Direct contact ultrasound assisted freezing of mushroom (Agaricus bisporus): Growth and size distribution of ice crystals

To reduce the size of ice crystals in mushroom (Agaricus bisporus) contact ultrasound (300 W, 20 kHz) was applied during freezing and frozen storage. Stereomicroscopy was used to observe the ice crystal morphology, and DSC and NMR spectroscopy were performed to evaluate the water states in the samples. Results indicated that ultrasound irradiation initiated the nucleation of ice and reduced the mean size of ice crystals during freezing and frozen storage, and therefore improved the frozen product quality compared to the control samples. Most of the ice crystals in the ultrasound assisted frozen (UAF) samples were in the size range of 0–80 microns while that for the control samples were in the size range of 50–180 microns. SEM photos also proved that due to the application of ultrasound, the sizes of the ice crystals was reduced. This micro-scale information on the documentation of ice crystals will assist in understanding the ice crystal growth phenomena in an ultrasound assisted freezing process.     

Effects of poly-vinyl alcohol on supercooling phenomena of water

The effects of a polymer additive on the supercooling of water were investigated experimentally. Poly-vinyl alcohols (PVAs) were used as the additives, and samples were prepared by dissolving the PVA in water. Since the characteristics of PVA are decided by its degrees of polymerization and saponification, these were varied along with the concentration as the experimental parameters. Moreover, the effect of purity of the water was also considered. Each sample was cooled and the temperature at the instant when ice appeared was measured. Since the freezing of supercooled water is a statistical phenomenon, many experiments were carried out and the average degree of supercooling was obtained. It was found that PVA affects the nucleation of ice in supercooled water and the degree of supercooling increases with the addition of PVA even for water with low purity. The average degree of supercooling increases with an increase in the degree of saponification of PVA.     

超声辅助冷冻技术在食品浸渍式冷冻中的研究进展

目的 概述超声辅助冷冻技术在食品浸渍式冷冻中的研究进展,为今后新型技术辅助浸渍式冷冻提供研究方向.方法 研究超声辅助冷冻的成核机理和对冰晶生长的影响,以及超声对溶液性质的影响,并对超声辅助冷冻技术在食品浸渍式冷冻中的应用进行综述.结论 超声辅助浸渍式冷冻技术可以广泛应用在各类食品加工中,有很大的研究和发展空间.超声辅助冷冻技术能够进一步加快食品浸渍式冷冻的冻结速率,减小食品内部冰晶尺寸,较好地改善了冷冻食品的品质和风味,在食品加工中具有广阔的应用前景,可以高效应用于食品工业.     

Modelling the freezing of butter

Butter is a water-in-oil emulsion so its behaviour during freezing is very different from that of most food products, for which water forms a continuous phase. The release of latent heat during freezing is controlled as much by the rate of crystallization of water in each of the water droplets as by the rate of heat transfer. Measurements of the freezing of butter show that the release of latent heat from the freezing water depends on the degree of supercooling, which, in turn, depends on the cooling medium temperature, the size of the butter item, the packaging and the type of butter. Four modelling approaches were tested against the experimental data collected for a 25 kg block of butter. A “sensible heat only model” accurately predicted the butter temperature until temperatures at which water freezing becomes significant were reached. An “equilibrium thermal properties model” predicted a temperature plateau near the initial freezing point of the butter in a manner that was inconsistent with the measured data. A third model used a stochastic approach to ice nucleation based on supercooling using classical homogeneous nucleation theory. The predicted temperatures showed that supercooling-driven nucleation alone is not sufficient to predict the freezing behaviour of butter. A fourth approach took account of time-dependent nucleation and ice crystal growth kinetics using classical Avrami crystallization theory. The relationship between the ice crystal growth rate and the supersaturation was assumed to be linear. The model predicted the experimental data accurately, particularly by predicting the slow rebound in the temperature following supercooling that is found when freezing butter under some conditions.     

Three-dimensional measurement of ice crystals in frozen beef with a micro-slicer image processing system

A novel technique has been developed for measuring the three-dimensional (3-D) structure and distribution of ice crystals formed in frozen beef by using a micro-slicer image processing system (MSIPS). The system has functions to reconstruct the 3-D image based on the image data of exposed cross-sections obtained by multi-slicing of a frozen sample with the minimum thickness of 1 μm and to display the internal structure as well as an arbitrary cross-section of the sample choosing observation angles. The size and distribution of ice crystals can be determined from the 2-D quantitative information, such as the periphery and area of the crystals. The effects of freezing conditions on the morphology and distribution of the ice crystals were demonstrated quantitatively from the observations of raw beef stained by fluorescent indicator. For the samples frozen at −15 °C, the network structure of ice crystals were observed mainly at intercellular space, having approximately 100 μm in cross-sectional size, while that prepared at −120 °C showed the spherical crystals of 10–20 μm in diameter within the cells. The 3-D image of the sample demonstrated that the growth of ice columns was restricted by the intrinsic structure of muscle fibers. The proposed method provided a new tool to investigate the effects of freezing conditions on the size, morphology and distribution of ice crystals.     

静电场对红细胞与冰晶间相互机械性作用的影响

以红细胞悬液为研究模型,通过在对其进行慢速冻结的过程中引入静电场,具体研究了静电场对降温过程中冰晶形成与生长的影响,以及由此而引起的冰晶与细胞间相互机械作用的变化.实验结果表明:静电场在一定程度上改变了冰晶的形成与生长特性,在较强的静电场的影响下,冰晶明显变粗,成为块状,细胞完全融入粗大的冰晶之中,在冻结的末期,细胞不再受到冰晶挤压,从而减少了其所受的机械性损伤.     

Investigating the ice crystal morphology in frozen cooked rice based on size,fractal dimension and ANN modeling

Cooked rice was frozen in an air blast freezer at freezing temperatures of −5, −10, −15, −30 and −45 °C and stored at −5, −10, −15, −30 and −45 °C for up to 90 days. Cross-sectional images were captured using a fluorescence staining method, and then the equivalent diameters and perimeters of ice crystals were determined. The size and fractal dimensions were affected by the relationship between the freezing and storage temperatures. Artificial neural network analysis revealed that the behavior of response surface curves of both sizes and fractal dimensions were similar. The models demonstrated that the storage temperature of −25 °C for 90 days was required for maintaining the size and morphology of ice crystal immediately after freezing at −25 °C. These models would be effective tools for identifying the optimum operating conditions of frozen cooked rice based on the relationship between the ice crystal size and morphology.     

有关因素对冰浆制取过程中过冷度影响的实验研究

实验研究了搅拌速度、液浴温度、添加醇类物质和成核剂等因素对冰浆形成过程中过冷度及结冰特征的影响。结果表明,在制冰浆过程中,对水溶液进行搅拌有利于提高水过冷现象的稳定性。在搅拌速度0~100r/min时,不容易出现过冷现象而直接结冰;过冷度随搅拌速度增大而增大,在搅拌速度为200r/min时达到最大值4.35℃,之后过冷度急剧下降。在液浴温度降低情况下水过冷度先明显变大,随后变化不明显。添加乙二醇后,有效的改善了冰晶的细腻程度,在低浓度区(乙二醇浓度6%),过冷度呈小幅上升趋势;在中高浓度区(乙二醇浓度6%),过冷度随着乙二醇浓度的增加急剧的减小。添加成核剂后过冷度明显下降,过冷解除时间提前,与硫酸铁和二氧化硅相比,硼砂成核性较差,但是形成的冰晶具有较好的特性。     

Effects of electrode materials on freezing of supercooled water in electric freeze control

In order to clarify effects of electric charge on freezing of supercooled water, experiments were carried out with various kinds of electrodes in supercooled water. Water sample was kept in a test tube and cooled down at a constant cooling rate. When the water sample was maintained under a supercooling state, an electric charge was applied to the water sample with a small electric current. The degree of supercooling was measured continuously. Then the degree of supercooling at freezing was determined. Six kinds of materials were used for electrodes. Those materials were Aluminum, Copper, Argentum, Aurum, Platinum and Carbon. It was found that the effects of electric charge were distinct according to the material used for electrodes. The degree of supercooling at freezing was the lowest in the case of Aluminum. On the other hand, the highest value of the degree of supercooling at freezing was obtained in the case of carbon. The reason for the difference in the degree of supercooling at freezing by six materials was discussed.     

Pressure effect on the release of supercooled water with dissolved air

It is proposed that vapor has been elucidated to having relation to the release of supercooled water.In this study, considering that the vapor has a relation to dissolved air, a supercooling experiment is performed to test tubes of pure water with three patterns of initial dissolved oxygen (DO_i = 4.1, 7.5, and 12.6 mg L⁻¹), i.e. dissolved air. The initial DO in each test tube is kept to the value as constant as possible during supercooling. And the pressure effect on supercooling release of pure water is observed by measuring supercooling degree and by visualizing bubbles enclosed to the ice after full crystallization of the pure water.From this study, it appeared that the factors such as cooling rate, initial DO and pressure of pure water are related to the release of supercooling (supercooling degree and supercooling time). Moreover, the initial DO was confirmed to the confined bubble in fully frozen ice of pure water.     

Etude quantitative de la structure à l'état congelé de muscle et de steak haché

The structure of frozen meat is studied after freeze-drying, with the technique of image analysis. The variable parameters are the freezing rate, the type of meat and the effect of grinding and mixing or not with pork fat.After freezing, the samples were cut (10 μ thick), freeze-dried, fixed and stained with Regaud's haematoxylin.Using a Quantimet 720 we measured the total volume occupied by ice crystals, the distribution in size of ice crystals and the specific area of freeze-dried samples. These results were compared with those obtained by two physical methods, mercury intrusion porosimetry and the volumetric method of krypton adsorption.The comparison of stereological and physical methods suggests a spindle-shaped model for the ice-crystals in frozen whole meat.Concerning the technological parameters, the results show that grinding involves an increase of the size of ice crystals and that mixing pork fat with ground meat induces a decrease in the size of ice crystals in the pieces of meat.

Résumé

On étudie la structure de la viande congelée, aprés lyophilisation, par analyse des images. Les variables sont la vitesse de congélation, le type de viande et l'influence du hachage et de l'addition ou non de tissue adipeux de porc.Aprés congélation, les échantillons ont été coupés (10 μm d'épaisseur), lyophilisés, fixés, puis colorés à l'hématoxyline de Regaud.En utilisant un Quantimet 720 nous avons mesuré le volume total occupé par les cristaux de glace, la répartition de leurs dimensions et la surface spécifique des échantillons lyophilisés. On a comparé ces résultats à ceux obtenus par deux méthodes physiques, la porosimétrie au mercure et la méthode volumétrique d'adsorption de krypton.La comparaison des méthodes stéorologiques et physiques améne à penser que les cristaux de glace du muscle de viande congelé entier ont une forme en fuseau.Quant aux paramétres technologiques, les résultats montrent que le hachage implique une augmentation de la taille des cristaux de glace et que le mélange de tissu adipeux de porc avec la viande hachée provoque une diminution de la taille des cristaux de glance dans les morceaux de viande.     

Three-dimensional measurement of ice crystals in frozen dilute solution

A Micro-Slicer Image Processing System (MSIPS) has been applied to observe the ice crystal structures formed in frozen dilute solutions. Several characteristic parameters were also proposed to investigate the three-dimensional (3-D) morphology and distribution of ice crystals, based on their reconstructed images obtained by multi-slicing a frozen sample with the thickness of 5 μm. The values of characteristic parameters were determined for the sample images with the dimension of 530×700×1000 μm. The 3-D morphology of ice crystals was found to be a bundle of continuous or dendrite columns at any freezing condition. The equivalent diameter of ice crystals were in the range of 73–169 μm, and decreased exponentially with increasing freezing rate at the copper cooling plate temperature of −20 to −80 °C. At the T_cp −40 °C, the volumes of ice crystals were in the range of 4.6×10⁴ μm³ to 3.3×10⁷ μm³, and 36 ice columns were counted in the 3-D image.     

Laboratory experiments on frazil ice growth in supercooled water

Presented herein are the results of a laboratory investigation of the influence of turbulence and water temperature on the nature and rate of frazil ice growth in a turbulent body of supercooled water. The results indicate that the rate and the quantity of frazil ice growth increase with both increasing turbulence intensity and with decreasing water temperature at the instant of seeding, when a small fragment of ice is placed in the supercooled water. The turbulence characteristics of a flow affect the rate of frazil-ice growth by governing the temperature to which the flow can be supercooled; by influencing heat transfer from the frazil ice to surrounding water; and by promoting secondary nucleation, crystal, platelet and floc fracture, thereby increasing the number of nucleation sites available for further frazil ice growth.Larger frazil ice platelets, beginning as single crystals then becoming laminar fusions of crystals, were observed to form in water supercooled to lower temperatures. However, platelet size generally decreased with increasing turbulence intensity, as platelets with a major diameter larger than a certain value tend to break when buffeted by turbulence eddies.The investigation of frazil ice growth involved the use of a simplified analytical model, in which the rate of frazil ice growth is related to temperature rise of a turbulent volume of water due to the release of latent heat of fusion of liquid water to ice. Experiments conducted in a turbulence jar with a heated, vertically oscillating grid served both to guide and to calibrate the analytical model as well as to afford insights into frazil ice growth.     

天然活性包装膜在冷冻肉贮藏中的应用研究进展

目的 对天然活性包装膜在冷冻肉贮藏中的应用研究进展进行总结,为后续研究提供理论参考。方法 在介绍反复冻融对冷冻肉品质影响的基础上,围绕天然活性包装膜的功能成分、成膜工艺及其在冷冻肉贮藏中的应用研究予以阐述,讨论现有研究的局限性和今后的研究方向。结果 冻融过程中冰晶的反复形成影响冷冻肉体系的细胞结构和理化性质,加剧肉品品质下降;天然活性包装膜可以通过降低干耗、抑制氧化等延长肉品货架期。结论 天然活性包装膜可有效保护冷冻肉品,在肉品保鲜领域具有广阔的应用前景。     

Study on anisotropy of growth rate of ice crystal in supercooled water

The purpose of this research was to investigate the ice growth of a single crystal in three dimensions. Three-dimensional pattern of ice crystal growth in supercooled water was observed using Mach–Zehnder spectro-interferometer. Temperature was varied from −0.3 to −1.6 °C. It was found that the ice crystal began to grow as a single crystal at the tip of the capillary tube and propagated freely in supercooled water. Time variation of the shape of dendrite on a–c plane was obtained. It was found that half parabola fits the shape very closely, and the coefficient of squared term, a, of a quadratic function was calculated. The coefficient, a varied in time but at quasi steady state it was found to be depending mostly upon the degree of supercooling. Furthermore, the growth velocity in c-axis at the flat surface was calculated from the thickness measured. It was found that the velocity in c-axis is independent of the degree of supercooling but depends upon time, in other words, the thickness in c-axis.     

Geometric properties of platelet ice crystals

Sea ice that forms in McMurdo Sound, Antarctica, which is adjacent to the McMurdo and Ross Ice Shelves, exhibits the uncommon ice fabric, incorporated platelet ice. This ice fabric is the subject of a high resolution thin sectioning study, consisting of ten closely spaced horizontal sections bounded above and below by vertical sections. From these we investigate the crystallographic and geometric properties of the ice grains and find a relationship between c-axis orientation and the minor axis of an ellipse fitted to a crystal's grain boundary. Although accuracy is dependent upon the size and shape of the crystal, the technique provides a means of extracting crystallographic information from historical datasets for which only thin section photographs remain. Identification of common grains in multiple, 2-D sections allows us to reconstruct an approximation of the original 3-D crystal structures. These structures exhibit a variety of growth interactions, including upward directed crystal growth and intertwining crystals. We also construct hypothetical crystal grain boundaries that might be observed for a variety of vertical thin section orientations. These indicate that grain shape can depend on thin section orientation and illustrates some of the limitations of 2-D representations of 3-D crystals. Serrated grain boundaries are identified between neighboring crystals in several vertical sections. Geometric arguments and crystallographic observations lead us to propose a mechanism of layer nucleation within grain boundary grooves that occurs as supercooling exceeds a threshold value.     

真空搅拌法流态冰制备特性的实验研究

本文设计了一套真空搅拌法流态冰制取装置,对冰浆的生成全过程进行了观测,通过实验研究了乙二醇添加剂、溶液体积、搅拌速度等因素对冰浆形成过程过冷状态的影响。结果表明:真空状态下冰浆的制取需经历溶液蒸发、沸腾、过冷及冰晶生成这四个阶段;冰晶生成瞬间系统的压力会发生突增,压力的升值即过冷结晶压差可用于表征过冷程度的高低;平均过冷结晶压差随乙二醇添加剂浓度的增大而减小,当乙二醇浓度从3%提高至6%时,过冷结晶压差从58.9 Pa降至49.4 Pa,降低了16.1%;溶液体积的增大会使平均过冷结晶压差减小,40 m L溶液的平均过冷结晶压差较20 m L溶液的平均过冷结晶压差下降了12.9%;搅拌速度对过冷程度几乎无影响。     

Microscale study of poly(vinyl alcohol) as an effective additive for inhibiting recrystallization in ice slurries

Scanning tunneling microscopy (STM) was used to investigate the surface morphology of ice crystals containing adsorbed poly(vinyl alcohol) (PVOH) molecules inside a cold room at −7.0°C. PVOH was used as a substitute for antifreeze protein (AFP) type I, which is an effective additive for making ice slurries resistant to recrystallization. The STM images revealed microscale grooves on ice crystals made from PVOH solutions, indicating that PVOH molecules significantly influence the surface structure of the ice crystal. The length of each groove was similar to that of a PVOH molecule, indicating that PVOH molecules were adsorbed on the ice crystal surfaces. The interaction force between PVOH molecules and the ice surface was discussed by assuming a molecular structure of PVOH on the ice crystal surface, and the depression of the local freezing point was analyzed based on the surface curvature of ice revealed by STM.     

Bioinspired Multifunctional Cellular Plastics with a Negative Poisson’s Ratio for High Energy Dissipation

Cellular plastics have been widely used in transportation, aerospace, and personal safety applications owing to their excellent mechanical, thermal, and acoustic properties. It is highly desirable to impart them with a complex porous structure and composition distribution to obtain specific functionality for various engineering applications, which is challenging with conventional foaming technologies. Herein, it is demonstrated that this can be achieved through the controlled freezing process of a monomer/water emulsion, followed by cryopolymerization and room temperature thawing. As ice is used as a template, this method is environmentally friendly and capable of producing cellular plastics with various microstructures by harnessing the numerous morphologies of ice crystals. In particular, a cellular plastic with a radially aligned structure shows a negative Poisson’s ratio under compression. The rigid plastic shows a much higher energy dissipation capability compared to other materials with similar negative Poisson’s ratios. Additionally, the simplicity and scalability of this approach provides new possibilities for fabricating high-performance cellular plastics with well-defined porous structures and composition distributions.     

冰晶对冻结水产品品质的影响及抑制措施

目的为进一步优化水产品的冻结方式、改善水产品在冻藏期间的品质提供理论参考。方法介绍冰晶对水产品中蛋白质、脂质、质构特性,以及色泽、气味等感官品质的影响,冻结时形成的体积大且分布不均匀的冰晶会对水产品品质造成不可逆转的破坏。综述在水产品冻结领域中能够有效改善冰晶对水产品品质影响程度的方法,包括超声辅助冻结技术、高压处理技术、添加抗冻剂等,并对冻结技术的发展进行展望。结论为了更好地抑制冰晶形成带来的危害,在后续的研究中除了优化现有冻结技术和开发新型冻结技术外,还可以尝试将不同技术进行复合使用,谋求更佳的协同作用。此外,目前的新型冻结技术大多处于实验阶段,仍需对其作用机制进行深入探究,同时对不同技术的工艺参数进行优化。