Aspects of the use of polyoxyalkylene glycols in polymer quenchants

Solutions of high molecular‐weight polymers, particularly polyoxyalkylene glycols (PAGs), are used widely in the heat treatment of metals known as ‘quenching’. This is mainly because of the non‐flammable nature of the polymer solution, compared with safety hazards associated with traditional mineral‐oil based quenchants. However, the use of PAG‐based quenchants for some heat treatment processes, particularly for slow cooling speeds, has been limited. This paper describes how, through an understanding of the quenching mechanism, the quench speed of PAG‐based quenchants can be slowed by the use of additives or controlling the conditions of operation. The paper also gives an overview of the experimental measurement of polymer quenching and the factors involved in quenching.     

An ultrastructural study of cryofractured myocardial cells with special attention to the relationship between mitochondria and sarcoplasmic reticulum

A comparative study of various cryofracturing techniques has been conducted on the mammallian myocardial cell. Quench freezing of fresh or fixed tissue in melting Freon 22 resulted in severe cellular damage due to ice crystallization. Fixation with Karnovsky's fixative prior to quenching had no modifying effect on the size and distribution of the ice crystals. The crystals were orientated primarily in the direction of the long axis of the myofibrils, manifested as empty tube-like structures in the scanning electron microscope (SEM). Regular cross-bridging often seen at the Z-band levels indicated that ice crystals, at least in some portions of the cells, were confined within the sarcomere. Within the same cell the size of the ice crystals could vary considerably. Treatment of the tissue with polyvinylpyrrolidone (PVP) prior to rapid freezing had no noticeable cryoprotective effect. The surface of the thin layer of PVP surrounding the freeze dried tissue appeared amorphous in the SEM. However, the first evidence of ice crystallization was found a few micrometres under the surface. The freezing artefacts were completely circumvented if the cryofracturing was carried out on ethanol-impregnated or on critical point dried material. While the first method resulted in a smooth fracture plane passing through the cell structures, the intracellular fracture plane of the critical point dried material followed the surface of the cell organelles. Separation of the cell organelles caused by freezing or by critical point drying revealed thread-like structures extending from the mitochondrial surface. Re-examination of SEM-processed material in the transmission electron microscope (TEM) revealed that these structures were part of the sarcoplasmic reticulum (SR), and that a close contact between the SR and the outer mitochondrial membrane existed. TEM of conventional prepared material revealed that strands of electron-dense material, here named ‘mito-reticular junctional fibres’, bridged the narrow gap between the mitochondrial surface and the SR. It is suggested that these fibres have a specific anchoring function.     

The direct measurement of temperature changes within freeze-fracture specimens during rapid quenching in liquid coolants

We have evaluated the cooling rates of specimens mounted in a variety of freeze-fracture holders when plunged into a series of liquid coolants. These rates were measured using miniature thermocouples placed within the mounted specimens. The most rapid cooling rates were obtained using propane at 83 K as the coolant. When mounted on a newly devised ‘copper sandwich’ holder, specimen cooling rates in excess of 4500 K/s have been recorded. A simple guillotine-like device for quenching freeze-fracture specimens under reproducible conditions is presented.     

轴承零件硝盐淬火性能分析

分别从硬度梯度、变形控制、冷却性能调节、压碎载荷等方面对硝盐淬火后的零件性能与油基淬火后的零件性能进行试验对比分析。结果表明:与油基淬火相比,硝盐熔液化学性质稳定,淬火冷却能力强,畸变小;淬后零件的硬度梯度平缓,淬透层深,钢球压碎载荷较快速淬火油淬火的普遍提高30%左右。     

Freezing patterns in quench frozen,freeze-dried polyvinylpyrrolidone (PVP)

An SEM investigation of the effects of freezing and freeze-drying on 2 mm diameter columns as well as on 10 mm diameter thick discs of PVP was carried out using standard techniques of quench freezing and cryofracturing followed by freeze-drying. Quench freezing in liquid Freon 12 or liquid propane led to patterns of ice formation that depended on the position in the sample, the orientation of the fracture plane observed relative to the geometry of the sample and the concentration of PVP. Vitrification did not occur. Quench freezing in liquid N₂ resulted in larger ice crystals and the pattern of the crystals was much less predictable.     

Simple procedures for evaluating the cryofixation of biological samples

Ultra-rapid cooling of biological material can be achieved in the absence of cryoprotectants by using thin samples. Three methods now employed to prepare thin samples for freeze-fracture electron microscopy are compared: contacting the sample against a liquid helium-cooled copper surface (Heuser et al., 1979), spraying the sample with a jet of propane (Mueller et al., 1980), and plunging a streamlined copper ‘sandwich’ into liquid propane (Costello, 1980). In the first method a thin surface layer of the sample is ultra-rapidly cooled while in the other methods the entire sample sandwiched between sheets of conducting metals is cooled. The morphology of fracture-faces of dilauryllecithin-water systems is used to evaluate the effectiveness of cooling methods. At optimum cooling rates the initial disordered arrangement of lipid in the lamellar (L_α) phase is preserved, giving smooth fracture faces. At slower cooling rates a worm-like texture appears which signals the formation of molecular ordering characteristic of the P_β, phase. All three methods are capable of cooling these lipid-water phases as well as other more dilute aqueous suspensions without evidence of ice crystal growth or damage. Measurement of cooling rates employing miniature thermocouples embedded in samples indicates that rates for all three methods are in excess of 10,000 K/s. The propane jet (32 times 10³ K/s, slope at 273 K) exposes the sample to coolant more rapidly than the sandwich plunging method (10 times 10³ K/s, slope at 273 K) and therefore produces slightly higher cooling rates for samples of equivalent mass and thickness. Each method has its advantages. The contact method is well suited for tissues; the sandwich method is simple and inexpensive; the jet method can potentially produce the highest cooling rates. The last two methods yield complementary replicas.     

Image comparisons of snow and ice crystals photographed by light (video) microscopy and low-temperature scanning electron microscopy

Light (video) microscopy and low-temperature scanning electron microscopy (SEM) were used to examine and record images of identical precipitated and metamorphosed snow crystals as well as glacial ice grains. Collection procedures enabled numerous samples from distant locations to be shipped to a laboratory for storage and/or observation. The frozen samples could be imaged with a video microscope in the laboratory at ambient temperatures or with the low-temperature SEM. Stereo images obtained by video microscopy or low-temperature SEM greatly increased the ease of structural interpretations. The preparation procedures that were used for low-temperature SEM did not result in sublimation or melting. However, this technique did provide far greater resolution and depth of focus over that of the video microscope. The advantage of resolution was especially evident when examining the small particles associated with rime and graupel (snow crystals encumbered with frozen water droplets), whereas the greater depth of focus provided clearer photographs of large crystals such as depth hoar, and ice. Because the SEM images contained only surface information while the video images were frequently confounded by surface and internal information, the SEM images also clarified the structural features of depth hoar crystals and ice grains. Low-temperature SEM appears to have considerable promise for future investigations of snow and ice.     

Cf/SiC复合材料低温铣削工艺优化研究

对超硬金刚石刀具低温铣削Cf/SiC复合材料进行工艺优化研究,主要研究聚晶金刚石刀具低温铣削Cf/SiC复合材料过程中,低温冷却介质(干冰、液氮)和冷却工艺参数(阀体出口压力和喷嘴喷射角度)对切削力、加工表面完整性和切屑的影响规律.研究表明:在干冰、液氮低温介质的冷却作用下,工件的加工表面质量得到了较大提高,主切削力显...     

35CrMnSiA铰接销轴淬火工艺研究

通过对液压支架中35CrMnSiA铰接销轴的淬火试验，详细研究和探讨了不同淬火介质对35CrMnSiA淬火销轴力学性能的影响，旨在找到最佳的热处理淬火介质。     

Ice crystal growth in skeletal muscle fibres

Ice crystal growth was studied in rapidly frozen skeletal muscle fibres which were treated with cryo-protective additives (glycerol, DMSO, sucrose) or which were untreated. Freeze cleaving and etching was the basic method, with conventional plastic embedding and cryo-ultramicrotomy as complementary techniques. Extensive crystal growth occurred during freezing in all unprotected fibres. Just below the fibre surface the crystals were numerous but small, while deeper in the fibre they were fewer but larger. The deeper within the specimen a fibre was located, the larger, in general, was the crystal size. The crystal volume density was about 55%, irrespective of crystal size. Ice recrystallization was practically absent at the temperature normally used in cryo-sectioning (–70°C). Anti-freeze treatment eliminated crystal growth. If the anti-freeze agents were used in non-toxic concentrations, however, their effect on crystal growth was very limited. ‘Dry’-cut, freeze-dried ultra-thin cryosections of protected and unprotected fibres confirmed these observations, while sections obtained by ‘wet’ cryo-cutting showed no apparent signs of crystal growth. In plastic sections of frozen and thawed fibres a previous occurrence of crystals was only slightly indicated. In interpreting the ultrastructure in ‘wet’-cut cryo-sections of unprotected frozen mucle fibres, the distorting effects of ice crystals through mechanical compression and alterations in sectioning conditions, must be taken into consideration. Crystal growth also strongly limits the possibilities of using ‘dry’-cut sections of untreated frozen tissue for analytical electron microscopy; only the most superficial parts of the fibres seem to be suitable for microanalysis.     

磨削表面白层厚度影响因素的实验研究

通过淬硬轴承钢GCrl5的磨削实验,研究了砂轮速度、工件速度、磨削深度以及冷却方式等磨削参数对白层厚度的影响规律.实验表明:白层是由磨削过程中工件快速升温和快速冷却以及强烈的塑性变形引起的,白层厚度的变化是磨削加工过程中各种参数共同作用的结果,而其中磨削深度是主要原因,其次是砂轮速度和工件速度;白层厚度随砂轮速度和磨削深度的增大而增大;低的砂轮速度和磨削深度以及良好的冷却条件能有效抑制白层的产生.根据实验统计结果提出了预测磨削白层厚度的经验公式.     

Bi-frontal debris bed quenching analysis using counter-current flow limitation conditions

A generalized one-dimensional time-dependent quenching model is developed to assess two-stage bi-frontal quenching process in cooling hot debris beds by top-flooding. The model is formulated by dividing the control mechanisms of the quenching process into the primary, namely counter-current flow limitation (CCFL) condition, and the secondary, i.e., the effects of subcooling of incoming coolant and steam cooling in dry channels on the quenching process. In order to evaluate the primary control mechanism, two methods are proposed by the name of Imaginary Tube Concept Approach (ITCA) and Packed Bed Concept Approach (PBCA). Comparison of each method with a few experimental data is presented. The predictions based on each method, specially that of ITCA, are in good agreement with the experimental data trends.     

Freeze-drying of articular cartilage: Investigation of rat femoral heads by SEM

The results of comparative investigations of freeze-drying of joint cartilage which had not been separated from the underlying bone are reported. Fixation and ethanol and amyl acetate substitution procedures cause marked loss of ground substance and thus create surface structures which are not present to the same degree in cartilage which is simply freeze-dried. Indeed, it is questionable whether these structures are present in vivo. They were most highly developed in critical-point-dried cartilage. The main difficulty with freeze-drying is the prevention of damage caused by ice crystals. A tissue temperature of ?130°C should always be aimed for and, because of the rapid growth of ice crystals, the temperature should never be allowed to rise above ?90°C. These conditions can be fulfilled if the specimen is in good thermal contact with the cold stage and if the cooling device is equipped with a condenser which is cooled with liquid nitrogen. The better the tissue was processed, the smoother was the resulting cartilage surface and the greater was the degree to which the chondrocytes fitted the walls of their lacunae. At tissue temperatures above ?90°C, the first change which became apparent was destruction of the cell membranes. This was followed by almost complete elution of the ground substance from between the fibers and, finally, the cell nuclei were also destroyed. This damage caused by ice crystals exposed fibrous structures on the surface of the cartilage, and the appearance of these structures was superior to that produced by enzymatic methods of preparation. The disruption caused by freezing uncovered intracellular structures.     

Making EBSD on water ice routine

Electron backscatter diffraction (EBSD) on ice is a decade old. We have built upon previous work to select and develop methods of sample preparation and analysis that give >90% success rate in obtaining high‐quality EBSD maps, for the whole surface area (potentially) of low porosity (<15%) water ice samples, including very fine‐grained (<10 μm) and very large (up to 70 mm by 30 mm) samples. We present and explain two new methods of removing frost and providing a damage‐free surface for EBSD: pressure cycle sublimation and ‘ironing’. In general, the pressure cycle sublimation method is preferred as it is easier, faster and does not generate significant artefacts. We measure the thermal effects of sample preparation, transfer and storage procedures and model the likelihood of these modifying sample microstructures. We show results from laboratory ice samples, with a wide range of microstructures, to illustrate effectiveness and limitations of EBSD on ice and its potential applications. The methods we present can be implemented, with a modest investment, on any scanning electron microscope system with EBSD, a cryostage and a variable pressure capability.     

Optimization of cryogenic milling parameters for aluminum honeycomb treated by ice fixation method

This paper presents the first comprehensive investigation that aluminum honeycomb has inevitable machining defect in milling process, such as deformation, burr, and collapse. Ice fixation method was used to clamp workpieces, and inner-injection liquid nitrogen was employed for a series of cryogenic milling machining. In the machining process, the main machining parameters including in honeycomb orientation, milling width, cutting depth, cutting speed, and feed were executed experimental research. Meanwhile, the machining parameter optimization, range, and significant analysis were adopted to analyze the influence of machining parameters on the machining surface quality, as well as the optimal parameter combination and milling machining surface quality were predicted and verified. The results show that the ice fixation aluminum honeycomb method with cryogenic milling is much advanced than that of conventional ones, and many machining defects are effectively restrained. At the same time, the influence of machining parameters on machining qualities in descending order is cutting depth, cutting speed, honeycomb orientation, feed, and milling width. The minimum roughness value (Ra?=?0.356 μm) of the predicted machining surface is similar to the actual machining result (Ra?=?0.362 μm). It verifies the feasibility of the optimization method. Furthermore, it is proved that the ice fixation + liquid nitrogen cooling method has a positive effect on the high milling quality and implement efficiency for aluminum honeycomb and other difficult-to-machine materials.     

Cooling in grind-hardening operations

The grind hardening process utilizes the heat dissipation in the grinding area for inducing metallurgical transformation on the surface of the ground workpiece. The workpiece surface is selectively heated above the austenitisation temperature and subsequently is self-quenched so as to achieve the anticipated surface hardening. In order for self-quenching to occur sufficient material mass must be present to conduct the heat away from the surface. However, in the case of grind-hardening of thin workpieces or cylindrical workpieces of small diameter, the quenching has to be assisted with the application of coolant fluid. In this paper, the utilization of the coolant fluid for the grind-hardening of small diameter cylindrical parts is investigated. The rapid heating of the workpiece and the short austenitising time are taken into consideration both for the estimation of the hardness profile and the hardness penetration depth (HPD). A finite element analysis (FEA) model is developed for this specific case and its predictions are verified experimentally.     

微孔砂轮射流冲击内外冷却技术在钛合金磨削中的应用研究

论述了钛合金材料理化特性和导致磨削加工困难的原因;阐述了冷却液在磨削中的基本作用;描述了微孔砂轮射流冲击内外冷却机理;给出了微孔砂轮射流冲击内外冷却磨削钛合金零件表面质量和砂轮表面形貌电子扫描分析报告;指出微孔砂轮射流冲击内外冷却新工艺最大限度地发挥了冷却液的冷却、润滑和冲淋作用,有效地解决了磨削钛合金零件表面产生拉伤、烧伤和砂轮表面粘结等工艺难题.     

Development of a pressurized internal cooling milling cutter and its machining performance assessment

In view of the serious problem of milling heat in milling nickel-based superalloys Inconel 718, this paper investigates the heat transfer performance of internal cooling in end milling Inconel 718, and the superiority of internal cooling milling cutter's heat exchange ability during processing is explored. The flow field characteristics of cutting fluid and milling temperature are studied by Computational Fluid Dynamics (CFD) and Finite Element Method (FEM). Compared with external flood cooling, the principle of internal cooling with excellent heat transfer performance is explained and the influence of coolant pressure on lubrication performance is analyzed. Experiments for end milling of Inconel 718 under different cutting speeds and cooling conditions have been carried out. The results indicate that the simulated and measured temperatures showed an acceptable agreement. The internal cooling has better heat transfer performance compared with flood cooling. With the increase of coolant pressure, the heat exchange efficiency is gradually enhanced. When the coolant pressure rises from 2 bar to 10 bar, the milling temperature at the measured point inside the workpiece reduces by 27.55 °C, the surface roughness reduces by 12.0%, the surface residual compressive stress increases by 68.37 MPa and better surface morphology is obtained. Besides, in the experimental range, with the increase of cutting speed, milling temperature increased, the pile-up effect on the sides of scratching was weakened and better machined surface integrity was found.     

The design and use of a simple device for rapid quench-freezing of biological samples

The detailed design of a simple device for rapid quench-freezing of biological samples under reproducible conditions is presented. With spring-augmented descent, sample immersion velocity of 10 m s^?1 into a cryogenic liquid is achieved. Biological samples, loaded in Balzers planchets, Denton holders, or a newly designed ‘titanium envelope’, are suitable for rapid-freezing with this device. Using 4 μm titanium foil, light weight (1 mg) streamlined holders can easily be made to enclose cell suspensions or tissue samples. The foil envelope is designed for efficient heat dissipation while protecting the sample from possible impact or flow distortions occurring from spring-augmented immersion. Human erythrocytes, quench-frozen in the titanium envelope, were prepared for electron microscopy by the freeze-substitution technique. Two opposing 25–30 μm surface zones were frozen in the apparent absence of ice. The extended depth of cryofixation is attributed to the advantages of thin foil in the titanium envelope design and the use of rapid-immersion technique.