New voices – Mehr Research https://mehr-research.science Chemistry — Information — Discovery Wed, 18 Sep 2024 09:00:23 +0000 en-US hourly 1 https://wordpress.org/?v=6.7.1 https://mehr-research.science/wp-content/uploads/2024/01/Group-logo-150x150.png New voices – Mehr Research https://mehr-research.science 32 32 Exploring Invisible Wonders: The Magic of Aerosol Reactors in Creating Super Materials https://mehr-research.science/2024/exploring-invisible-wonders-the-magic-of-aerosol-reactors-in-creating-super-materials/ https://mehr-research.science/2024/exploring-invisible-wonders-the-magic-of-aerosol-reactors-in-creating-super-materials/#respond Wed, 18 Sep 2024 09:00:23 +0000 https://mehr-research.science/?p=756 Hello curious friends! I’m Chen Junyi, currently a graduate student specializing in Advanced Functional Materials at the University of Glasgow. Today, I want to take you on an exciting journey into the microscopic world of materials science, where tiny particles create big wonders! This adventure began with my post-graduate project, and now I’m thrilled to share it with you.

In the Scottish Highlands, verdant slopes and winding paths form a vivid backdrop. Standing before this spectacular landscape, with majestic mountains enshrouded in mist behind me, I’m immersed in the tranquility and harmony of nature.

What are COFs and MOFs?

Imagine building a miniature city, not with bricks and mortar, but with molecules! This is what we explore in research, using Covalent Organic Frameworks (COFs) and Metal-Organic Frameworks (MOFs). These aren’t just ordinary materials, but super materials that can help clean the environment, store gases, or even deliver drugs precisely where they’re needed in the body.

COFs and MOFs are made by connecting molecules into a repeating 3D pattern, kind of like constructing a giant crystal lattice but on a nanoscale. These materials are super porous, meaning they have lots of tiny holes that can capture or release other molecules. This makes them incredibly useful for a wide range of applications!

So, what is the difference between COFs and MOFs? Although both are composed of molecules connected in a repeating 3D pattern, the main differences lie in their composition and the way they are linked:

COFs : These are made entirely of light elements such as carbon, hydrogen, oxygen, etc., and are interconnected through covalent bonds (strong connections like the ones between hydrogen and oxygen in water molecules). This material is very stable and difficult to break down.

MOFs : These contain metal ions and organic ligands (molecules that help arrange the metal ions), linked via coordination bonds (a more flexible type of connection). This allows MOFs to have many different structures and a broader range of uses.

In short, if you think of them as buildings, COFs are like constructions made with one type of sturdy brick, while MOFs are built with a variety of materials, including some metal components, allowing for more complex structures. This makes MOFs more flexible in adjusting and optimizing their performance.

Crystal structure of MOF-5, constructed from octahedral Zn4O(—COO)6 SBUs and linear ditopic BDC linkers. (Image source)
What does SBU mean?

SBU (Secondary Building Unit) refers to the fundamental building blocks in COFs (Covalent Organic Frameworks) and MOFs (Metal-Organic Frameworks), typically consisting of metal ions or clusters coordinated with organic ligands to create porous structures.

How do we make these materials?

Creating COFs and MOFs can be tricky. Traditional methods are like slow cooking; they take a lot of time and energy. But under the guidance of my mentor, Dr. Hessam Mehr, we use something called an aerosol reactor. This reactor is like a magic box that allows us to create these materials faster and with less waste, which is great for the environment!

Design of the aerosol reactor used in my project. Control and activation components including Raspberry Pi Pico and atomiser driver circuit (left). Deposition area with piezoelectric atomisers and glass slides (right).
What does Piezoelectric atomiser means?

Piezoelectric atomisers use the piezoelectric effect to generate ultrasonic vibrations, which rapidly transform a liquid into a fine mist or aerosol. These devices are commonly used in applications ranging from medical nebulizers to fragrance diffusers, leveraging their ability to produce fine, consistent particles without heat.

What’s special about an aerosol reactor?

An aerosol reactor works by spraying tiny droplets or particles through a mist, which then transform into COFs or MOFs. Think of it as using a spray paint can to create a detailed mural. Each droplet has all the ingredients needed to form our materials, and when they meet, they stick together in just the right way.

Schematic diagram of aerosol reactor operation.

This method is not only quick but also very efficient. It allows us to experiment with different recipes for making COFs and MOFs, tweaking the process until we get the best possible material for a specific job, like finding the best ingredients for a super cake.

Why does this matter?

You might wonder, why should we care about these tiny materials? Well, they could be game-changers in many fields. For example, they could capture harmful gases from the air or help store renewable energy more efficiently. They might even be used in medical treatments to deliver drugs precisely where they are needed, minimizing side effects.

SEM image of IRMOF-2 synthesized using an aerosol reactor. The complex porous structure is widely used.
What does SEM means?

A Scanning Electron Microscope (SEM) is a high-resolution microscope that utilizes an electron beam to scan the surface of a specimen, creating images that reveal the surface topography and composition of materials. SEM is extensively used in fields such as materials science, biology, and industrial inspection, providing detailed insights at the nano to micro scale.

The future is bright!

Research in this field is like being both a magician and a scientist. Every day, we discover more about what these tiny structures can do and how they can help us solve some of the world’s big problems.

I hope this brief introduction to the world of COFs and MOFs has sparked your curiosity. Perhaps one day, you’ll join us in the lab to discover even more materials that can make the world a better place. Until then, keep wondering, asking questions, and exploring the world around you.

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Putting aerosols to work in supramolecular chemistry https://mehr-research.science/2024/putting-aerosols-to-work-in-supramolecular-chemistry/ https://mehr-research.science/2024/putting-aerosols-to-work-in-supramolecular-chemistry/#respond Tue, 03 Sep 2024 16:13:29 +0000 https://mehr-research.science/?p=758 Hi, my name is Li Zehua, a master students of Advance Functional Materials at the University of Glasgow, I recently completed my practical project in the Mehr research group.

This is me in France.

During my undergraduate studies, I developed a strong interest in organic chemistry. My main focus was on alkali metal catalysis and photo-induced phase change energy storage dyes, primarily using solvent-based methods to synthesize reactants and explore their reaction mechanisms— a process that was quite “traditional”. When I joined Hessam’s lab, I encountered parallel aerosol reactors for the first time. I was amazed by this novel method of synthesis and decided to experiment with synthesizing known compounds using the aerosol reactor to test its potential in compound synthesis.

Due to the exceptionally high surface area to volume ratio of droplets in aerosols, substances can more rapidly interact with the heat source or reaction environment, thereby accelerating heat transfer and reaction rates. This means that chemical reactions can be effectively promoted even at lower temperatures. In addition, the evaporation of the solvent is an endothermic process, which allows the aerosol droplets to locally increase their temperature during evaporation without the need for an external heat source. These properties make aerosol methods particularly suitable for synthesis reactions that require mild heating or low thermal initiation.For instance, in the synthesis of macrocyclic Schiff bases from aldehydes/ketones and amines, the dehydration step involved not only stabilizes the product by forming double bonds but also releases heat, providing the necessary activation energy for the reaction. This is beneficial for synthesizing longer chains or even [3+3] type macrocyclic Schiff bases. Consequently, we chose macrocyclic Schiff bases as our target products for synthesis.

What is a Schiff base?

Schiff bases are a type of chemical compound that often come up in organic chemistry. They’re made when an amine (that’s a molecule containing nitrogen bonded to three different organic groups) reacts with an aldehyde or ketone (these are types of compounds that have a carbonyl (C=O) group, which includes a carbon atom double-bonded to an oxygen atom). When they react, they form a new compound called an imine or Schiff base featuring a double bond between a nitrogen and a carbon atom. This reaction is pretty simple but super important because Schiff bases can be used in lots of different ways, like in dyes, pigments, and even some medicines.

Macrocyclic Schiff bases are like the bigger, more complex cousins of regular Schiff bases. The “macro” part of the name means large, and “cyclic” means ring-shaped, so these are large ring-shaped molecules. They also have the characteristic nitrogen-to-carbon double bond, just like regular Schiff bases. What makes them special is their size and structure, which allow them to form very stable complexes with metals. This makes them useful in more advanced applications, like catalysis (which helps speed up chemical reactions), or in creating materials that can grab and hold onto specific molecules, a bit like how a lock holds a key. This can be really handy in areas like environmental science, where you might want to capture pollutants, or in medicine, for delivering drugs to specific parts of the body.

Metals captured in a Schiff base macrocycle. Picture source: https://pubs.acs.org/doi/full/10.1021/ic701385m

What are aerosols and why use them in our experiments?

Aerosol synthesis is an innovative chemical synthesis technique that suspends reactants as extremely fine particles in a gas, with the goal of enhancing reaction efficiency and product quality. This method stands out compared to traditional solution-based approaches for several reasons. First, the reactants in aerosol form have a much larger surface area, which may speeds up reactions and increases their progress towards completion. This makes aerosol synthesis particularly suitable for chemical reactions that require fast reactivity and high yield.

Another major advantage of aerosol synthesis is its environmental friendliness. Traditional chemical synthesis often involves large amounts of organic solvents, which are not only costly but also pose significant environmental risks. Aerosol technology can significantly reduce or even eliminate the use of solvents, thereby lowering environmental impact and reducing energy consumption. For instance, in the production of nanomaterials, aerosol methods can avoid the use of organic solvents at high temperatures, reducing the emission of harmful substances.

This is our aerosol reactor

Despite its many benefits, aerosol synthesis does have some limitations. For example, it requires specialized equipment to generate and control aerosol particles, which means higher technical requirements and initial investments. Additionally, maintaining the stability of aerosols and precisely controlling particle size are technical challenges that need to be addressed in experiments. However, with ongoing technological advancements and further research, aerosol synthesis is showing tremendous potential in fields like pharmaceuticals, catalyst fabrication, and high-performance materials synthesis. As technology continues to advance, it is expected that aerosol synthesis will play an increasingly important role in chemical manufacturing, especially in an era that emphasizes green and sustainable chemical processes.

How did we approach the problem?

We started by searching for reaction formulas related to the synthesis of macrocyclic Schiff bases using the traditional bulk solution method, selecting reaction systems that are mild, with temperatures slightly above or equal to room temperature. Next, we replicate these reactions using the original published protocol to make sure they are reproducible. Once verified successfully, we then attempt to synthesize the macrocyclic Schiff bases using aerosol synthesis in our aerosol reactor.

Simplified representation of an aerosol reactor. A piezoelectric actuator (a) is used to turn the reactants in the glass vials into aerosol droplets. A cotton wick (b) connects the piezoelectric atomizer to the solvent. Products are collected on a glass slide.

To create macrocyclic Schiff bases using an aerosol reactor, we prepared two reagent vials. In one, we dissolved the amine in solvent; in the other, we dissolved aldehyde also in solvent. We also added a small amount of acid to the aldehyde mixture because acid can speed up or catalyze Schiff base formation.

Next, we fitted each reagent vial with a piezoelectric element, whose role is to convert the solution into a mist of aerosol particles, and placed the vial assembly inside the aerosol reactor. Finally, we connected the reactor to a computer which is programmed to control the emission aerosol by activating the piezoelectric elements.

What is a piezoelectric actuator?
A commercial piezoelectric actuator.

A piezoelectric atomizer is a small device that uses quick vibrations to turn liquids into a fine mist. It works by using a special material that vibrates rapidly when electricity is applied, creating pressure waves that break the liquid into tiny droplets. You can find these atomizers in everyday items like humidifiers, which add moisture to the air, aroma diffusers, which spread essential oils, and medical devices like nebulizers, which help people inhale medicine. They’re popular because they can create a fine mist without using heat, making them efficient and safe for delicate liquids.

By positioning the vials at a slight angle relative to each other, we encouraged microdroplets from each source to collide with each other to form the Schiff base. We collected the products of aerosol reaction on two glass slides within the reactor, one at the top and one at the bottom. This setup allowed us to capture and analyze the products separated afterwards.

The image above is taken from an optical microscope after the experiment, showcasing the glass slides used to collect samples. Panels (a) and (c) display the top glass slide, while panels (b) and (d) show the bottom glass slide. The bottom slide appears to have more product deposits, primarily because many of the unreacted reactants settled on it due to solvent evaporation and the effects of gravity.

After the Schiff base reaction is completed, the amine (-NH2) and aldehyde (-C=O) groups undergo a condensation reaction to form an imine bond (-C=N-). Therefore, we can use infrared spectroscopy to detect functional groups in the product and look for the (-C=N-) absorption peak, which indicates the presence of the imine bond. After calculating the theoretical molecular weight of the target product, we also used mass spectrometry to measure the mass-to-charge ratio of the reaction product, from which we can infer the actual mass of the product. By comparing the measured mass with the calculated mass, we can verify whether the molecule obtained is the target product. These steps help us to get a better idea of which product molecules have formed.

What is infrared spectroscopy?
IR Spectroscopy Instrumentation principle
Picture source(https://byjus.com/chemistry/infrared-spectroscopy/)

Infrared spectroscopy (IR) is a practical chemical analysis technique that identifies and studies chemical substances by measuring specific frequencies at which compounds absorb infrared light. Each chemical has its unique “molecular fingerprint,” consisting of a series of specific absorption peaks that reflect the vibrations of chemical bonds within the molecule. This technique allows us to quickly determine the type and molecular structure of substances and is widely used in research, quality control, and environmental monitoring. The advantages of IR spectroscopy include its speed and non-destructive nature, providing accurate chemical information without damaging the sample.

What is Mass spectroscopy?
Mass spectrometry principle demonstration diagram.
Picture source
https://en.wikipedia.org/wiki/Mass_spectrometry#/media/File:Mass_Spectrometer_Schematic.svg

Mass spectrometry (MS) is an analytical technique used to identify compounds and measure their abundance by analyzing the mass-to-charge ratio (m/z) of sample molecules. In this process, the sample is first ionized to create charged particles, which are then accelerated in an electromagnetic field and separated based on their mass-to-charge ratios. A mass spectrometer generates a spectrum by detecting these separated ions, showing the distribution of ions with different m/z values, which helps to identify the chemical substances and their structures within the sample.

The applications of mass spectrometry are vast and include drug development, biological research, environmental science, and forensic science. The main advantages of this technique are its high sensitivity and the ability to detect trace amounts of substances, providing precise molecular mass information. Mass spectrometry can also analyze multiple components in complex samples, making it an indispensable tool in modern analytical science.

The above image is a mass spectrometry image of some LC-MS, demonstrating the synthesis of macrocyclic Schiff bases. We noticed some Schiff bases in the mass spectra, but it seemed that the reaction time was not enough for the full macrocycle to be assembled.

Future plan

This study primarily showcases an innovative synthesis technique—using aerosol chemistry to manufacture macrocyclic Schiff bases. Although macrocyclic Schiff bases themselves have been extensively studied, the highlight of this research is the development of a brand new method of preparation. This method, which synthesizes through the collision of micron-sized aerosol droplets, not only enhances synthesis efficiency but also reduces environmental impact, offering a sustainable and efficient option for the field of chemical manufacturing.

In the future, we can focus on further refining this technology by introducing electrodes to enhance interactions between aerosol droplets using electrostatic forces to improve the success rate of reactions. Additionally, adjusting the boiling point of solvents and precisely controlling reaction temperatures will enhance reactivity and reduce unwanted side reactions, increasing the quality and yield of products.

These improvements will not only provide an opportunity to deeply understand the mechanisms of aerosol chemical reactions but also suggest that this new method could transform the future of chemical manufacturing. With this innovative synthesis approach, we look forward to opening a new chapter in chemical synthesis, especially in terms of efficient and environmentally friendly synthesis strategies.

This is Chen Junyi and I presenting a poster about our projects at the 2024 Macrocyclic and Supramolecular Chemistry Conference in Glasgow.

Over the past three months, I have had the privilege of being guided by Dr. Hessam Mehr, which has allowed me to rediscover the field of organic synthesis from an aerosol perspective. Without his guidance, I would not have been able to complete this complex project. Dr. Mehr’s extensive knowledge in organic chemistry, supramolecular chemistry, and software programming has been immensely beneficial to me. His expertise not only helped me address various challenges in the laboratory but also greatly broadened my academic horizon. Working with him has been a highly enjoyable and fruitful experience, deepening my understanding of chemical research.

I sincerely thank Dr. Hessam Mehr for his meticulous guidance and selfless assistance, and I hope to have the opportunity to collaborate with him again in the future. I would also like to express my gratitude to the other members of the Hessam group. I am particularly thankful to Zhang Luokun for his significant help with modeling the vial holder, Ms. Mariam Kalathil for her support in carrying out the experiments, and fellow student Chen Junyi for his valuable writing advice. Their assistance has been crucial to my research work.


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Welcoming Josu https://mehr-research.science/2024/welcoming-josu/ https://mehr-research.science/2024/welcoming-josu/#respond Fri, 24 May 2024 17:27:51 +0000 https://mehr-research.science/?p=622 We are delighted to welcome Josu to the group. Josu is visiting us from the Public University of Navarre (UPNA)’s celebrated UPNALAB group, well known for their creative solutions touching human-computer interaction, different domains of engineering, physics, and yes, chemistry. He will be staying with us until early July as he looks at the possibilities of controlling chemicals using sound waves.

More about Josu

¡Hola!

My name is Josu Irisarri and I came from Spain as a visiting researcher to learn about sound chemistry and aerosols within my 3rd PhD year. I’m really grateful for having the opportunity of sharing science, time and passion in Mehr research group at the Advance Research Center (ARC) of the University of Glasgow. I got in touch with Hessam Mehr after he came to Pamplona to visit our laboratory (UPNALAB). I was later invited to an acoustic chemistry workshop at Glasgow where I could present my research work of the past years. After that, I got on board into this lovely journey.

The UPNALAB crew wowed Hessam with their fascinating research projects last year.

This experience will be crucial not only for my personal career but also for developing my transversal skills, such as, multicultural communication or networking. Here in the ARC there are researcher from many different countries all around the world with whom I’m always enjoying good conversations.  My current main interests are in human computer interaction and contactless haptics and I’m willing to spread my maker and technical knowledge among this laboratory family.

Josu busy with experiments in the lab.

Taking black coffee with hot milk in a glass with ice cubes is my favourite activity when sited on a terrace surrounded by friends and sunny nice day. You can find me hiking the highest mountains of Scotland or visiting the mysterious lakes and islands around. Sometime I like to stop for local beer and food or trying to pronounce right the Scottish accent with words like “Hiya”, “Awright”, “Wee”, “Hapnin” or “Edinbruh”. The climate isn’t the best, although since I’m here it is mainly sunny. They say that I have brought the good weather somehow.

¡Hasta la vista!

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Exploring chemistry beyond the flask: My final year project on aerosol microdroplets https://mehr-research.science/2024/exploring-chemistry-beyond-the-flask-my-final-year-project-on-aerosol-microdroplets/ https://mehr-research.science/2024/exploring-chemistry-beyond-the-flask-my-final-year-project-on-aerosol-microdroplets/#respond Thu, 04 Apr 2024 13:42:43 +0000 https://mehr-research.science/?p=525 Hello! My name is Jakub Wosik and I’m a BSc Chemistry (Hons) student just finishing up my fourth year here at the University of Glasgow.

Last summer I was faced with the decision of what subfield of Chemistry my final year project was going to revolve around. Following a six-week summer internship in the Complex Chemistry labs of the University’s Advanced Research Centre (ARC), I was particularly keen about the possibility of tackling areas that deviated a bit more from our base curriculum or areas that one may initially associate with the field of Chemistry. I was eager to witness and understand more about the ever-evolving incorporation of automation and digitisation into the field, and learn some new, relevant skills along the way. As such, I selected “Complex Chemistry” as my top preference for my Honours project and was fortunate enough to join Dr. Hessam Mehr’s research group as a result.

In Grudziądz, Poland.

Brief project background

My seven weeks in the Mehr Group revolved around the exploration of aerosol microdroplets as a reaction medium for chemical synthesis. The idea behind this stems in part from the successful applications of other departures from traditional “flask-based” synthetic approaches, such as flow chemistry and microfluidics, with their own sets of advantages. The two main incentives for performing chemistry in the aerosol medium, i.e. in “spray” form are:

  1. The potential of different chemical pathways/reactivity as a result of substantially confined volumes — reaction acceleration in microdroplets has been a prominent observation in literature.
  2. Performing chemistry within this medium is inherently “stochastic”. Is there potential for novel pathways for a given set of chemical building blocks based on the probabilistic nature of droplet interactions within an aerosol cloud?

My experience

More specifically, my experience in the lab was very much focused on demonstrating the feasibility of some known organic reactions via an ultrasonic atomiser-based apparatus for droplet generation. The “reactor” (photographed below) was connected to a computer via a MicroPython circuit, and any chosen reaction was controlled and tuned via a Python program. One thing I very much appreciated and enjoyed was getting to assemble a physical circuit from scratch, coupling it with a script and seeing it all come to life when testing out the spraying of a solvent of choice. Hessam was very helpful and keen to demonstrate processes such as soldering and laser-cutting (for the assembly of the acrylic box, as seen in the photograph), as well as explaining the unfamiliar features of the algorithm and circuitry.

Ultrasonic atomiser set-up for a three-solution (ternary) reaction in the aerosol medium.

The biggest challenge within the project certainly had to do with my choice to explore organic reactivity in the medium, coupled with our primary method of droplet detection — microscopy. The droplets generated during a given aerosol reaction were allowed to settle onto a glass slide for visualisation under a Raspberry Pi-based RGB microscope. A reaction is deemed to have proceeded if distinct reagent and product droplets can be identified. This distinction is typically attributed to a significant difference in colour between the two — something that organic chemistry is not particularly known for. As such, my resilience was certainly tested when scouring the lands for an organic reaction that would undergo a distinct colour change in a reasonable timeframe under mild conditions. What this meant was that the eventual sight of a beautiful contrast between distinct red/orange and colourless droplets following an ado-dye synthesis in the aerosol medium put a big smile of excitement and relief on my face.

Droplets resulting from the synthesis of Sudan I in the aerosol medium.

Nearing the end of my project, with the help of Dr. Mehr’s programming expertise, I had the opportunity to witness the seemingly simple, yet promising potential of changing up the algorithm loop to facilitate multi-step reactivity involving an unstable intermediate, i.e. stoichiometric spraying in a sequential manner, as opposed to the simultaneous spraying of two atomisers as per a simple binary reaction. Starting to see the extent of how such an affordable apparatus could be tailored and fine-tuned through the power of code to facilitate a truly hands-off approach to performing mainstream chemistry in an atypical medium was, needless to say, a very rewarding way to wrap up my project.

Final thoughts; what next?

It is an understatement to say that I am incredibly grateful to Dr. Hessam Mehr for all the patience and guidance throughout my time here. The group provided me with a refreshing look at a different side of Chemistry that aims to take full advantage of where the world is heading technologically — and it’s doing so with accessibility and ease-of-communication in mind. While my time in the group is now over, with the prospect of exploring various other yet-unclear endeavours, the experience I have gained working in Mehr Research is nothing short of invaluable, and the skills I’ve developed will undoubtedly aid me in any facet of Chemistry, or many other potential career path for that matter.

At the time of writing this post I’m preparing for my final degree exams coming up in just under three weeks, so fingers crossed! What keeps me going are some great destress socials with friends; playing some great games and talking for hours about Japanese animation and graphic novels! Following graduation I hope to take some time to enjoy some lovely (hopefully!) sun with my family in Poland, as well as take my partner around some places she’s not seen there yet!

That’s all, folks!

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Crafting next-generation reaction containers out of mists of tiny particles https://mehr-research.science/2024/crafting-next-generation-reaction-containers-out-of-mists-of-tiny-particles/ https://mehr-research.science/2024/crafting-next-generation-reaction-containers-out-of-mists-of-tiny-particles/#comments Thu, 21 Mar 2024 16:48:43 +0000 https://mehr-research.science/?p=280 Hi everyone! My name is Zhang Luokun, a master student of Advanced Functional Materials from the University of Glasgow. I am currently working as an intern in the Mehr research group.

This is me in Glasgow.

Two years ago, I came to Glasgow after finishing my undergraduate studies in China. For my program, I learnt the synthesis technology and characterisation (such as atomic force microscope, transmission electron microscope, etc.) of some popular advanced materials (such as quantum dots, perovskite batteries, etc.), which will be the basis of my research work in the future.

When Hessam pitched the idea of using microdroplets as reactors, I was attracted by this crazy idea, and so embarked on a project to create micron-sized soft materials out of seaweed. This blog post is to share with you why these materials are so interesting and how we hope to use them to make the next generation of chemical containers.

What really is a chemical container?

When it comes to chemical reactions, many people think of two solutions mixed in a beaker or test tube, changing from one colour to another. The function of beakers or test tubes is to isolate the reaction from the environment. As a traditional reaction container, they have the advantages of low price and easy operation, but the disadvantages of only carrying out one kind of reaction at the same time are also obvious. If I need to do four chemical reactions and try five reactant ratios for each reaction, assuming I need 5 mL of reactant for each reaction, then I need 20 beakers or test tubes and 100 mL of reactant solution. This soon starts to become impractical when we need to examine a larger number of reactions and conditions.

Separtte one container into several parts could make different reactions do at the same time.

Perhaps you can say that, under the premise of constant total volume, if the interior of a container is divided into several smaller partitions, the above problem can be solved. This is true and indeed it’s the design idea behind more modern reaction vessels like 96 well plates.

96 well plates like the one above have become ubiquitous in the biosciences (image source).

You can even go above 96 wells and well plates with 384, 1536, and even 12,000 wells are available commercially. However, this idea soon runs into limitations. Not only would tinier wells become prohibitively expensive to manufacture, manually using them would be cumbersome and time consuming, even with the help of automation, such as robotic pipetting machines.

This is where our idea of using aerosols comes in: if we are able to turn individual aerosol particles (each just a few microns in size) into chemical containers, it would provide a fast and easy way to make millions of tiny containers that we would never be able to create manually.

Why calcium alginate?

Let’s look more closely at how exactly we are planning to create our next-generation reaction vessels. In order to build a container around an aerosol particle, the easiest way is to form it within the medium where the reaction will take place, called in situ in chemistry. Can this strategy address the challenge of building microscopic isolated chemical environments?

What does in situ mean?

The phrase in situ come from Latin, literally meaning “in its original position or place”. It can mean “locally”, “on site”, “on the premises”, or “in place” to describe where an event takes place and is used in many different contexts.

In chemistry, in situ refers to the formation of an intermediate or catalyst and its direct usage in a subsequent reaction or process without isolating or purifying it.

In related fields like metallurgy, in situ formation of intermediates can be useful as well. For example, if we want to generate TiC particles in situ in an iron alloy, we do not need to directly add TiC particles, but add titanium powder and carbon-containing toner and react them to produce titanium carbide.

This puts forward new requirements for the chemistry used to form our reaction vessels: the reaction generating the container needs to be robust and reliable (not easily affected by the reaction conditions such as temperature, pH, etc.), and it should be possible for small molecules to enter and leave the container.

The structure of alginic acid, from which alginate salts such as sodium alginate are derived (image source).

In my project, we focused on alginate-based materials to meet this challenge. Alginate is a natural polysaccharide derived from brown seaweed. Due to its unique properties such as biocompatibility, biodegradability, and the ability to form gels in the presence of divalent cations like calcium, alginate is widely used in various industries, including food, pharmaceuticals, and biomedical applications.

Calcium alginate happens to meet all of the above conditions. It is produced by cross-linking alginate using calcium ions, which works under a wide range of conditions. As a bonus, the soft structure generated this way can be rapidly dismantled in the presence of compounds like ethylenediaminetetraacetic acid (EDTA), so that we can easily release the contents of our container.

Ethylenediaminetetraacetic acid (EDTA) is a compound known for its ability to bind metal ions like Ca2+.
What does cross-linking mean?

In chemistry and biology a cross-link is a bond or a short sequence of bonds that links one polymer chain to another. Cross-linking leads to gel formation, which improves the mechanical strength and stability conpared to uncross-linking solution. The cross-linking is widely applied in drug delivery, tissue engineering, food encapsulation, etc.

How did we do it?

Usually, calcium alginate is produced by reacting sodium alginate solution with calcium chloride solution. In order to obtain micron-scale calcium alginate, though, we needed to create tiny sodium alginate droplets (smaller than the diameter of a human hair). Obviously, these droplets wouldn’t be practical to make manually, so we turned to a somewhat unusual method instead: using an ultrasonic atomiser.

What is an ultrasonic atomiser?

Ultrasonic atomisers are devices that using ultrasonic vibrations to create a fine mist or spray of liquid. They are commonly used in various applications such as humidifiers, medical nebulisers, spray-coating systems, and even in certain types of fuel injectors used in cars.

Ultrasonic humidifiers can make a fine mist of water droplets resembling steam without having to heat water up to its boiling point, so the resulting mist is cool to the touch (image source).
There’s no real fire burning in this decorative fireplace! What you see is a fine mist of water droplets with a clever orange backlight that makes it look like the flames of a wood fire. Photo credit: electric-fireplace.co.uk.

Here is how our atomiser setup works. First, we have a very cool electronic component called a piezoelectric actuator. What does the actuator do? It moves in response to an electric potential (aka voltage). If we change the voltage very rapidly (say a few hundred thousand times a second), the actuator starts to vibrate fast enough that any liquid that comes into contact with it is smashed into microscopic droplets. Second, we need a way to bring the solution in the bottle to the actuator. For this we use a wick made of cotton. One end of the wick is in contact with the liquid in the bottle and the other end touches the piezoelectric element at the mouth of the bottle. The solution is diffused through the cotton wick to the top. To summarise, when sodium alginate solution is poured into the vial the cotton wick draws it up and brings it into contact with the actuator.

The reaction space is filled with microdroplets.

Next, we energise the piezoelectric element. We can control exactly when this happens using a computer program that can be customised according to our experiment. When activated, the actuator undergoes periodic deformation, producing sound wave. But these sound waves are very high in frequency, so we cannot hear them; that’s why they are called ultrasonic pulses. The overall result is that our sodium alginate solution is broken up into microscopic droplets and ejected upward.

In our experiments, we tried two different methods of preparing calcium alginate. One was to make sodium alginate and calcium chloride solution form droplet, which reacted after collision in the air and collected by glass sheet; The other is to allow a solution of sodium alginate to form droplets, which are collected in a petri dish or beaker containing a solution of calcium chloride. We found that the second method works better when there is no intervention (such as using an electromagnetic field to control the movement of the droplets). This is probably because the likelihood of alginate and calcium droplets colliding in the air is not very large in the first method.

We didn’t only use sodium alginate and calcium solutions in our experiments. The table below shows some of the other combinations that we tried (there were many many more!). Some of these combinations gave us very interesting results that you can see in the microscopy pictures at the bottom.

ExperimentSolution 1Solution 2
aSodium alginateCalcium chloride
bSodium alginate + Sodium ferrocyanideCalcium chloride + ferric chloride
cSodium alginate + Sodium ferrocyanide + Iron oxide particleCalcium chloride + ferric chloride
dAdding EDTA (Ethylene Diamine Tetraacetic Acid) after experiment b
A list showing some of the solutions that we used for our lab experiments.

Then, we tried to introduce the reaction of iron ions into the formation of calcium alginate reaction vessel to verify that the calcium alginate generated in situ can serve as the reaction vessel. When sodium ferrocyanate solution is mixed with ferric chloride solution, the mixed solution will change from light yellow to blue. We added sodium ferrocyanate solution to sodium alginate solution so that the resulting droplets were a mixture of sodium alginate and sodium ferrocyanate, and a mixture of calcium chloride and ferric chloride was added to the petri dish. At the end of the reaction, the blue droplets can be clearly observed under the light microscope at 5.6 times magnification. This means that the reaction can be carried out in calcium alginate reaction vessels.

The next question that came to our mind was whether we could put anything, such as solid particles, inside our microscopic containers. To see if this was possible, we added iron oxide powder to the above solution of sodium ferrocyanide and sodium alginate. After the reaction, the solid particles can be clearly observed under the optical microscope (see picture c below).

These images are some of results of our experiments recorded using a microscope attached to a camera. In part (a), you can see the almost colourless calcium alginate in the dotted box. Part (b) shows the result after adding iron reaction, the microdroplets are blue. In part (c), you can see the black dots on the surface of microdroplets, which are the iron oxide particles we added in the alginate solution. Part (d) shows the result after adding EDTA in the calcium alginate droplets.

Finally, we added EDTA (Ethylene Diamine Tetraacetic Acid) to the petri dish after the reaction was completed, and after a few seconds, all the blue products previously appeared disappeared, which means that the cross-linked structure of calcium alginate can be destroyed in a short time.

Looking to the future

Many thanks to Dr. Hessam Mehr for his unwavering support and patient guidance, which enabled me to complete this project. Making tiny chemical containers is a very exciting area of research and we think that we have only begun to scratch the surface in the short period working on this project. We need to try more types of reactions to understand what other unique materials can be made using our aerosol-powered and computer-controlled techniques.

We had to tackle many challenges in this project. For example, when forming sodium alginate droplets, we found that different components of the solution require adjusting parameters such as voltage and frequency, and finding the optimal values seems to be tricky, which is also the challenge of this technology.

These days, I spent the weekends visiting some small towns around Glasgow, and enjoying the beautiful scenery, which always gives me the energy to continue my experiment with the complete enthusiasm when back in the lab.

This is me in the Oban.

At the same time, this project has allowed me to face everything that happens in scientific experiments with peace of mind. Not all experiments are a success but you can always learn something from each one, and there are always new challenges when you least expect them. I regard this period as a gentle prelude to my future academic life.

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