超声波强化溶液冻结的机理研究
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摘要
超声波辅助结晶技术以其促进固态晶核（一次晶核与二次晶核）生成、抑制晶体生长、控制结晶体粒径分布、提高结晶质量等优点，为溶液结晶以及新鲜食品冻结保存提供了一种理想的方法。但是，当前对超声波强化结晶的机理尚不清楚。本文以研究超声结晶的机理为目标，对液态溶液与固态马铃薯样品在超声场中的冻结现象进行了以下的实验研究工作：
研究了超声波诱发冰晶成核的机理。将超声波分别应用到过冷的脱气纯水与未脱气纯水，每次实验中，水样品均以0.15℃/min的速度进行冷却；均当水样品温度降为0℃时开始施加超声波直至样品容器内生成冰晶核，测量此冰晶成核温度。脱气纯水与未脱气纯水在超声波作用下的冰晶成核温度均有上升，但未脱气纯水生成冰晶核所需的过冷度要比脱气水少的多。因而推断超声波在过冷水中引发的“空化”以及“密度、能量与温度的波动起伏”对冰晶成核均有影响，但空化效应是诱发冰晶成核的主要因素。
研究了超声波促进冰晶分裂（二次结晶）的机理。利用自行研制的超声波冷却实验台，分别研究了超声波对脱气蔗糖稀溶液与未脱气蔗糖稀溶液中树枝状冰晶体的影响。实验结果表明，未脱气溶液中的树枝状冰晶体受超声波辐射2秒后已发生分裂，而脱气溶液中的树枝状冰晶体受功率相同的超声波辐射6秒后却仍未分裂。表明超声场中冰晶发生分裂的主要原因是空化效应，而不是超声波对传声介质所施加的声压。
研究了超声波抑制冰晶生长的机理。运用自制的超声波冷却实验台分别研究了超声波对脱气蔗糖稀溶液与未脱气蔗糖稀溶液中树枝状冰晶生长的影响。实验结果显示，超声波对脱气蔗糖稀溶液与未脱气蔗糖稀溶液中树枝冰晶生长速度均有抑制作用，但未脱气蔗糖溶液中树枝冰晶的生长速度要大大低于脱气蔗糖溶液中树枝冰晶的生长速度。这表明超声波在溶液中引起的空化效应是抑制冰晶生长的主要因素。
研究了超声波细化结晶体粒径尺寸的机理。分别研究了超声波对脱气饱和氯化铵溶液与未脱气饱和氯化铵溶液结晶的影响。结果显示，在相同超声波辐射下，脱气饱和氯化铵溶液与未脱气饱和氯化铵溶液的结晶均得到了强化，但未脱气饱和氯化铵溶液白浊化开始时间显著小于脱气饱和氯化铵溶液白浊化开始时间,未脱气氯化铵溶液结晶晶粒比脱气氯化铵溶液结晶晶粒更细小。这表明超声空化以及声场中溶液分子振动引起的能量、温度及密度的波动对饱和溶液的结晶均有影响，但空化是强化饱和溶液结晶的主要因素。
研究了超声波对马铃薯中液态水结晶过程的影响。通过实验分别研究了超声波对脱气冷冻液与未脱气冷冻液中马铃薯样品冻结速度的影响，研究表明，超声波在乙二醇水溶液中引起的空化效应与液相分子振动均有助于促进马铃薯样品与冷冻剂间的热量交换，进而对固态食品冻结过程起到强化作用，但空化是强化沉冻结的主要因素；
本文提出的超声波强化结晶的机理对优化超声波辅助结晶技术以及拓宽其应用领域具有重要的参考价值。
Ultrasound-assisted freezing is an excellent method for long preservation of someliquid and solid food products. With the enhancement by ultrasound during freezing,nucleation rate of crystal can be enhanced and crystal size can be reduced. Althoughultrasound has long been used to influence crystallisation of solution, the exactmechanism that explains this influence is still not clearly understood. In order to clarifyeffects of ultrasonic waves on supercoold water, the following studies were carried out:
The mechanism of nucleation of ice induced by ultrasound was studied. Theultrasonic waves have been applied to supercooled pure water and degassed water,respectively. For each experiment, water sample is cooled at a constant cooling rate of0.15°C/min and the ultrasonic waves are applied from the water temperature of0°Cuntil the water in a sample vessel nucleates. This nucleation temperature is measured.The use of ultrasound increased the nucleation temperature of both degassed water andpure water. However, the undercooling temperature for pure water to nucleate is lessthan that of degassed water. It is concluded that cavitation and fluctuations of density,energy and temperature induced by ultrasound are factors that affect the nucleation ofwater. Cavitation is a major factor for sonocrystallisation of ice.
The mechanism of secondary nucleation of ice induced by ultrasoundwasinvestigated. Experiments on ice crystals in degassed sucrose solutions and untreatedsolutions have been carried out using a novel ultrasonic cold stage device. For eachexperiment, the ultrasonic waves that are applied operated at a power output of120W.The results show that the ice dendrite crystals growing in a sucrose solution can bebroken up into smaller fragments when ultrasound was applied for2s, but thepre-existing ice dendrite crystals in a degassed sucrose solution are still unbroken whenultrasound was applied for6s. These findings confirm that cavitation induced byultrasound is a major factor for the fragmentation of ice crystals.
The mechanism of ultrasound inhibition of dendritic ice growth was studied. Theeffect of ultrasonic waves on the growth of dendritic ice in degassed sucrose solutionsand untreated solutions was investigated using a novel ultrasonic cold stage device. Theresults show that the use of ultrasound could inhibit the growth of dendritic ice in bothuntreated and degassed solutions, but the growth velocity of dendritic ice in untreated sucrose solutions is much less than that in degassed solutions. It is concluded thatcavitation and heat effect induced by ultrasound are factors that affect the the growthprocess of ice crystal. But cavitation is a major factor for the inhibition of dendritic icegrowth.
The mechanism of ultrasound reduction of crystal size was investigated. The effectsof ultrasonic waves on crystallization process of saturated ammonium chloride solutionand degassed solution are investigated by using a novel ultrasonic cold stage device.The results show that the use of ultrasound could accelerate the crystallization processof both ammonium chloride solution and degassed solution, but the cooling rate andcloudiness time of ammonium chloride solution are much less than those of degassedsolution. Furthermore, sonocrystallisation of ammonium chloride solution can result insmaller crystals than those induced by sonocrystallisation of degassed solution. It isconcluded that cavitation and fluctuations of density, energy and temperature inducedby ultrasound are factors that affect the crystallization process of saturated solutions.But cavitation is a major factor for the enhancement of saturated solution crystallization.
Immersion freezing of potatoes with the aid of ultrasound was studied. The effect ofultrasonic waves on freezing rate of potatoes in degassed coolant and untreated coolantwas investigated. The results show that cavitation and vibrational motion of the coolantmolecules induced by ultrasound are factors that affect the heat transfer between thepotato samples being frozen and the refrigerating medium. But cavitation is a majorfactor for the enhancement of the heat transfer.
The Mechanism of enhancement of solution crystallization by ultrasound putforward in this thesis could be valuable to optimization of sonocrystallisation.
研究了超声波诱发冰晶成核的机理。将超声波分别应用到过冷的脱气纯水与未脱气纯水，每次实验中，水样品均以0.15℃/min的速度进行冷却；均当水样品温度降为0℃时开始施加超声波直至样品容器内生成冰晶核，测量此冰晶成核温度。脱气纯水与未脱气纯水在超声波作用下的冰晶成核温度均有上升，但未脱气纯水生成冰晶核所需的过冷度要比脱气水少的多。因而推断超声波在过冷水中引发的“空化”以及“密度、能量与温度的波动起伏”对冰晶成核均有影响，但空化效应是诱发冰晶成核的主要因素。
研究了超声波促进冰晶分裂（二次结晶）的机理。利用自行研制的超声波冷却实验台，分别研究了超声波对脱气蔗糖稀溶液与未脱气蔗糖稀溶液中树枝状冰晶体的影响。实验结果表明，未脱气溶液中的树枝状冰晶体受超声波辐射2秒后已发生分裂，而脱气溶液中的树枝状冰晶体受功率相同的超声波辐射6秒后却仍未分裂。表明超声场中冰晶发生分裂的主要原因是空化效应，而不是超声波对传声介质所施加的声压。
研究了超声波抑制冰晶生长的机理。运用自制的超声波冷却实验台分别研究了超声波对脱气蔗糖稀溶液与未脱气蔗糖稀溶液中树枝状冰晶生长的影响。实验结果显示，超声波对脱气蔗糖稀溶液与未脱气蔗糖稀溶液中树枝冰晶生长速度均有抑制作用，但未脱气蔗糖溶液中树枝冰晶的生长速度要大大低于脱气蔗糖溶液中树枝冰晶的生长速度。这表明超声波在溶液中引起的空化效应是抑制冰晶生长的主要因素。
研究了超声波细化结晶体粒径尺寸的机理。分别研究了超声波对脱气饱和氯化铵溶液与未脱气饱和氯化铵溶液结晶的影响。结果显示，在相同超声波辐射下，脱气饱和氯化铵溶液与未脱气饱和氯化铵溶液的结晶均得到了强化，但未脱气饱和氯化铵溶液白浊化开始时间显著小于脱气饱和氯化铵溶液白浊化开始时间,未脱气氯化铵溶液结晶晶粒比脱气氯化铵溶液结晶晶粒更细小。这表明超声空化以及声场中溶液分子振动引起的能量、温度及密度的波动对饱和溶液的结晶均有影响，但空化是强化饱和溶液结晶的主要因素。
研究了超声波对马铃薯中液态水结晶过程的影响。通过实验分别研究了超声波对脱气冷冻液与未脱气冷冻液中马铃薯样品冻结速度的影响，研究表明，超声波在乙二醇水溶液中引起的空化效应与液相分子振动均有助于促进马铃薯样品与冷冻剂间的热量交换，进而对固态食品冻结过程起到强化作用，但空化是强化沉冻结的主要因素；
本文提出的超声波强化结晶的机理对优化超声波辅助结晶技术以及拓宽其应用领域具有重要的参考价值。
Ultrasound-assisted freezing is an excellent method for long preservation of someliquid and solid food products. With the enhancement by ultrasound during freezing,nucleation rate of crystal can be enhanced and crystal size can be reduced. Althoughultrasound has long been used to influence crystallisation of solution, the exactmechanism that explains this influence is still not clearly understood. In order to clarifyeffects of ultrasonic waves on supercoold water, the following studies were carried out:
The mechanism of nucleation of ice induced by ultrasound was studied. Theultrasonic waves have been applied to supercooled pure water and degassed water,respectively. For each experiment, water sample is cooled at a constant cooling rate of0.15°C/min and the ultrasonic waves are applied from the water temperature of0°Cuntil the water in a sample vessel nucleates. This nucleation temperature is measured.The use of ultrasound increased the nucleation temperature of both degassed water andpure water. However, the undercooling temperature for pure water to nucleate is lessthan that of degassed water. It is concluded that cavitation and fluctuations of density,energy and temperature induced by ultrasound are factors that affect the nucleation ofwater. Cavitation is a major factor for sonocrystallisation of ice.
The mechanism of secondary nucleation of ice induced by ultrasoundwasinvestigated. Experiments on ice crystals in degassed sucrose solutions and untreatedsolutions have been carried out using a novel ultrasonic cold stage device. For eachexperiment, the ultrasonic waves that are applied operated at a power output of120W.The results show that the ice dendrite crystals growing in a sucrose solution can bebroken up into smaller fragments when ultrasound was applied for2s, but thepre-existing ice dendrite crystals in a degassed sucrose solution are still unbroken whenultrasound was applied for6s. These findings confirm that cavitation induced byultrasound is a major factor for the fragmentation of ice crystals.
The mechanism of ultrasound inhibition of dendritic ice growth was studied. Theeffect of ultrasonic waves on the growth of dendritic ice in degassed sucrose solutionsand untreated solutions was investigated using a novel ultrasonic cold stage device. Theresults show that the use of ultrasound could inhibit the growth of dendritic ice in bothuntreated and degassed solutions, but the growth velocity of dendritic ice in untreated sucrose solutions is much less than that in degassed solutions. It is concluded thatcavitation and heat effect induced by ultrasound are factors that affect the the growthprocess of ice crystal. But cavitation is a major factor for the inhibition of dendritic icegrowth.
The mechanism of ultrasound reduction of crystal size was investigated. The effectsof ultrasonic waves on crystallization process of saturated ammonium chloride solutionand degassed solution are investigated by using a novel ultrasonic cold stage device.The results show that the use of ultrasound could accelerate the crystallization processof both ammonium chloride solution and degassed solution, but the cooling rate andcloudiness time of ammonium chloride solution are much less than those of degassedsolution. Furthermore, sonocrystallisation of ammonium chloride solution can result insmaller crystals than those induced by sonocrystallisation of degassed solution. It isconcluded that cavitation and fluctuations of density, energy and temperature inducedby ultrasound are factors that affect the crystallization process of saturated solutions.But cavitation is a major factor for the enhancement of saturated solution crystallization.
Immersion freezing of potatoes with the aid of ultrasound was studied. The effect ofultrasonic waves on freezing rate of potatoes in degassed coolant and untreated coolantwas investigated. The results show that cavitation and vibrational motion of the coolantmolecules induced by ultrasound are factors that affect the heat transfer between thepotato samples being frozen and the refrigerating medium. But cavitation is a majorfactor for the enhancement of the heat transfer.
The Mechanism of enhancement of solution crystallization by ultrasound putforward in this thesis could be valuable to optimization of sonocrystallisation.
引文
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