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Lithium-Ion Battery Production, Elemental Analysis, and a Tale as Old as Time

The challenge may not be a tale as old as time, but for those of us in many laboratories and production facilities, it's close. The issue: Achieving Both High Accuracy and Precision. And in the case of battery packagers, producers, and researchers of lithium-ion (Li-Ion) batteries for e-mobility, electronics, automotive (and more) applications, the issue of high accuracy and precision in elemental analysis is critical.

Consider how many lithium-ion batteries power your own life. Count the smartphones, laptop computers, electric vehicles (EVs), cordless power tools, and much, much more. Even with recharging and recycling, the demand for lithium batteries to power current and new applications will grow the global lithium-ion battery market to more than US$94 billion by 2025, according to one research source.

Elemental analysis is a vital element of the research and production processes. Starting materials, intermediates, and finished products must be checked for impurities that could impact battery performance. In addition, the stoichiometry of the main components of the finished material must be verified. 

Among the materials on the list for analysis are electrolytes, carbon, graphite, and lithium composite oxide cathode materials, of which there are a variety. Of these, lithium nickel manganese cobalt oxide (NMC) is easily the most prevalent. NMC is manufactured in different compositions. Verifying the ratios is critical to both the production process and the quality control for finished cathode materials — and must be measured with extremely high accuracy.

Using ICP-OES as the means of analysis, there are various strategies to help improve accuracy — from using a balance for the preparation of standards to measuring fully simultaneously. Additionally, the instrument must be in good condition — sample introduced, optimized, warmed up and stable, and preferably operated using radial plasma observation. All done, precision can be improved, and with repetitive measurements, about 0.05% RSD may be achieved.

But, as they say, more must be done. Of possible approaches bracketing a solution from the Precious Metals Industry, where high-precision and accuracy in analysis is nothing less than critical, provides further improvements.

In the Bracketing technique, an unknown sample is analyzed by cyclic analyzes of the sample and a high and a low standard in between. The high and low standards are used to calculate a correction function, which is respectively used to correct the result of the unknown sample measurements. 

Our new application report, "Analysis of Lithium Composite Oxide Cathode Materials by ICP-OES With Radial Plasma Observation," provides details of achieving both high precision and accuracy — using the bracketing technique together with the industry-leading SPECTRO ARCOS ICP-OES spectrometer with radial plasma observation. 

Featuring both simultaneous ICP-OES analysis and superior stability over time, the ARCOS analyzer offers a simple and reliable way to lithium composite oxide cathode materials at any step of the production process, from raw materials to the finished product.

With the ARCOS, sub mg/kg limits of detection can be achieved for many elements And while NMC type materials and their precursors were used for the report, other cathode materials can be analyzed using the same methodology.

Explore the bracketing methodology to tackle the challenge as old as time — achieving both high accuracy and precision in the analysis of lithium composite oxide cathode materials — by utilizing ICP-OES with radial plasma observation.

Download the new report now.
Recent Blog Posts
Julia Kiessling
Investing in the Future: From Thesis to the U.S.
Julia Kiessling, born and raised in Germany, knows SPECTRO. She completed her bachelor's degree thesis using a SPECTRO instrument and her master's degree thesis at SPECTRO in Kleve. She was hired by SPECTRO as an Application Specialist and relocated to our US headquarters in Wilmington, Massachusetts (see image below), where she's also a member of our US sustainability council. She's one of a small group of company professionals trained on all SPECTRO product lines. Julia knows SPECTRO. Let's get to know Julia.
 
SPECTRO Headquarters in Wilmington, MA, USALet's start at the beginning. What was your first contact with SPECTRO?
I was working with SPECTRO before I realized it. Writing my thesis for my bachelor's degree in Chemistry at the Niederrhein University of Applied Sciences involved analyzing the coating of metal sheets at thyssenkrupp Steel Europe AG, a steel company in Germany. I performed my analysis on a SPECTRO ARCOS, an ICP-OES instrument. That was my first contact with SPECTRO.

For my master's degree in Analytical Chemistry, I had to decide again if I wanted to write my thesis at the university or go to a company. My preference was always to get some real experience in work life and go to a company. After considering and discussing with my supervisor at the university - Professor Schram – he pointed me in the direction of SPECTRO. It was Dr. Dirk Ardelt, R&D Director Science, that I contacted there. After that call, the decision was clear.
 
How did you become interested in analytical chemistry?
To be honest, I wasn't too good at chemistry during school. I was around average, but it was always the most interesting subject. While working a year abroad in New Zealand, after school, I had enough time to think about what was interesting enough for me to spend a lot of time on to start a career. So I decided to spend time learning something that I'd enjoy doing. At university, I always thought Analytical Chemistry was the most interesting and logical, so I chose that field as my specialization.

How was your experience at SPECTRO in Kleve?
It was great! When writing my thesis, I had a lot of freedom to try things myself. And I had so much support. Whenever I had a question, they helped me. After six months, I asked the person overlooking my work on my thesis if he could imagine me staying at SPECTRO. He liked the idea and sent in my information. After two weeks, he came back to me with an answer and a question. He said they liked the idea of me working for them, but how about in the USA?

It was all really funny: Yeah, but how about three years in the USA? So I took the weekend to think about and discuss it with my partner. If you could imagine: Will you join me and go to America? He said yes, and we said Yes. So that turned out great for us!

That's a big step. First job. New continent.
But it was not right away. I had to stay for another six months in Kleve to qualify for a visa. It turned into eight months because everything was delayed because of COVID. But that was good because I spent all the time learning as much as possible about all the product lines. 

Today, I am an application specialist. I measure samples for all our products, including XRF, ICP-OES, and Spark Instruments. In addition, I do customer support, mainly for Spark applications but also a bit for ICP-OES. Last week, I was in Illinois doing customer training on a SPECTROGREEN, one of our ICP instruments. Next week, I will be in Atlanta where I will attend a trade show for Metal Forming and Welding. We will be there with one of our mobile XRF instruments.

I really like what I do. Analytical chemistry is a little bit like a riddle. Sometimes you follow recipes and know what you need to do. Sometimes it's completely different, and you must rethink what to do. It's challenging, but it's logical. Like puzzles. Solving them is the fun part.

How do you like America? What is different?
So far, very good. America is great. New England is great, especially with the white mountain forests next door. How is it different? I think the winter will be a lot different, way colder. The people seem more friendly than in Germany. Small talk is definitely easier here. Everybody's a little bit more relaxed.

Three years ago, where did you imagine you be?
When I started at SPECTRO with my thesis, I could imagine working there, but in Kleve. I had no idea that I would come to the US. That was a once-in-a-lifetime chance, and the timing was perfect. It couldn't get any better. But was I planning all this two or three years ago? No way.

And three years from now?
That's a good question since my last three-year plan got totally bombarded. I hope my manager will say stay in America. Then, maybe, my visa could be extended up to five years. That is the maximum for my visa. After that, I have to return to Germany. But in three years, I still see myself with SPECTRO. I don't know if in the USA or Germany — or somewhere else.

What's the best part of what you do here now?
I have a lot of freedom to plan my work. No one is watching every step I take. I enjoy working with and helping our customers. I also travel quite a bit when I can't help a customer over the phone and need to see the instrument and application. Every customer I visit is different. The applications are different. Some companies are small, and some are huge. Just last week, I visited a large corporation. I could see their facility from the plane. When I was there, I almost needed a map to get around. All the customers are interesting. And the locations. I have been to Texas, California, Michigan, Illinois, and Georgia next week. All in just six months, which is pretty cool.

Any special experiences?
My favorite experience so far isn't work-related. I was in California, Los Angeles for a week and spent most of my time working and training with our customer. Then, on my last day, I got up very early to go to Santa Monica Pier. I had the whole beach to myself, and I saw dolphins around 10 meters away. They were playing around in the water. That was the most magical moment. Later I was told they were probably hunting, but I kept telling myself they were playing.

Any advice for future students?
Take chances. I was very lucky, and I took all the opportunities offered to me. I never planned to end up with three years in America on my CV, but when I got the offer, I agreed. I had to. It would never be that easy to accept an offer like that again. So, my advice is: take all the chances available and be open to new experiences

And thoughts about your future?
I am very excited about being at SPECTRO. They are a great company and the market leader for metal analyzers. So that's an excellent place to start your working career. But mostly, it was the people who impressed me. Even though they didn't know me, they just took me in. And now I am in America doing my work, which I enjoy every day. So, with SPECTRO, it has been a very good partnership since the beginning, and I plan for it to continue like that in the future. 
SPECTRO and Karl-Kisters-Realschule
Investing in the Futures: Of Students, Communities, and Innovation
When officials at SPECTRO partner with and invest in the Karl Kisters Realschule in Kleve-Kellen, Germany, they are doing so with their eyes on a most ambitious return-on-investment ROI: a return on the future. In fact, many returns on many futures. The future of Karl Kisters students. The future of Kleve and surrounding communities. The future of advanced technology in industry and academia. And, of course, the future of SPECTRO and its continuing innovation and leadership.

Founded in 1997, the Karl Kisters Realschule in Kleve-Kellen today serves nearly 700 students from Kleve, Emmerich, Kranenburg, Bedburg-Hau, and Uedem, who attend the school's 24 classes in an attractive, modern facility. 

A closer look at the school's guiding principles and operation provides a clue as to SPECTRO's continuous involvement since its founding. First, there is a clear focus on delivering students options "in their personality development so they may formulate an independent vision for the next step in their education" after graduation. This includes solid opportunities for successful careers in and contributions to the fields of technology. Specifically, the school offers the start of dual training to learn a trade and later, if necessary, to train as a technician or master craftsman.

Among other fundamentals, the school embraces professional advice on school careers, the individual promotion of diverse talents, and team orientation in shared learning. Its differentiators include close links to the region and tried and tested cooperation with the regional economy, including the support of experts in the classroom.

Thus, as a partner, contributor, and supporter, SPECTRO, as a global leader in high technology research and development, innovation, and manufacturing, the fit is natural.

Around the world, the number of students pursuing vocational careers is down, threatening continued advancements and innovation in technology research, development, and manufacturing. But in Kleve, Karl Kisters focuses on math, physics, and chemistry – precisely the training SPECTRO and technology-focused institutions worldwide seek. Today, more than ever, the strategic importance of SPECTRO's multi-year relationship with Karl Kisters is evident for all involved.

SPECTRO is one of the largest employers in the region and is well known for its highly qualified vocational training. The company's partnership with the school helps give students valuable exposure — hopefully sparking an interest to consider potential paths — to technical careers in which qualified technical individuals can succeed in earning good salaries. For SPECTRO, there's a bonus: those careers can and have proven to be a source of quality career trainees for the company. It is truly a win/win endeavor.

SPECTRO's support for local educational institutions is multi-faceted and includes: 
• Lending technical experts to classes for the in-class instruction of physics in real applications so that students may learn about physics "in practice" and apply school lessons they have learned to real-world applications — and even career opportunities.
• Enabling two weeks of "practice time" at the company for practical, hands-on experience
• Undertaking specialty outreach programs to attract more women to experience potential careers in technology fields — which are currently a dominating 92% male.
• Hosting open house nights at SPECTRO to increase awareness of the public at large as to the benefits of specializing in a technology career.

In addition, this summer, to promote even closer contact between the school and the company, SPECTRO donated a host of additional resources, including physic kits, electronics kits, tools, and more, totaling around 5,200 EUR.

SPECTRO's vocational training results are impressive. More than 160 students have participated in the program since its inception, and the number of enrolled students increases yearly. SPECTRO currently employs a number of program interns, working students, and apprentices, as well as students working on their Bachelors/Masters theses. In fact, of the pupils who complete the vocation training portion of the program and receive degrees, approximately half are hired by SPECTRO. Many of the others continue their studies in pursuit of university diplomas, with some returning to SPECTRO for employment after earning their university diploma. 

In one shining example of "giving back," one former SPECTRO apprentice, Oliver van Well, is employed as a teacher at Karl Kisters. He will even serve as coordinator there for MINT jobs (mathematics, information technology, natural sciences, and technology).

Of SPECTRO's innovative partnership with Karl Kisters, one company manager explained it as such: "We are investing in improving the future — of our students, communities, and schools — as well as our technology, company, and industries. The truth is that we are investing in the future of us all."
 
Phosphate Recovery
Defusing the Phosphorus Time Bombs
The element phosphorus (P) doesn’t get enough respect. In actuality, the phosphorus originating in phosphate minerals provides nutrients essential to both animal and plant life on this planet. In humans, it’s crucial for the development, structure, and functioning of our bones and teeth, muscles, cell membranes, RNA, and DNA, for starters.

The Phosphorus Problem

Unfortunately, our supply of this vital element faces two related problems. Phosphorus is running off — and it’s running out. So we’re threatened by both environmental and sustainability phosphate time bombs. 

Both are concerns for individuals, corporations, and other organizations that try to improve environmental, social, and governance (ESG) factors to ensure a sustainable future. Can we do something about both problems? Yes. 

To understand how to defuse these twin time bombs, let’s examine the phosphorus cycle.

Mined from phosphate mineral, phosphorus is a key component of the fertilizers that help us grow crops for consumption by humans and livestock. Via both agricultural runoffs plus human and animal wastes (as well as runoffs from mining and even natural erosion), this valuable resource is eventually lost to the sea.

The runoffs lead to myriad ecological problems. These include toxic trace element buildups, harmful algal blooms, global-scale biodiversity loss, oxygen “dead zones” threatening fisheries, and the contamination of drinking water supplies.

As for the threat of phosphorus running out: while we still have substantial global deposits of phosphate suitable for extraction, accessing any given reserve may be hindered by regional supply chain issues and geopolitical barriers.

Also, phosphorus is different even from other nonrenewable resources such as oil. Because as far as we know, phosphorus won’t be replaced with something else as supplies dwindle. It can’t be made in a lab or factory. 

And without phosphorus, we can’t produce food.

Recovery and Recycling

The ultimate goal may be a closed loop: use/recover/recycle/reuse indefinitely. But meanwhile, sustaining our supply of phosphorus and managing it via environmentally sound approaches are important efforts.

Their urgency may be spurred by ongoing regulatory efforts. Example: in Germany, phosphorus recovery will become mandatory for large wastewater treatment plants by 2029. 

Also, phosphorus recovery/recycling projects can make good economic sense. Any phosphorus that’s recovered from waste products contributes to sustainability, lessens pollution — and may even increase profits.

Multiple Methods

Some older plants extract phosphorus directly from sewage sludge via thermochemical processing, yielding struvite — composed of phosphorus, ammonia, and magnesium (Mg). More recently, numerous specialized incinerator plants are under development to obtain phosphorus-rich ash from sewage sludge and other effluents. Other plants may produce phosphoric acid. Struvite, ash, and phosphoric acid all make excellent primary fertilizer ingredients.

In addition, procedures are being developed to extract phosphorus from biogas. Fermentation materials left over from the biogas generated by sewage, silage, and organic waste can be incinerated into phosphorus-bearing ash for fertilizer.

Subsidiary procedures, both thermomechanical and metallurgical, can reduce the heavy metals content of all these products.

Analytical Solutions

Whatever the process or product, accurate measurements of phosphorus, metals, and other elements are critical at multiple points in recovery and recycling. Two spectrometer technologies offer the best results for analyzing elemental contents — from incoming inspection to in-process or outgoing product quality control.

ICP-OES: SPECTROGREEN

Instruments utilizing inductively coupled plasma optical emission spectrometry (ICP- OES) are already standard for tasks such as sewage sludge and phosphoric acid analyses.

Leading analytical instrument supplier SPECTRO and its parent company AMETEK are dedicated to enabling sustainable practices in the circular economy. Example: the SPECTROGREEN analyzer. Its unique radial dual side-on interface (DSOI) plasma viewing technology equals the sensitivity of the newest vertical-torch dual-view systems — while avoiding their complexity and headaches.

Such ICP-OES instruments are already written into various industry and governmental standards for recovery/recycling analysis.

ED-XRF: SPECTRO XEPOS

A newer alternative may prove even more preferable for some facilities. Analyzers based on energy dispersive X-ray fluorescence (ED-XRF) are generally even simpler, easier to operate — often calling for little or no sample preparation.

Consider SPECTRO XEPOS, the company’s flagship ED-XRF spectrometer. It fills out SPECTRO’s analytical solution suite for the entire phosphorus recycling/recovery value chain.

This late-model, compact ED-XRF analyzer provides exceptionally fast, easy, accurate multi-elemental analysis of major, minor, and trace element concentrations, such as uranium, thorium and cadmium. Innovations in excitation and detection furnish higher sensitivity and lower detection limits than other XRF instruments in its class.

The above techniques and instruments can provide easy, efficient measurement at crucial recovery/recycling points. They’re critical to helping defuse the world’s twin phosphorus time bombs.

Get all the details in our white paper, “Effluent Phosphate Recovery & Recycling: The Latest Analytical Solutions.” No waiting!

Download now!