My Secondment to Hiden Analytical

One of the industrial partners within EUROPAH is Hiden Analytical, a company with a more than 35-year long history of design, development and manufacture of quadrupole mass spectrometers for advanced research applications and specialist process monitoring. The application possibilities of Hiden’s mass spectrometers and advanced systems range from vacuum, gas, plasma to surface science and if the solution to your problem is not yet included in Hiden’s product range, they provide solutions to meet client specific requirements.

As an ESR within EUROPAH I had the opportunity to accomplish a 2-month internship as a secondment at Hiden Analytical, located in Warrington, United Kingdom, in order to gain experience working in an industrial environment. Managing Director Peter Hatton and I were in contact for several weeks in order to figure out a schedule and a project plan for my time at the company. My secondment began in mid-March, right after the EPoLM-4 meeting many of us ESRs attended in Madrid.

My first week started off with a detailed introduction into the world of Hiden’s quadrupole mass spectrometers and their wide range of applications. Paul Jones, Production Director, heartily welcomed me to the Hiden team and introduced me to his coworkers as well as many different instruments and systems. Paul has worked at Hiden for over 26 years and is responsible for the day to day production. This includes managing customer orders, ensuring that all parts from the quadrupole assembling, the vacuum build, and the electronics department come together in time for being tested and finally shipped to the customer. Paul has to estimate and communicate the shipping date to the customer which means he has to consider difficulties and make sure everything concerning the production of the ordered mass spectrometer system runs smoothly. He relies on his colleagues’ knowledge who have a total of several hundreds of years of experience. Paul considers himself very lucky to have gotten the opportunity to work in such a stable and pleasant environment and these positive vibes are exactly what he sends out every day. During this first week, I learned a lot about the concept of quadrupole mass spectrometry, how to master Hiden’s own software in order to run their mass spectrometers and system testing in general.

The largest part of my secondment at Hiden was a characterization project of differently coated silicon samples using the TPD Workstation and the SIMS Workstation.

The differently coated silicon samples reflect different wavelengths and therefore shimmer in different colours.

My supervisor for the temperature programmed desorption (TPD) experiments was Dr David Lundie who is Product Manager for Advanced Systems at Hiden. His industry-based PhD research topic catalysis opened the doors to Hiden, where he develops new solutions for temperature programmed processes since 2003. Once a newly developed advanced system is sold to the customer, David is also responsible for the installation and training of the customer for this new product at the customer’s site. This means David regularly travels to various places including not only Europe, but also North America, Asia and Australia, which is one of the tasks he enjoys the most about his job. David trained me on the Hiden TPD Workstation, an advanced experimental system consisting of an ultrahigh vacuum chamber, a load lock system, primary and turbomolecular pumps, as well as a quadrupole mass spectrometer which can measure mass-to-charge ratios from 1 to 300 amu, specialized for TPD experiments in which the species desorbing from a heated surface are collected by a mass spectrometer. The TPD Workstation is widely used for analyzing the surface, interlayer and bulk desorption properties of semiconductor and metal samples. Once I was familiar with the instrument, we analysed six different samples for the desorption of hydrogen, water and carbon monoxide, which play an important role in the production and characterization of solar cells. Since the TPD Workstation provides a very high resolution and sensitivity, the formation of sharp peaks was observable in the spectra. By having a closer look on the used samples, we noticed that during the heating some of the samples’ coatings developed blisters which can be seen by the use of a microscope but also by eye.

The TPD Workstation with its 1000° C hot heating plate.

We decided to further investigate the blistering with help from the secondary ion mass spectrometer (SIMS) specialists Dr Graham Cooke and Dr Kareem El-Abiary who are responsible for developing and maintaining the SIMS Workstation. 

Graham first came in contact with SIMS during his PhD in semiconductor analysis and, since 2006, he develops new SIMS related instruments at Hiden. One of his first big accomplishments was the design and manufacture of a cesium ion gun which is an important feature for the SIMS Workstation. But as Principal Scientist, Graham is also responsible for liaising with his Hiden colleagues about SIMS related problems and the support and service of ca.thirty big SIMS instruments distributed around the globe, which he proceeds through Skype or Team Viewer sessions as well as visits to the customer’s site. For this large variety, Graham appreciates his job; “You never quite know what will happen each day”, he says. The variety and the supportive environment are also Kareem’s favorites about his job at Hiden. Similarly to David, Kareem graduated in catalysis and started his career with a knowledge transfer partnership which means he worked 50% in research and 50% in industry. Kareem is fairly new to the company as he started as a trainee in 2017 but evolved to be Hiden’s SIMS Application Specialist now. His main responsibilities include customer support regarding operating the different SIMS stations and testing of customer’s samples. Together with Graham, he also tests upgrades and new components for the SIMS Workstation and writes technical sheets and application notes which are helpful features for those who attend conferences in order to inform about Hiden’s products. 

The inside of the SIMS Workstation ultrahigh vacuum chamber.

Graham and Kareem introduced me to the SIMS Workstation which was designed to perform high sensitivity analysis of surfaces and thin solids. In SIMS experiments, a primary ion beam is directed to a sample positioned in an ultrahigh vacuum chamber. When impinging the surface, the primary ions sputter small amounts off the sample’s surface. These small amounts composed of elements and molecules – the secondary ions – can then be detected and identified with a mass spectrometer. As the primary ions sputter more and more off the sample over time, depth profiles can be recorded yielding insights into the concentrations of impurities or layers within the bulk sample. 

We made use of that technique in order to further investigate the blistering of our coated silicon samples. Positive oxygen ions are very surface sensitive which we used to record surface images that show the blisters as a lack of surface material compared to a significant signal of bulk material which should not be visible for a uniformly coated sample. Depth profiles recorded with the help of the cesium ion gun revealed that the bulk material may have diffused into the surface coating during the TPD measurements which makes further discussions with the customer on how to prevent this process in the future indispensable.

Surface images taken with SIMS. On the left, the bulk material which is more intense within the blisters (lighter areas) is depicted. On the right, the image of the surface material shows a lack of surface material in the exact same areas.

My supervisors at Hiden chose an interesting and exciting research topic within an industrial environment and professional partnership for me. I appreciate to have learnt so much about the different quadrupole mass spectrometers, the TPD and SIMS experiments as well as Hiden’s corresponding TPD and SIMS Workstations. My time at Hiden provided me with insights into the work of a scientist in a manufacturing company and it was a great pleasure to work together with such an experienced team. 

If you want to know more about Hiden’s TPD or SIMS Workstations I worked on, check out these links:

TPD Workstation – https://www.hidenanalytical.com/products/for-catalysis-and-thermal-analysis/tpd-workstation/

SIMS Workstation – https://www.hidenanalytical.com/products/for-thin-films-plasma-and-surface-engineering/sims-workstation/

This blog post was written by ESR 13, Gabi Wenzel, who is currently pursuing her PhD in laboratory astrophysics at the Insitut de Recherche en Astrophysique et Planétologie and the University of Toulouse, France.

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