高分子量聚碳硅烷的合成及其表征

以常压合成的低分子量聚碳硅烷(PCS)为原料,分别在470℃高压及常压下反应一定时间,制备了高分子量PCS先驱体。研究了反应时间对：PCS分子量及其分布、软化点、Si—H键含量及可纺性的影响。研究表明,随着反应时间的延长,PCS低分子量部分逐渐减少,高分子量部分逐渐增加,分子量分布逐渐变宽,从而PCS分子量逐渐增大,软化点逐渐升高,Si—H键含量逐渐降低,可纺性逐渐变差。在相同的反应时间下,高压比常压对PCS分子量的增长更有利。在470℃高压或常压下反应时间2～3h时,可获得分子量高、可纺性良好的PCS先驱体。     

聚二甲基硅烷高温高压合成聚碳硅烷工艺研究

以聚二甲基硅烷(PDMS)为原料,在高压釜内高温高压反应制备了聚碳硅烷(PCS)先驱体,研究了合成条件对反应终压、Si-H键含量、产物产率、软化点、分子量及其分布及可纺性的影响.研究表明,随着反应温度的提高,反应时间的延长,反应终压逐渐增大,产物的分子量与软化点增高,但同时分子量的分散性增大使可纺性变差.当PDMS在高压釜内460℃下反应4～6h,或450℃下反应6～7h时,可以制得软化点约为200～220℃的PCS,其高分子部分含量约 5%～10 %(质量分数),Si-H键含量大于0.9,可纺性较好,适合于制备SiC纤维.     

反应温度对液态聚硅烷高压合成聚碳硅烷性能的影响

以液态聚硅烷(LPS)为原料,在高压釜内反应制备了聚碳硅烷(PCS)先驱体。研究发现,随着反应温度的升高．PCS的分子量增大,产率提高,软化点提高．Si—H键含量降低．在反应过程中LPS首先转化为小分子量的PCS．然后是小分子的PCS间发生脱氢及少量脱甲烷缩合使分子量长大。450℃后,反应产率明显增加,分子量分布出现中分子量峰。     

含铍碳化硅陶瓷先驱体聚铍碳硅烷的合成

以氢氧化铍、硫酸和乙酰丙酮为原料合成了乙酰丙酮铍(Be(acac)2).用乙酰丙酮铍和聚碳硅烷在加热的条件下反应一定时间,生成了树脂状的产物.反应中乙酰丙酮铍被消耗,生成产物熔点相对起始聚碳硅烷熔点升高.元素分析表明产物中含有铍元素,凝胶渗透色谱分析表明产物分子量相对起始聚碳硅烷向增大的方向发生变化.傅立叶红外光谱分析表明产物中主要存在如下结构:Si(CH3)2—CH2—,—Si(CH3)·(H)—CH2—.核磁共振1H-NMR分析表明反应物中Si—H键被消耗.根据分析结果推测了反应机理,Si—H键的消耗在产物的形成中起了重要作用.实验与理论分析表明先驱体产物是一种含铍聚碳硅烷,可以命名为聚铍碳硅烷(PBeCS).在1200℃的高温处理下产物作为先驱体可以转化为碳化硅陶瓷,元素分析表明碳化硅陶瓷中含有铍,是含铍碳化硅陶瓷.     

高压合成聚碳硅烷的分子量分布与可纺性

采用高压合成方法合成了聚碳硅烷（PCS）,研究了高低分子含量、分散系数对PCS软化点、分子量分布及可纺性的影响。结果表明,可以用软化点加分子量分布来判断PCS的熔融可纺性．当PCS的软化点低于200℃,分散系数小于1．8,高、中分子含量比例小于0．1时,可纺性很好;随着分子量的增大,软化点的升高,高分子含量增加,分子量分布宽化,可纺性开始变差,当软化点大于260℃,分散系数大于2．2,高、中分子含量比例大于0,3时,可纺性很差,甚至失去可纺性。要得到软化点高、分散系数低、可纺性好的PCS,必须控制PCS的高、中分子含量比例约为0．1～0．3,低、中分子含量比例约0．8左右,分散系数约为1．8～2．2。     

聚碳硅烷纤维在环己烯气氛中的不熔化处理

将聚碳硅烷(PCS)纤维在环己烯气氛中进行化学气相交联不熔化处理,其氧含量比空气不熔化处理大大降低,组成和结构也发生了变化,气体副产物中存在环己烷和小分子硅烷.在环己烯气氛中,随着温度的升高,PCS分子的Si-H键的反应程度逐渐提高,纤维的凝胶含量逐渐增大.环己烯受热引发PCS分子中的Si-H和Si-CH3键断裂生成Si自由基和Si-CH2自由基,促进PCS分子间形成Si-CH2-Si交联结构;同时,环己烷作为侧基引入到PCS分子结构中,使纤维的碳含量随之增高.随着反应温度的升高,部分环己烷侧基和少量小分子硅烷会从PCS分子主链脱出.     

SiC陶瓷纤维先驱体——聚铝碳硅烷的合成与表征

在高温常压下,以聚二甲基硅烷(Polydimethylsilane,PDMS)和乙酰丙酮铝(Al(AcAc)3)为原料,合成了碳化硅(SiC)陶瓷纤维先驱体———聚铝碳硅烷(Polyaluminocarbosilane,PACS)。采用红外光谱法和凝胶渗透色谱法对制备的PACS进行了结构和分子量表征;通过正交实验设计,研究了反应温度、裂解温度、反应时间和原料配比4种因素对PACS的Si-H键含量、支化度和数均分子量Mn的影响,并用极差分析法进行了主次因素分析,结果表明反应温度是上述三指标的主要影响因素。综合分析各指标对PACS后续纺丝性能和高温碳化过程的影响,确定制备PACS较优的实验条件为:反应温度390℃、裂解温度490℃、反应时间10h及原料Al(AcAc)3与PDMS配比4%(质量分数)。     

含硼聚碳硅烷的制备及热解行为EI北大核心CSCD

为制备陶瓷产率高、高温性能优良的碳化硅(SiC)陶瓷先驱体,利用频那醇硼烷(PINB)与聚碳硅烷(PCS)的脱氢偶合反应,对聚碳硅烷进行化学改性。改变PINB与PCS的质量比(1∶20、1∶10、1∶5),制备了一系列不同硼(B)含量的含硼聚碳硅烷(PBCS)。通过傅里叶变换红外光谱分析、核磁共振氢谱分析、热重分析以及X射线衍射分析等手段研究了PBCS的组成、结构及热解行为。结果表明,通过B-H键的反应将B元素以PINB骨架形式引入PCS结构;引入B元素可以将PCS的陶瓷产率从78%提高至92%;另外,B元素的引入引起PCS的交联,PBCS的热解过程分3个阶段。同时B元素的引入抑制了SiC晶体的生长,将材料的耐温性能提高至1400℃。     

含铍聚碳硅烷的合成机理研究

含铍SiC陶瓷纤维是一种新型的高性能SiC纤维,而优质含铍聚碳硅烷先驱体(PBCS)的合成是得到该种纤维的重要保证。以乙酰丙酮铍(Be(acac)_2)和聚碳硅烷(PCS)为原料制备得到PBCS,并对其合成机理进行了深入研究,采用PCS和石蜡分别与Be(acac)2进行对比反应,用GC-MS对反应小分子产物进行分析,确定了Be(acac)_2与PCS的成键反应实际是Be与Si—H键反应,C—H键没有参与含铍键的形成反应;根据小分子反应产物的生成途径,合理分析了PBCS的合成反应原理。     

固/液态聚碳硅烷共混制备碳化硅纤维的研究

以超支化液态聚碳硅烷(LPCS)与固态聚碳硅烷(纯PCS)的共混物作先驱体,熔融纺丝;所得原丝再在热空气气氛中氧化交联,在高温氮气气氛中热裂解,得到碳化硅纤维。研究表明,15%(质量分数)LPCS的加入,可使纯PCS先驱体的纺丝温度,从285℃降低到225℃;纺丝性能和纤维表面质量明显提高;还可以提高氧化交联的效率,降低交联温度,从而减少纤维部分融并、粘结的弊端;虽然纤维的室温力学强度有所降低,但抗氧化性能提高,1400℃氧化交联后,力学性能几乎不变;而纯PCS的力学性能却降为原来的50%。     

Insertion of triangulated surfaces into a meccano tetrahedral discretization by means of mesh refinement and optimization procedures

In this paper, we present a new method for inserting several triangulated surfaces into an existing tetrahedral mesh generated by the meccano method. The result is a conformal mesh where each inserted surface is approximated by a set of faces of the final tetrahedral mesh. First, the tetrahedral mesh is refined around the inserted surfaces to capture their geometric features. Second, each immersed surface is approximated by a set of faces from the tetrahedral mesh. Third, following a novel approach, the nodes of the approximated surfaces are mapped to the corresponding immersed surface. Fourth, we untangle and smooth the mesh by optimizing a regularized shape distortion measure for tetrahedral elements in which we move all the nodes of the mesh, restricting the movement of the edge and surface nodes along the corresponding entity they belong to. The refining process allows approximating the immersed surface for any initial meccano tetrahedral mesh. Moreover, the proposed projection method avoids computational expensive geometric projections. Finally, the applied simultaneous untangling and smoothing process delivers a high‐quality mesh and ensures that the immersed surfaces are interpolated. Several examples are presented to assess the properties of the proposed method.     

The Research of Anti-Wear Properties of Organomolybdenum Compounds in the Engine Oils

A four-ball tester was used to evaluate the anti-wear performance of three kinds of organomolybdemun compounds in the engine oils, i. e., molybdenum dialkyldithiophosphate (MoDDP), molybdenum dialkyldithiocarbamate ( MoDTC), and sulphur and phosphorus freeorganomolybdeum (Molybdate). The results indicate that a low concentration of MoDDP doesn' t improve the anti-wear properties of the commercial engine oils, but a high concentration of MoDDP can obviously improve the anti-wear properties and the load-carrying capacity of the engine oils. MoDTC doesn' t improve the antiwear properties of the engine oils, but worsens the anti-wear properties of the oils. Signifi can timprove ment of frictional and wear characteristics is obtained with Molybdate added in the commercial engine oils and the formulated oils.     

Certification Institutions Expected to Update and Transfer Information on Present Standards

Standards are the basis for production enterprises to organize production, ex-factory inspection, trade (delivery) and technical exchanges, product certification, quality arbitration and supervision.……     

Flow calorimeter for enthalpy increment measurements on condensed gases

A flow calorimeter for enthalpy increment measurements on condensed gases is presented. A better knowledge of the properties of the liquefied natural gas is needed, and therefore a liquid loop has been designed for our flow calorimeter. The fluid loop in the calorimeter is designed in order to avoid the two-phase region, since two phases would give compositional disturbances in the measurements. The avoidance of the two-phase region is made possible by increasing the pressure of the test fluid after the measurement section, then heating the fluid at super-critical pressure past the critical point. Finally, the fluid is throttled to the low-pressure gas state at the inlet condition of the compressor that circulates the fluid. To perform the pressure increase, a new cryogenic pump has been designed. To evaluate the new equipment, measurements were taken on liquid ethane over the temperature range 146–256 K at pressure between 0.9 and 5.1 MPa.     

Refrigerators Enter a New Era of Health Preservation Frestech initiates the establishment of China's first standard for household sterilization refrigerators

On November 30, 2007, the China Association for Standardization (CAS) held a press conference at Beijing Diaoyutai State Guest House. Leaders from the China Household Electric Appliance Research Institute, the China Household Electric Appliance Association, and the China Consumers' Association attended and made speeches.……     

A study of centrifugal cast high boron high speed steel

In the present study a high‐boron high speed steel (HSS) roll material was designed. Many expensive alloy elements have been substituted by cheap boron alloy, and high‐boron high speed steel roll has been manufactured by centrifugal casting method. The microstructures, mechanical properties and wear resistance of centrifugal casting high‐boron high speed steel roll have been investigated by optical microscopy (OM), scanning electron microscopy (SEM), and X‐ray diffraction (XRD) analysis, hardness test, impact test and wear test. The results indicated that the solidification microstructures of high‐boron high speed steel roll consisted of M₂(B,C), (W,Mo)₂(B,C), M₃(B,C), M₂₃(B,C)₆ type borocarbides and martensite, a small amount of retained austenite. Borocarbides were continuously distributed over the grain boundary. After quenching from 1050 °C, local broken network appeared in partial borocarbides, and fine secondary borocarbide precipitated from the matrix. After tempering from 525 °C, the amount of precipitated borocarbide increased significantly. After heat treatment, the hardness of high‐boron high speed steel roll excelled 60 HRC, and its impact toughness excelled 8.0 J/cm². The single groove steel rolling amount of high‐boron high speed steel rolls increases by 500% than that of bainite cast iron roll, when the rolls are used in K₁ mill housing of bar mill.     

Optimum-Simulation von Ernteprozessen

Zusammenfassung Bei der Gestaltung von Ernteprozessen — beispielsweise des Prozesses Mähdrusch, Körnertransport und -abnahme — als transportverbundene Fließarbeitsverfahren mit mindestens zwei verschiedenen Arbeitsmitteln gibt es einen großen Optimierungsspielraum. Solche Prozesse sind mehrstufige Bedienungsprozesse mit gemischter Anordnung der Bedienungseinrichtungen. Außerdem besitzen sie stark ausgeprägte räumliche Aspekte. Es wird vor allem gezeigt, welche Merkmale solcher Prozesse in Simulationsmodellen abgebildet sein müssen, welche Zielgrößen in Abhängigkeit von welchen Einflußgrößen unter Berücksichtigung welcher Prozeßbedingungen ermittelt werden sollten und wie der Bewertungsprozeß zur Ermittlung der gewünschten Informationen gestaltet werden muß.     

Certification Becomes Important for the I Quality; and Safety Supervision of the Chinese Liquor Sector

The end of 2007, over 200 unit products of more than 80 Chinese firms have passed the quality grade certification for liquor products. These products involve distilled spirits, beer, wine, yellow wine, fruit syrup wine and others, and cover over 80% of the national top-branded liquor products.……     

Deposition and Coating Properties on CVD Tungsten

Surface characterization and microstructure studies are performed on chemical vapor deposited (CVD) tungsten coating. There is about 2 μm thickness diffusion layer of tungsten in the molybdenum substrate. The thermal shock test shows tungsten coating has good adhesion with molybdenum substrate, but the elements of oxygen and carbon in the tungsten coating have the bad affection to the adhesion. The result of high-temperature diffusion experiment is the diffusion rate from molybdenum substrate to tungsten coating is faster.