facts were found. (1) The addition of iron particles in ethanol decreased both the wear rates of SiC and TiC disks and the mating pins, and also decreased the wear rate of the Al₂O₃ disk but increased that of the mating pin. The addition increased the wear rates of both ZrO₂ and Si₃N₄ disks and the mating pins. (2) The average coefficients of friction with the addition of iron particles were greater than those without iron particles. (3) The wear rates of pin and disk depended on the topographies of wear surfaces and the wear index Γ.