XRD Flourishes in a Broad Market

An X-ray diffraction (XRD) system transmits X-ray beams to a sample (generally a single crystal, metallic solid or a powder) and records the diffraction pattern that occurs when the X-ray photons encounter the inter-atomic gaps within the crystal structure. The results from the scattered photons are used to determine various properties of a sample, such as molecular composition, texture, phase and can even be used to find stress points within a material.

XRD systems are used in a variety of fields, ranging from mining to semiconductors to drug discovery. Such a diverse customer base partly accounts for the market’s growth. In addition, technical advances in XRD systems have increased the type of applications for which XRD is utilized, also contributing to its growth. These technical advances have led to a steady stream of products that have further stimulated demand.

There are two sectors of the XRD market that this article covers: single crystal XRD, which is used primarily for basic research and drug discovery, and powder diffraction XRD, which is principally used for industrial applications. Single crystal XRD has the more promising growth forecast, with sales estimated to grow in double digits in 2008. Academic research accounts for the majority of the single crystal XRD market and includes drug development. The pharmaceutical industry also employs single crystal XRD for drug development. The powder diffraction XRD market is growing steadily, with sales expected to increase more than 10% this year. Industrial applications for powder diffraction XRD include the analysis of environmental samples, metals analysis and materials identification.

Rigaku is the leading company in the XRD market. It provides both single crystal and powder diffraction XRD systems and has its strongest base in Japan. In June, the company established Rigaku Innovative Technologies Europe (RITE) in Prague, Czech Republic. “The new company in Europe not only enhances Rigaku’s optics and detector capabilities . . . but also provides a manufacturing base within Europe. By being now, at least in part, a European company, Rigaku—by virtue of proximity and unique capabilities—can more readily participate in cutting edge European scientific endeavors,” said Tom McNulty, vice president of Materials Analysis for Rigaku. According to Mr. McNulty, in addition to providing more access to private European customers, RITE also gives the company an opportunity to participate in European publicly funded activities.

In June, Rigaku introduced the RAPID II XRD system for small molecule applications using either single crystal or powder diffraction XRD. The RAPID II features Rigaku’s large-area curved imaging plate (IP) detector, which, according to Mr. McNulty, allows for “a range of 204° at a single-detector setting for maximum reciprocal space coverage and, by using extremely low noise and wide dynamic range IP technology, the RAPID II can collect a massive solid angle of very high quality data in a single exposure for superior productivity.” The IP detector is the backbone of the RAPID line. The principal technical advancement of the RAPID II is “the new Rigaku 2DP software, which further enhances productivity with project-based batch processing of two-dimensional XRD data,” he said. “This capability allows manipulation of multiple images at the same time with various analytical protocols.” The RAPID II is also now compatible with the MicroMax-007 HF generator, which can handle smaller or poorly diffracting crystals for structural biology applications.

Oxford Diffraction, which was acquired in April by Varian for more than $37 million (see IBO 4/15/08), provides single crystal XRD systems for both small molecule and macromolecular applications, but is more associated with macromolecular applications. For Varian, the acquisition provides a greater presence in the pharmaceutical market and the opportunity to grow the business through distribution. Varian can also package its NMR systems together with Oxford Diffraction’s XRD devices. “In chemistry, a high majority of crystallography users will also collect NMR data and likewise, most NMR users will also use crystallography,” said Paul Loeffen, CEO of Oxford Diffraction. “In protein structural biology, many crystallographers complement their investigations with NMR and vice versa. It is fairly frequently seen that NMR and crystallography instruments are purchased as a bundle for small molecule applications,” he stated.

Released in August, Varian’s Supernova XRD system for single crystal XRD employs X-ray micro-sources, and is the first commercial system to solely use X-ray micro-sources for beam generation, according to the company. “The new SuperNova system incorporates high-intensity microsource X-ray technology in a product designed for higher throughput,” said Mr. Loeffen. The intensity of the beam strength results in shorter exposure time, contributing to higher throughput. “The SuperNova targets high-throughput crystallography for pharmaceutical labs and structural genomics institutes,” he explained. The Supernova’s molybdenum micro-source is two-and-a-half times stronger than the molybdenum X-ray source of the Gemini, the company’s previous dual wavelength XRD system. Its copper micro-source is six times stronger than the Gemini’s copper X-ray source. This strength is due to the SuperNova’s use of a microfocus tube and multilayer X-ray optics, which together deliver a greater number of X-rays and better directs them.

Mr. Loeffen explained that the increases in detector speed and sensitivity, as well as system throughput and beam strength have expanded the company’s customer base. “The development of new technologies in X-ray imaging, such as the CCD detector, X-ray generation, and structure solution and refinement software have all opened up a very specialist area of research to a much wider and more general research community where application is useful.” He added, “the company’s primary customer base was built upon chemical crystallographers in academia. Over the last few years, the company has expanded to include industrial chemical research labs and protein crystallography labs in both academia and industry.” According to Mr. Loeffen, another effect of the new technology is that developing countries that are R&D intensive, such as China and India, have also quickly adopted XRD techniques.

Unlike Rigaku and Oxford Diffraction, PANalytical only offers powder diffraction XRD systems. The company’s XRD products primarily cater to industrial applications such as materials analysis and characterization for the cement, metals, steel, nanomaterials, plastics, petrochemicals and semiconductor industries. In fact, PANalytical claims it is the largest XRD provider for the thin film and polycrystalline materials market. Spectris, PANalytical’s parent company, stated in its half-year report that PANalytical’s growth was strong in the metals and mining industries and in R&D for the semiconductor industry. Growth has also been strong, according to the company, in emerging regions such as India and China due to an increase in the establishment of R&D centers by pharmaceutical manufacturers.

Targeting routine applications in the pharmaceuticals markets, rather than high-end research, in February, PANalytical launched the CubiX Walk-Up system, a fully automated, easy to use powder diffraction XRD system. Peter Munk, marketing manager of XRD systems at PANalytical, told IBO, “the Cubix Walk-Up is a system that was derived from our industrial line, from systems that were proven in many applications. It’s a tool that is completely aimed at the non-XRD expert user. It’s a system that’s very capable in a variety of applications and is finding use in many areas of the pharma industry.”

According to Mr. Munk, XRD for the pharmaceuticals industry is about 15%–20% of the company’s business. Within this market, the company serves a number of applications throughout drug development and manufacturing. Among the applications for powder XRD in pharmaceuticals, which includes the growing market for counterfeit drug detection, “the nondestructive nature of XRD makes it an ideal tool for systematic drug-excipient compatibility studies in preformulation. And it is also the perfect technique for monitoring the crystal morphology of active ingredients or the excipients and to optimize process parameters to ensure final product stability,” he stated. “It is ideally suited in production control for monitoring batch or dosage uniformity and the detection of polymorphic impurities.”

PANalytical’s offerings outside of the pharmaceutical industry are further evidence of the diversity of XRD’s market. “We are heavily involved in modern markets in thin film, especially in LED and photovoltaic cell development . . . an additional important activity is our industrial focus on process control and process monitoring in diverse industries [such as] cement, mining and aluminum for example,” explained Mr. Munk. He believes that compound semiconductors, solar energy and cement are growing industrial areas for PANalytical’s XRD business.

In the future, Mr. Munk believes yet another novel field, the commercialization of nanomaterials, will generate the most growth for XRD: “The whole nanotechnology market is a large area where, although XRD is already used extensively, we see significant growth potential in the future. For example, as soon as nanomaterials are used in areas such as thin films, coatings and self growing materials, the XRD market will grow again.”

Chart: XRD Total Market Value

2007 2008 2009

Total Market Value 424 480 540

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