Insights into measuring fluid inclusions with FTIR spectroscopy

Researchers in Beijing, China are using cutting-edge technology to advance our understanding of the composition of fluid inclusions trapped in minerals. In this work, researchers probe the ongoing challenge of how to observe phase changes of these materials as a function of temperature with IR spectroscopy, whilst also accounting for temperature deviations due to the IR itself.

Improved suppression of cancerous cells by regulating the toxicity of chemotherapy medication

Doctors and researchers are investigating ways to reduce the side effects of chemotherapy medications without impacting their effectiveness. Cisplatin is a common and widely used medication that has successfully increased the cure rate of a range of cancers, including breast, lung, brain and testicular cancers, but it is not without an array of side effects from nausea to kidney failure. The aim of this research, therefore, is to increase the effectiveness of the drug enabling a reduction in the dose and thus toxicity.

Monoglyceride-structured emulsions as a probiotic delivery system for low-fat ice cream

The introduction of friendly bacteria into low-fat ice cream is a breakthrough in the search for healthy alternative comfort foods

The introduction of friendly bacteria into low-fat ice cream is a breakthrough in the search for healthy alternative comfort foods

A research group in Italy is making breakthroughs in research into improving the ability to add good bacteria, known as probiotics, into low-fat ice cream. Probiotics have been promoted for their role in maintaining or improving digestive health, and consumer awareness of these possible health benefits has led to a huge increase in demand for probiotic-enriched food and beverages, in particular  in dairy products. One difficult step has been introducing these probiotics into low-fat and healthy foods. Here, we go into more details about how the research group of the University of Udine (Italy) have achieved this.

Probiotics are live microorganisms, mainly bacteria, which are generally considered to provide beneficial effects to the human gastrointestinal system by adding “friendly” bacteria to the gut flora - some common probiotics and their purported properties are listed in the figure below.  A sufficient amount of live probiotic bacteria needs to be delivered to the intestine for these friendly bacteria to have an impact. Probiotic bacteria are susceptible to damage from the food processing and storage, as well as from the transit throughout the gastrointestinal tract.

Four types of probiotic bacteria, and some of their health-boosting properties

Four types of probiotic bacteria, and some of their health-boosting properties

Significant research efforts are being put into designing probiotic delivery systems able to protect the probiotics against the adverse conditions they face during food production, handling and consumption. One such delivery system is attracting considerable attention in the research community: Saturated monoglyceride structured emulsions (MSEs), which are emulsions consisting of oil and water phases stabilised by saturated monoglyceride. In this case, probiotics have been added to the water phase of skimmed milk.

The group from the University of Udine in Italy investigated the potential of MSEs as delivery systems of probiotics in ice cream. Firstly, they investigated the microbial viability in the emulsions during storage at 4 °C. They found the inclusion of a probiotic Lactobacillus rhamnosus strain in MSEs resulted in a high cell viability during storage at 4°C for up to 2 months [1].

Students look at structured emulsions under the microscope using various Linkam stages in the lab at the University of Udine

Students look at structured emulsions under the microscope using various Linkam stages in the lab at the University of Udine

The research team that developed the study was composed of researchers  belonging to the Department of Agricultural, Food, Animal and Environmental Sciences of the University of Udine (Italy), including Marinela Marino and Sonia Calligaris. Commenting on the research: “In our research group food technologists and food microbiologists merge their expertise to obtain functional foods containing probiotics at the microbial load considered able to confer beneficial effects to the host's health (at least 106–107 CFU/g). In this study we focused our attention on ice-cream that is a particularly challenging product. In fact, both the freezing process and the storage at very low temperatures are known to damage the cell structures leading to a reduction of microbial viability”.

In their breakthrough paper published in LWT – Food Science and Technology [2], the group used a temperature-controlled stage Linkam CSS450 to investigate the microstructure of ice-cream containing MSE delivering probiotics. The images were acquired by placing the ice cream between the parallel plates of the temperature controlled stage, cooled at -7°C. This is facilitated by the precise heating and cooling capabilities of the CSS, as well as its transparent quartz windows on the shear plates enabling optical observation.

The authors were able to observe the distribution of air bubbles into ice-cream made from different formulations with probiotics dispersed by MSEs. They were categorised into three groups as those made with sunflower oil (Oil-MSE), Anhydrous Milk Fat (AMF-MSE), and a control batch formulated with milk fat without MSEs. Air cells in each image were subdivided into three classes, depending on the maximum length of the longest line joining two points of the cell's outline and passing through the centroid (average size): class 1 consisted of air cells with 0–20 μm size, class 2 consisted of air cells with 20–40 μm size, class 3 consisted of air cells with more than 40 μm size. The percentage ratio between the number of air cells belonging to each class and the total number of air cells in the image was calculated.

Meltdown dynamics of ice creams formulated with MSEs compared to the control sample

Meltdown dynamics of ice creams formulated with MSEs compared to the control sample

Oil-MSE ice cream exhibited the lowest number of air cells that were uniformly distributed. On the other hand, AMF-MSE ice cream displayed the highest number of air cells, but they were non-uniformly distributed and closely packed leading to a structure similar to that of a foam. Finally, the control sample showed air bubbles and distribution size so that comparisons could be made between the ice cream prepared with MSE containing oil and that containing anhydrous milk fat. The researchers concluded that the presence of crystalline monoglycerides in oil-MSE containing samples probably allowed partial fat coalescence during whipping and freezing steps, leading to air bubble stabilization which resulted in higher overrun (the amount of ice cream successfully aerated).

The meltdown stability of ice cream is another quality parameter that is affected by the lipid phase structure. The results of this test are shown in the figure above. In this study, the control and the Oil-MSE ice creams showed similar meltdown profiles, whereas the sample containing AMF-MSE had the lowest meltdown resistance. Based on observations of optical microscopic images, it is likely that the high overrun value together with the very close distribution of air cells may have increased the melting rate of AMF-MSE ice cream. The images from the optical microscope can be found in the full article here.

The oil-MSE demonstrated the ability to create a melt-resistant fat network structure in ice cream when milk fat was replaced with sunflower oil. It was concluded that the monoglyceride crystalline structures formed in the MSE played both a probiotic protective and structuring role. The use of MSE containing sunflower oil makes it possible not only to successfully protect probiotic bacteria, but also to formulate a low saturated fat ice cream – which could deliver added appeal for health-conscious consumers.

Please contact Dr Marilena Marino for more information on this research.

For more information on the Linkam instrument, please contact Linkam’s Application Specialist Dr Robert Gurney.

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References

[1] Marino, M., Innocente, N., Calligaris, S., Maifreni, M., Marangone, A., & Nicoli, M. C. (2017). Viability of probiotic Lactobacillus rhamnosus in structured emulsions containing saturated monoglycerides. Journal of Functional Foods, 35, 51–59.

[2] Calligaris, S, Marino, M, Maifreni, M, Innocente, N (2018), Potential application of monoglyceride structured emulsions as delivery systems of probiotic bacteria in reduced saturated fat ice cream, LWT – Food Science & Technology, 96, 329-334.

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Researchers reveal high temperature stability of exotic Silicon phases

Silicon-based solar panels, first developed in the 1950s, are still evolving by virtue of pioneering new research into the high temperature stability of Silicon

Silicon-based solar panels, first developed in the 1950s, are still evolving by virtue of pioneering new research into the high temperature stability of Silicon

Silicon is a key component for optoelectronic devices such as solar panels and transistors. New observations on the stability of exotic silicon phases have revealed that some types of Si are stable to a much higher temperature than previously thought. Since high temperature processing is common in the development of optoelectronic devices, this has positive implications for how these new types of silicon can be used in future solar energy materials.

In a paper published in the Journal of Applied Physics, researchers at The Australian National University in collaboration with the University of Melbourne, Oak Ridge National Laboratory and the Universidad de La Laguna found that metastable silicon states achieved by indentation remained stable up to 450 °C. The research has clarified how these indentation-formed phases of silicon evolve through metastable structures such as r8-Si, to nanocrystalline phases such as hd-Si and Si-XIII.

Researchers used a combination of high-pressure indentation and high temperature annealing to ensure the silicon would undergo phase transitions into the desired phases. After the initial indentation, pressure is gradually released, and the phases are subsequently formed during the annealing step.

As the sample heated, Raman spectroscopy was used to map characteristic peaks in the silicon and thus identify the phase. As shown in the figure below, the silicon phases follow the pathway bc8/r8→Si-XIII/hd-Si→hd-Si→dc-Si, with the key finding here being that Si-XIII is seen at 100 °C and remains until 240 °C, and the crystalline hd-Si appears at around 200 °C and impressively remains beyond 450 °C.

(Top) Silicon can be in various metastable phases depending on the annealing temperature (Bottom) Chemical structures of two of these silicon phases: hd-Si and r8-Si

(Top) Silicon can be in various metastable phases depending on the annealing temperature
(Bottom) Chemical structures of two of these silicon phases: hd-Si and r8-Si


Sherman Wong, who performed the research The Australian National University (now working as a researcher at RMIT University), said: “This work allowed us to show differences in the Raman spectra of the silicon samples as a function of temperature, which lets us see when different phases are starting to appear or disappear. We were particularly interested in when Si-XIII started appearing, as it is a completely new phase, and how high a temperature we needed to go before hd-Si disappeared. It was exciting to find that hd-Si is stable at 450°C, as modern Si devices are processed at this temperature.”.

(Left to Right) Dr Sherman Wong, Prof. Jim S. Williams and Prof. Jodie E. Bradby in their lab at the Australia National University

(Left to Right) Dr Sherman Wong, Prof. Jim S. Williams and Prof. Jodie E. Bradby in their lab at the Australia National University


One of the key studies in this work was the comparison of three different annealing methods: furnace, laser, and hotstage ramped annealing. The researchers attribute their new, more accurate temperature readings for the silicon phase transitions to the improved accuracy of their temperature measurement as different phases absorbed the laser’s heat at different rates, as well as a better understanding of thinning behaviour in the samples. For the hotstage annealing, a Linkam THMS600 temperature control stage was used to precisely control the annealing temperature within a nitrogen environment. The temperature stage was also used to perform in situ Raman microscopy at a range of temperatures, as pictured in the figure below. The Raman peaks were used to identify the silicon phases, and the change in Raman intensity was then observed as a function of temperature to show when phases started changing from one to another.

Electron diffraction reflections from samples that had undergone (a) laser and (b) hot stage annealing. (c) Measured Raman peaks identifying each silicon phase at various and (d). The intensity ratio in Raman spectra for the bc8 and r8 phase as a fu…

Electron diffraction reflections from samples that had undergone (a) laser and (b) hot stage annealing. (c) Measured Raman peaks identifying each silicon phase at various and (d). The intensity ratio in Raman spectra for the bc8 and r8 phase as a function of temperature change


Silicon has been at the heart of the semiconductor industry since the mid-20th century due to its ability to be doped to achieve better electrical properties. Dopants such as phosphorus or boron are introduced into the silicon lattice to create an electron-rich (n-type) or electron-depleted (hole rich, p-type) semiconducting material. Current and voltage can then be generated from incident light via the photovoltaic effect. Silicon itself has various phases which can be induced by high pressure and temperature. By controlling the atomic structure, it is possible to enhance the absorption of incident light, which raises the photovoltaic efficiency. For example, r8-Si is predicted to have an absorption spectrum which overlaps more with the solar spectrum than standard diamond cubic silicon.

References

Wong, Sherman, et al. "Thermal evolution of the indentation-induced phases of silicon." Journal of Applied Physics 126.10 (2019): 105901.

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