基于螺旋刻划方法的KDP晶体临界切削厚度研究

为了取得贴近切削加工的临界切削厚度,本文提出了一种采用金刚石刀具对KDP晶体进行螺旋刻划、基于所得刻槽微观形貌特征参数计算临界切削厚度的新方法;分析了切削速度和材料各向异性对临界切削厚度的影响;通过切削实验验证所得临界切削厚度.结果表明,晶体材料的各向异性对临界切削厚度有显著影响;在低速切削范围内,切削速度对临界切削厚度影响不显著;基于所得临界切削厚度选择切削参数,实现了KDP晶体全晶向延性域切削,取得了表面粗糙度为2.57 nm(Ra)的超光滑表面.     

基于声发射的单晶SiC材料去除机理研究

根据声发射理论,采用金刚石刀具在自动划痕仪上进行SiC单晶塑脆转换的临界条件实验,建立了SiC划痕实验过程中的声发射(AE)信号模型,利用扫描电镜(SEM)观察SiC单晶的表面形貌.结果表明,SiC划痕过程中也存在着明显的声发射Kaiser效应点,表面的划痕和切屑也表明该单晶材料同其它典型硬脆材料如玻璃和硅类似,材料去除存在着塑性到脆性的转换过程,同时分析了划痕过程中的微细粉末状碎屑的产生机理和刀具角度与塑脆转换的关系.     

玻璃陶瓷车削表面形成机制及实验研究

以玻璃陶瓷为加工对象,通过单因素车削实验研究了硬脆性材料车削机理,分析了车削深度、车削速度和进给速度对表面粗糙度的影响规律.已加工表面质量观测结果表明,随着切削深度的增加,刀具与工件挤压作用增强,表面损伤加重;随着切削速度的增加,刀具与工件作用时间减小,裂纹扩展缩短,表面破坏减弱;将切削过程分为挤压与切削两个阶段,随着进给速度的增加,在挤压阶段刀尖和工件的接触区域产生更深层裂纹,切削阶段材料崩碎加剧.测量已加工表面粗糙度,结果表明:粗糙度随切削深度和进给速度增加而增加,随切削速度增加而减小.     

SiC单晶片研磨机理及试验

SiC因其优良的物理机械性能而广泛应用于大功率器件以及IC领域.但其高的硬度和脆性导致其加工过程非常困难.本文分析了SiC单晶在研磨过程中的材料去除机理,讨论了塑性去除时磨粒的临界切削深度,建立了塑性条件下的材料去除模型.采用不同粒度的金刚石磨粒对SiC晶片进行研磨实验,验证了理论模型的正确性,结果表明在塑性模式下的材料去除能获得良好的表面形貌和较低粗糙度,同时对不同磨粒粒度的材料去除率进行了讨论.     

单晶金刚石刀具切削各向同性热解石墨的磨损机理

为了研究各向同性热解石墨切削过程中单晶金刚石刀具磨损及其对加工质量的影响,对各向同性热解石墨材料进行了切削试验.观测了刀具磨损形貌的演变过程,分析了刀具磨损机理以及刀具磨损对加工表面质量的影响.研究结果表明,在切削距离逐渐增加的情况下,单晶金刚石刀具后刀面磨损区域逐渐增大,磨损形貌分为平行沟槽和微细网状两种.切削过程中产生的颗粒状切屑和交变应力分别是导致磨粒磨损和解理磨损的主要原因.切削距离300 m内,试件加工表面粗糙度值Ra在0.2～0.4 μm之间波动,切削距离达到l000 m以后,试件加工表面粗糙度值明显增大,但是保持了相对稳定,表面粗糙度值Ra约为0.8μm.     

不同碳源浓度金刚石涂层刀具切削石材的性能研究

采用不同碳源浓度金刚石涂层刀具与未涂层刀具铣削石材,研究切削参数对切削力及加工表面质量的影响,分析刀具磨损机理,找到金刚石刀具最佳切削参数,进而实现切削优化.采用正交实验法,通过测力仪测量出不同刀具、不同切削参数下的切削力,测试已加工材料的表面粗糙度,观测刀具磨损情况.结果表明,对铣削分力Fx、Fz影响最大的是涂层碳源浓度;对铣削分力Fy影响最大的是切削深度;对表面粗糙度影响最大的是进给速度;当主轴转速达到n=3000 r/min、进给速度为vf=300 mm/min、切削深度d=1.0 mm、涂层碳源浓度为3;时,刀具切削性能最佳;3;涂层碳源浓度金刚石刀具较其他碳源浓度(含未涂层)刀具,加工后的石材表面粗糙度最低、切削力最小、耐磨性高,提高了加工精度,延长刀具的使用寿命.     

显微激光拉曼光谱法鉴别SiC晶体的多型体结构

利用显微激光拉曼光谱法对掺氮6H-SiC单晶中的寄生多型体进行了鉴别,结果表明其中有4H-SiC和15R-SiC两种寄生多型体.不同SiC多型体的纵光学声子与等离子体激元的耦合模(LOPC模)表明:在掺氮6H-SiC单晶的生长条件下,6H-SiC的掺氮效应与4H-SiC存在明显差别,而与15R-SiC的掺氮效应相似.     

基于单磨粒微米划刻的单晶硅精密切削机理研究

为了探究硅片器件精密磨削加工的切削特征与机理,运用三棱锥形状的金刚石磨粒以不同加载压力划刻单晶硅材料表面模拟磨削加工过程,分析了划痕形貌特征、切削力与切削深度的演变规律,阐释了单晶硅的微米级切削加工机理。单晶硅微破碎去除发生的临界条件为法向切削力80 mN,临界切削深度2.03 μm;剥落去除发生的临界条件为法向切削力800 mN,切削深度5.65 μm。切削深度、切削力比在不同切削机理条件下具备可区分的差异化特征。平均切削深度随加载压力的变化规律呈现出鲜明的自相似性特征。此外,还分别构建了塑性去除、微破碎去除、剥落去除三个阶段的切削力方程,更准确地描述了切削力与切削深度的密切关系。     

4H碳化硅单晶中的位错

4H碳化硅(4H-SiC)单晶具有禁带宽度大、载流子迁移率高、热导率高和稳定性良好等优异特性,在高功率电力电子、射频/微波电子和量子信息等领域具有广阔的应用前景。经过多年的发展,6英寸(1英寸=2.54 cm)4H-SiC单晶衬底和同质外延薄膜已得到了产业化应用。然而,4H-SiC单晶中的总位错密度仍高达10³~10⁴ cm^-2,阻碍了4H-SiC单晶潜力的充分发挥。本文介绍了4H-SiC单晶中位错的主要类型,重点讲述4H-SiC单晶生长、衬底晶圆加工以及同质外延过程中位错的产生、转变和湮灭机理,并概述4H-SiC单晶中位错的表征方法,最后讲述了位错对4H-SiC单晶衬底和外延薄膜的性质,以及4H-SiC基功率器件性质的影响。     

高质量半绝缘Φ150mm 4H-SiC单晶生长研究

采用数值模拟研究PVT法Φ150 mm 4H-SiC单晶生长的功率、频率选择、坩埚位置及保温厚度等关键生长参数.研究表明Φ150 mm 4H-SiC单晶生长功率是2inch 4H-SiC生长功率的2倍,优化的加热频率在5 kHz以下,系统分析不同生长参数下生长腔内径向及轴向温度梯度的变化规律.在此基础上初步的进行了Φ150 mm 4H-SiC单晶的生长工作,获得了无裂纹、直径完整的高质量SiC衬底材料.拉曼光谱Mapping测量显示Φ150 mm SiC衬底全片无多型,均为4H-SiC晶型.X光摇摆曲线显示半宽小于30 arcsec.采用掺杂过渡金属V杂质,获得了电阻率超过5×109 Ω·cm的150mmSiC衬底.     

Triethyl ammonium salt of O,O′-bis(p-tolyl)dithiophosphate, [Et3NH]+[(4-MeC6H4O)2PS2]−

Triethyl ammonium Salt of O,O′-bis(p-tolyl)dithiophosphate and O,O′-bis(m-tolyl)dithiophosphate have been obtained by reaction of p- and m-cresol, respectively with P₂S₅ in toluene and have been characterized by elemental analysis, IR, ¹H and ³¹P NMR spectroscopy. The molecular structure of O,O′-bis(p-tolyl)dithiophosphate has been determined. Crystal data: [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻: Monoclinic, P2₁/c, a=15.2441(9) ?, b=10.415(2) ?, c=3.9726(9) ?, β=91.709(7)°, V=2217.5(1) ?⁻³, Z=4.Supplementary materials Additional material available from the Cambridge Crystallographic Data Centre (CCDC no. 600927 for [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻ comprises the final atomic coordinates for all atoms, thermal parameters, and a complete listing of bond distances and angles. Copies of this information may be obtained free of charge on application to The Director, 12 Union Road, Cambridge CB2 2EZ, UK (fax: +44-1223-336033; email: deposit@ccdc.cam.ac.uk or www:http://www.ccdc.cam.ac.uk).     

Crystal structure of Zn4Na(OH)6SO4Cl·6H2O

The structure of Zn₄Na(OH)₆SO₄Cl·6H₂O, a secondary mineral from Hettstedt, Germany, was determined by single-crystal X-ray diffraction. The crystals are hexagonal,a=8.413(8),c=13.095(24) Å, space group $P\bar 3$ , Z=2. The structure was refined to R=0.0554 and R_w=0.0903 for 970 reflections with I≥3σ(I). The structure can be described as zinc hydroxide layers perpendicular toc, from which sulfates and chlorides extend. The layers are held together by a system of hydrogen bonds involving hexaaquo Na⁺ ions which occupy the interlayer space.     

Synthesis and Crystal Structure of 5-[2-(6-bromonaphthalenyloxymethyl)]-3-(4-morpholinomethyl)-1,3,4-oxadiazole-2(3<Emphasis Type="Italic">H</Emphasis>)-thione

Abstract  The title compound, C₁₈H₁₈BrN₃O₃S, a derivative of 1,3,4-oxadiazole, crystallizes in the triclinic space group P-1 with unit cell parameters a = 6.8731(3), b = 8.9994(4), c = 15.7099(6) ?, α = 92.779(3)°, β = 130.575(3)°, γ = 107.868(4)°, Z = 2. The dihedral angle between the mean planes of the planar naphthyl and morpholine (chair) rings with the planar oxadiazol ring is 50.1(8) and 76.8(6)°, respectively. The planar naphthyl ring is twisted 52.2(5)° with the mean plane of the morpholine ring. A group of four intermolecular close contacts are observed between a bromine atom and hydrogen atoms from the closely packed naphthyl, morpholine and oxy–methyl groups in the unit cell. These molecular interactions in concert with an additional series of π–π stacking interactions that occur between the center of gravity of the two 6-membered rings of the naphthalene group influence the twist angles of each of these three groups. A MOPAC AM1 calculation of the conformation energy of the crystal structure [226.0128(9) kcal] compared to that of the minimum energy structure after geometry optimization [29.9744(1) kcal] reveals a significantly reduced value. The twist angles of the three groups above also change after the AM1 calculation giving support to the influence of both intermolecular C–H···Br short-range interactions and Cg π–π stacking interactions on these angles which therefore play a role in stabilizing crystal packing. Graphical Abstract  Crystal structure of 5-{[(6-bromonaphthalen-2-yl)oxy]methyl}-3-(morpholin-4-ylmethyl)-1,3,4-oxadiazole-2(3H)-thione, C₁₈H₁₈BrN₃O₃S, is reported and its geometric and packing parameters described and compared to a MOPAC computational calculation. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal structure of irisolidone from the flowers of Pueraia lobata

Irisolidone (5,7-dihydroxy-6,4′-dimethoxyisoflavone) was isolated from the flowers of Pueraia lobata and its crystal structure was examined by X-ray single crystal diffraction. The crystal structure of irisolidone is monoclinic, space group P2₁/c with a = 15.491(9) ?, b = 7.895(4) ?, c = 13.321(7) ?, β = 110.546(9)° and Z = 4. Hydrogen bonding and aromatic π–π stacking assemble the title compound into a three-dimensional networking structure.     

Synthesis of spinacine and spinacine derivatives: crystal and molecular structures of Nπ-hydroxymethyl spinacine and Nα-methyl spinaceamine

The natural amino acid L-Spinacine (4,5,6,7-tetrahydro-1H-imidazo[4,5-c]pyridine-6-carboxylic acid) has been synthesized following a new pathway which gives a chemically and optically pure product with an excellent yield. The crystal structures of a synthetic intermediate, N^π-hydroxymethyl-spinacine, and a spinacine derivative, N^α-methyl-spinaceamine, have been investigated through X-ray diffraction: Spi(πMeOH)·H₂O, monoclinicP2 _i,a=8.571(1),b=6.682(1),c=8.588(1) Å, and β=94.67(1)^o. Spm(αMe)·2HCl·H₂O, triclinicP l,a=7.492(4),b=10.799(3),c=7.040(2) Å, α=91.88(2), β=98.36(3) and γ=73.34(3)^o. Spi(πMeOH) crystallizes with a water molecule and displays a zwitterionic character. The carboxylate group is in equatorial position and forms a short electrostatic interaction of 2.618(2) Å between one of its oxygens and the protonated nitrogen of the tetrahydropyridine ring. The crystal packing is assured by strong O?H???O, O?H???N, N?H???N intermolecular hydrogen bonds and C?H???O close contacts. The biprotonated compounds Spm(αMe) crystallizes with two Cl^? anions and a water molecule. The positive charge on the imidazole ring is delocalized on the conjugated moiety N=C?N. The crystal is built up by clusters formed by two biprotonated Spm(αMe) molecules, four Cl^? anions and two water molecules linked together by hydrogen bonds.     

X-ray Crystal Structures of [Et3NH][{(CO)5Mo(P(OCH2CMe2CH2O)O)}2H] and (CO)5Mo{μ-Ph2POPPh2}Mo(CO)5, Two Complexes Derived from the Hydrolysis of Coordinated Chloro-Phosphorous-Donor Ligands

Abstract X-ray crystal structures of [Et₃NH][{(CO)₅Mo(P(OCH₂CMe₂CH₂O)O)}₂H], 3, and (CO)₅Mo{μ-Ph₂POPPh₂}Mo(CO)₅, 2, are reported. Crystallization of 3 occurs in P-1 space group with a = 9.6944(19) ?, b = 10.814(2) ?, c = 19.730(4) ?, α = 94.24(3)°, β = 92.23(3)°, γ = 113.47(3)°, Z = 4. Crystallization of 2 occurs in C2/c space group with a = 10.357(2) ?, b = 20.149(4) ?, c = 17.155(3) ?, α = 90°, β = 97.28(3)°, γ = 90°, Z = 8. Compound 2 is a bimetallic complex with a P–O–P bridging group containing bond distances similar to that of other complexes in which two metal centers are bridged by a single R₂POPR₂ ligand. Compound 3 contains intermolecular hydrogen bonded P–O–H–O–P linkages with bond distances comparable to those seen in similar structures with intramolecular hydrogen bonding suggesting that the distance is a function of the nature of the bond and not affected by the cis arrangement of the ligands about the metal center. Graphical abstract X-ray Crystal Structures of [Et ₃ NH][{(CO) ₅ Mo(P(OCH ₂ CMe ₂ CH ₂ O) O)} ₂ H] and (CO) ₅ Mo{μ-Ph ₂ POPPh ₂ }Mo(CO) ₅ , Two Complexes Derived from the Hydrolysis of Coordinated Chloro-Phosphorous-Donor Ligands Samuel B. Owens Jr., Abha A. Kaisare and Gary M. Gray X-ray crystal structures of [Et₃NH][{(CO)₅Mo(P(OCH₂CMe₂CH₂O)O)}₂H], 3, and (CO)₅Mo{μ-Ph₂POPPh₂}Mo(CO)₅, 2, have been determined.      

Preparation,spectral studies and X-ray crystal structure of 1,3,5-triphenyl-1,5-pentanedione,C23H20O2

1,3,5-triphenyl-1,5-pentanedione, C₂₃H₂₀O₂, has been prepared and characterized by spectroscopic methods and single crystal X-ray analysis. Crystals are monoclinic, space groupP2₁/n, a=28.124(4),b=5.997(1),c=10.434(1)Å, -98.42(1)Å,Z=4. The structure has been refined to a finalR-value of 0.040 for 1625 reflections withF _o>3(F _o). The compound contains the two carbonyl groups in a mutuallycis arrangement.     

Isotope Effects in Liquid Crystal Systems: I: Phase Relationships in the Dodecylamine-H2O,Dodecylamine-D2O Systems

The phase diagrams and heats of fusion and transition have been determined for the dodecyl amine (-NH₂)/H₂O and dodecyl amine (-ND₂)/D₂O systems using direct optical observation and differential scanning calorimetry.     

Spherulitic crystallization of β‐In2Te3 by physical vapour deposition

Different morphologies of indium telluride (In₂Te₃) including novel spherulites were crystallized using the physical vapour deposition (PVD) method, by varying the difference in the growth and source zone temperature (ΔT) of a dual zone horizontal furnace assembled indigenously. Whiskers and kinked needles of In₂Te₃were grown at ΔT = 250 K and 300 K respectively, maintaining the growth zone at 500 °C. At high supersaturation (Δ T = 400 K), spherulitic crystals were obtained. The stoichiometric composition of these crystals has been confirmed using energy dispersive analysis by x‐rays (EDAX). The structure of β‐In₂Te₃ spherulitic crystals is identified as zinc blende with lattice parameter a = 6.159 Å, from x‐ray diffraction (XRD) studies. The scanning electron microscope (SEM) images revealed the radial structure of the grown spherulites. The growth mechanism for the spherulitic crystallization of β‐In₂Te₃ crystals has been discussed based on the theoretical models. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)