Scott Gilbert, left, and Todd Miller collaborated in developing this industrial micromixer. (Photo: Karl Maasdam)

Dime-sized mixers perform a critical step in high-value chemical operations including nanoparticle synthesis, precision blending and laboratory automation, but they can also add value to the broader chemical industry. Microflow CVO’s microfluidics architecture leverages integrated-circuit design concepts to create devices that can be scaled and designed to manufacturer specifications, said Todd Miller, prototyping manager at the MBI and president of the new firm. Miller said the company has licensed rights to patent applications he has made over the past five years while at OSU.

A market analysis by the OSU College of Business estimates the global micromixer (also called “microreactors”) market in the life sciences at $2 billion. “It’s a rapidly changing and growing market,” said John Turner, OSU instructor and CEO of Microflow CVO. He and OSU MBA student Ken True identified more than 1,000 researchers at 270 institutions in 30 countries using microreactors in pharmaceutical research. “We expect the market to exceed $3 billion by 2014. And that’s only in the life sciences. Other chemical manufacturing markets raise the potential for these products,” added Turner.

The problem that Microflow CVO has addressed seems simple: how to efficiently mix two liquids with consistently high-quality results. Manufacturers commonly perform this step in large vats where batches of liquids are stirred and then processed.

In contrast, microfluidic technologies push liquids through channels slightly larger than a human hair where mixing occurs under precisely controlled conditions. While the results can meet manufacturer specifications, existing micromixer designs tend to be fragile, expensive and hard to adapt to specific circumstances.

This micromixer made by OSU-spinoff company Microflow CVO combines liquids in the pharmaceutical, petrochemical and consumer products industries. (Photo: Karl Maasdam)

Compared to existing designs, Microflow CVO’s stainless steel microreactors, perform better, cost less and can be customized easily for existing processing operations, said Miller. “Currently, most users of micromixers are forced to adapt their processes to a discrete number of available designs,” added Norm Galvin, vice president of sales. “Microflow CVO’s mixers can be built to customer specifications. We adapt to our customer’s needs; they don’t have to adapt to ours.”

The company currently offers two products for sale and will expand its offerings to more than 15 by the end of the calendar year. The additional offerings will provide options in flow rates, fluid inputs and operational scale.

Microflow CVO began with a chance encounter at a Portland, Ore., meeting hosted by the Oregon Nanoscience and Microtechnologies Institute (ONAMI). Miller met Scott Gilbert, an expert in microfluidics then affiliated with the University of Washington. Gilbert was looking for a microfluidics device that could provide precision blending of modestly viscous fluids (such as anti-freeze) at a high flow rate but a low pressure drop. His target was the petrochemicals industry.

Years before, Miller had made prototypes of such devices, but further development was slowed as other duties and projects required his attention.  Gilbert’s question sent him back to the drawing board — in this case, computer modeling software — where he worked out the details. The prototype Miller built at the MBI exceeded mixture specifications without additional processing.

Since then, Miller has developed and tested other micromixers to produce copper nanoparticles, a collaborative effort with Gilbert, OSU chemistry professor Vincent Remcho and the Department of Energy’s Pacific Northwest National Laboratory. With proof-of-concept in hand, he applied for and received “gap funding” assistance through ONAMI, which supports efforts to commercialize technology originating from the Oregon University System. “ONAMI has been critical to this whole process,” said Miller. “Without ONAMI, we wouldn’t be here.”

Gilbert now serves as chemical safety officer and research associate at the MBI and is chief technology officer of Microflow CVO. Ormond “Norm” Galvin is vice president of sales for the company.

More information is available at http://www.microflowcvo.com.

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Based in Corvallis, Oregon, Microflow CVO designs innovative high-performance micromixers and microfluidic components that improve industrial processes, reduce waste and lower capital costs. The company maintains close ties to the Oregon State University Microproducts Breakthrough Institute and the Oregon Nanoscience and Microtechnologies Institute.

Editors note: Photos of the new Microflow CVO™ device and of Scott Gilbert and Todd Miller are available on Flickr:

http://www.flickr.com/photos/oregonstateuniversity/7158821648/

http://www.flickr.com/photos/oregonstateuniversity/7158820442/

Illustration by Marc Lehman, University Marketing

For researchers at Oregon State and Portland State, this black box is a microbial fuel cell, a renewable energy source that uses bacteria to convert biodegradable materials, like wastewater, into electricity. And the knobs in this scenario are connected to nanostructures, such as carbon nanotubes. Frank Chaplen and Hong Liu of OSU’s Department of Biological and Ecological Engineering and Jun Jiao of Portland State’s Department of Physics are using nanotubes to boost the power output of microbial fuel cells.

Some evidence in the scientific literature suggests that adding nanostructures to the surface of the fuel cell’s anodes, components on which the bacteria live, could improve the power output, but the researchers didn’t know how or why. Not only that, it’s difficult to control the properties of nanostructures, like width or density. With so many variables to work with, they were struggling to solve their problem in a reasonable amount of time.

This is where Alan and Xiaoli Fern come in. Chaplen asked the couple, who teach in OSU’s School of Electrical Engineering and Computer Science (EECS), to create a mathematical solution. In this case, Chaplen was looking for a mathematical algorithm, a procedure expressed as a set of rules, that would inform the researchers which of the myriad variables would be best to tackle first — in other words, which way to turn the knobs.

Alan Fern is an expert in automated planning and decision theory, which uses computing power to make intelligent decisions about sequential problems. His wife, Xiaoli, specializes in active machine learning, a discipline that aids in identifying the most useful data points for solving a problem.

And so, for the first time, although they have been together since graduate school, the Ferns’ academic interests converged, and they began working on the problem together.

“Traditional research has focused mostly on design problems that have clean, analytical solutions, which require many simplifying assumptions. We come at the problem from a different angle. We start with realistic, messy problems and design algorithms that solve them with raw computing power,” Alan Fern explains.

Mathematical Challenge

They saw the fuel cell project as an opportunity to make a difference, not only for microbial fuel cell research, but for experiments that are difficult to control. For example, in the fuel cell project, instead of requiring an exact density of the nanomaterial, their algorithm could account for a range of densities.

It was just the kind of math-oriented challenge that graduate student Javad Azimi was looking for when he joined the project as a research assistant, helping to design the algorithms and writing the software.

“I really love math, and I like working with real data. So when they told me about it, I said, ‘Yeah, let’s do it!’” Azimi says.

The team set to work on helping Chaplen and Liu find out which nanomaterials (such as gold, iron or carbon nanotubes) and what properties (such as length, width and density) would most likely produce the best power output.

“These statistical models try to capture the researcher’s uncertainty about regions they haven’t explored and take advantage of regions they have explored fairly thoroughly,” Alan Fern adds.

They also performed simulations that can be run repeatedly by a computer. The Ferns and Azimi used this type of modeling to inform decisions about the best experiment to run next and which experiments would be advantageous to run simultaneously, or as computer scientists say, in parallel. Answering such questions saved Chaplen, Liu and Jiao both money and time.

”These experiments are very time consuming, and the researchers can’t afford to run them sequentially, so they have to be in parallel, and we can help them figure out which experiments would complement each other in terms of the information they provide,” Xiaoli Fern adds.

More Electricity

Using this approach, the team was able to successfully identify nanomaterials that enhanced power production by 10 to 20 times. Their efforts were funded by a four-year grant from the Oregon Nanoscience and Microtechnologies Institute in collaboration with the U.S. Army Research Laboratory.

The Ferns and Azimi have also applied their work to data from a project examining hydrogen produced by cyanobacteria, another potential renewable energy source.

In the future, they expect to continue working with the microbial fuel cell team. In fact, they have already submitted another grant proposal, which would help Jiao advance the understanding of nanostructure properties. Nanotechnology has diverse applications in many areas including medicine, electronics and green energy production.

Azimi said that after presenting their research in papers and at conferences he has discovered that it could apply to areas that they hadn’t considered, such as improving the movement of robots.

“Because we are working to solve real problems with our algorithms, I believe the impact of our work will be really high,” says Azimi, who plans to continue this work for his dissertation.

“The concept is to use new, fundamental scientific advances to drive more efficient production and fabrication methods, use green materials and reduce environmental impacts,” says Douglas Keszler, center director and distinguished professor of chemistry at OSU. “The focus will be on electronics and related areas. This is cutting-edge science and technology, and it was born and bred here in Oregon.”

State investment in ONAMI, the Oregon Nanoscience and Microtechnologies Institute, has helped to pave the way for the new center which, if successful, could be in line for up to $25 million in federal funding over the next five years.

Dave Johnson, center co-director and Rosaria P. Haugland Foundation Chair in Pure and Applied Chemistry at the University of Oregon, says that state support for ONAMI was key. “ONAMI investments in facilities, increased ties to Oregon and regional industry, an ONAMI spin-out company and the intercampus collaborations were all key elements in putting together this winning proposal.”

“Among projects sponsored by the Oregon Nanoscience and Microtechnologies Institute, I believe this new center holds great potential for future growth in both the research enterprise and commercial entities,” says Skip Rung, ONAMI president and executive director.

Linsa Truong studies how gold nanoparticles behave in the body. (Photo: Nick Houtman)

Truong, who grew up in the Seattle area, wants to know how gold nanomaterials behave in the body. Through ONAMI’s Safer Nanomaterials and Nanomanufacturing Initiative, she is testing products from Professor Jim Hutchison’s University of Oregon lab, which has created “green” methods (highly efficient, precise and less toxic) for making gold nanomaterials.

“We actually know how they’re made every step of the way,” says Truong. Such information about manufacturing methods, chemical composition and purity is crucial for linking nanomaterial characteristics to the outcomes of tests in the OSU zebrafish lab.

Moreover, ONAMI provides Truong with direct access to information. “I can pick up the phone and ask questions about a nanomaterial I’m working with. I can ask how many ligands (a molecule that bonds with a metal) is on the surface of a nanomaterial, rather than have to look it up or wait online,” she says.

Truong’s desire for better health care is personal. As a child, she watched her grandparents struggle with heart problems. Diagnostic tests and treatments made them sick. “I didn’t want to be a doctor,” she says. “But I wanted to develop the technology that would help them.”

Lisa Truong is a Ph.D. student in the Department of Environmental and Molecular Toxicology.

In OSU’s micro- and nano-materials lab, Anna Putnam puts a printed layer of lithium iron phosphate precursor into a tube furnace, where it decomposes and forms nanosize gas bubbles. The result is a nanoporous material that is suitable for an electrode in small, lightweight batteries. (Photo: Karl Maasdam)

Undergrad Anna Putnam is squirming. The interviewer has touched a raw nerve in the chemical engineering major. “You’re digging deeply into my life,” she says, shifting in her chair. Her confession comes with reluctance: “My first term at OSU, I struggled in math.” Pressed, she admits the worst: “I got a C in vector calculus.”

For the University Honors College student who had breezed through Advanced Placement calculus and chemistry at Oregon’s Clackamas High School, a grade of “average” was a jarring wake-up call. “Before I got to the university,” the 2005 senior class valedictorian explains, “I never had to study very hard.”

In the three years since that rude awakening, nothing less than an A has darkened Putnam’s grade report. She has gone on to collect scholarships like most students collect songs on their iPods. The American Engineering Association Scholarship from Intel and OSU’s Presidential Scholarship are among them.

Now, Putnam has advanced from the front of the class to the front edge of innovation, where chemical engineering meets nanoscience and “drop-on-demand” printing technologies. As a research assistant for Professor Chih-hung “Alex” Chang, Putnam is fabricating a “nanostructured” electrode for a new generation of lithium ion battery. An initiative of ONAMI (Oregon Nanoscience and Microtechnologies Institute) in collaboration with Pacific Northwest National Labs (PNNL), the project’s ultimate goal is a revolutionary new battery: smaller, lighter, faster, tougher. The U.S. Army — eager to equip soldiers with more compact, lightweight, durable gear — is funding the research. And Hewlett-Packard, a leader in ink-jet design for novel applications in labs and factories, has donated a research-grade thermal printer to the effort.

The jumbled micro- and nano-materials lab in Graf Hall is Putnam’s base camp 20 hours a week. As comfortable with ultrasonicators (for breaking up particles) and vacuum furnaces (for superheating chemicals) as other people are with video players and microwave ovens, she has found a way to synthesize lithium iron phosphate, a compound with superior properties to the nickel cobalt or lithium cobalt used in most batteries today. Now, aided by the advanced electron microscopy capability at Portland State University (for viewing nanostructures) and the HP thermal printer (for creating imperceptibly thin layers of nano-materials called “thin films”), Putnam is taking the next step toward better batteries.

With financial backing from the OSU Research Office’s Undergraduate Research Innovation Scholarship Creativity grant, she will spend the summer of 2008 making nanoporous thin-film electrodes in various shapes and thicknesses on the HP printer.

Professor Chang describes Putnam as “devoted to the field of nanotechnology.” It was, in fact, one of Chang’s ONAMI colleagues, Jun Jiao of PSU, who serendipitously led Putnam to nanoscience. During Anna’s last summer in high school, she heard about Saturday Academy’s Apprenticeship in Science and Engineering from a friend. The Portland-based program aims to pull more girls and minorities into the sciences. Putnam didn’t know it then, but her career plans were about to morph. Her summer studying the conductivity of carbon nanotubes in Jiao’s lab “changed my life,” she reports. When the internship started, she wanted to be a K-12 teacher. When it ended, she was set on becoming an engineer.

Although prestigious private college Harvey Mudd dangled a hefty scholarship, the small California college’s status as one of the nation’s premier engineering schools couldn’t compete with the broad diversity of students and opportunities available through Oregon State. One of those opportunities came along the summer after her freshman year, when she studied nanotreatments for breast cancer in the lab of PSU chemist and ONAMI researcher Scott Reed.

“I designed my own experiments making porphyrins and gold nanoparticles and quenching them together,” she explains matter-of-factly.

A star in the College of Engineering’s K-12 outreach and mentoring program, Putnam wows high school girls with her “real and vibrant” personality, showing them that it’s “OK to love math and chemistry, and that it doesn’t make you a ‘geek’!” says her first-year adviser Professor Willie “Skip” Rochefort, who actively recruited Putnam to OSU.

As for that hated C in vector calculus, that intolerable stain on Putnam’s near-perfect GPA, soon it will be only a painful memory. She is retaking the class. When she applies for graduate work at MIT or Berkeley, she intends that nothing average will blot her resume, or her prospects.

• Alex Chang’s Web page
• College of Engineering
• ONAMI
• Pacific Northwest National Laboratory
• Hewlett-Packard
• The Campaign for OSU

OSU nanotechnology researchers are leveraging the power of molecular-scale processes to improve quality and create new products.

Nanotechnology has arrived. No longer do we just have to imagine the benefits. Advertisers tout them in cosmetics, clothing, batteries, dental adhesives, paint and golf clubs. In 2004, nanotech consultant Lux Research, Inc., estimated the worldwide sale of products containing nanomaterials at $158 billion. And new products are on the horizon: medicines, sensors, filters and more efficient solar collectors.

If you take a historical view, we’ve been driving to work on nanotechnology for the past century. About one-quarter of an automobile tire consists of nanosize-carbon black particles. Without them, our treads would lack strength and wear resistance.

“Nano” refers not just to small but to a specific kind of smallness. One nanometer is one-billionth of a meter, the width of a human hair sliced lengthwise into 100,000 strands. It takes 10 carbon atoms to span one nanometer. Lined up side by side, 152 million carbon atoms are as wide as a penny.

In 1959, Caltech physicist Richard Feynman issued a call to arms for research at this scale. He explained to a conference of his colleagues how all 24 volumes of the Encyclopaedia Britannica could fit on the head of a pin. Not only is there enough room among the atoms to encode that much information, he argued, “there is plenty of room,” enough for all the world’s books to be copied onto a mote of dust.

Among Feynman’s nanotech dreams were room-sized computers shrunk to the size of a briefcase (check that one off), ingestible surgical devices that could repair a damaged heart and factories that make flawless products, atom by atom.

Today, OSU researchers in engineering, chemistry, physics and wood science are among those putting Feynman’s ideas into practice. Through the Oregon Nanoscience and Microtechnologies Institute (ONAMI), they are working with colleagues at the University of Oregon, Portland State University, the Pacific Northwest National Laboratory and the private sector (HP, FEI, Intel, IBM and others) on projects designed to address manufacturing and safety issues as well as to develop new materials and products. Funding support comes from the State of Oregon and the federal government’s National Nanotechnology Initiative.

The Joke Among Chemists

Among scientists, this investment is both a welcome source of support and validation of existing ideas. “The joke among the chemists is, ‘have you heard about nanotechnology? It’s the new name for chemistry,’” says OSU physicist Janet Tate. “We’ve been doing nanotechnology for a long time in physics and chemistry. A lot of what we talk about when we teach quantum mechanics is inherently nano in scale.”

Tate grew up in South Africa, received her Ph.D. at Stanford and has won awards for her teaching and research since coming to OSU in 1989. A major focus has been OSU’s transparent electronics initiative, nanoscale research that demonstrated the world’s first transparent thin-film transistor in 2003 and integrated circuit in 2006.

“Transparent electronics is a new field, but it exploits old ideas,” says Tate. It all starts with semiconductors in which the flow of electricity can be easily manipulated. Most semiconductors, such as silicon-based materials in computers, cell phones and other electronic devices, are visible because they absorb light. However, some semiconductors let particles of visible light (photons) sail right through them untouched. Thus, they are as clear as glass.

The trick with invisible semiconductors (indium oxide, zinc oxide, tin oxide and others), adds Tate, is to find ways to make them conduct electricity without making them visible. In her research, she collaborates with Doug Keszler (Chemistry), John Wager (Electrical Engineering and Computer Science) and a team of technicians and students to make transparent semiconductor films that are tens of nanometers thick. By placing other molecules into the films, they hope to achieve the kind of control over the flow of electricity that is now possible with silicon-based semiconductors.

“You inevitably shift off into the fringes where things are not quite as transparent, and you discover that maybe it’s useful for something else like solar cells,” Tate adds.

Common as Wood

That kind of opportunity strikes a chord with John Simonsen, a chemist in OSU’s Wood Science and Engineering Department. After receiving his Ph.D. from the University of Colorado, he worked in the private sector before coming to OSU in 1990. He specialized in wood-plastic composites and wood preservatives. Strength is a problem with composites, he says, especially the bond between wood and synthetic polymers. “They just don’t have the mechanical properties at the cost that we expect for building materials. You have to go to exotic polymers to get strength. You’re talking dollars a pound. Wood costs a dime a pound.”

So he became intrigued when he began learning about the ability of nanosize-cellulose crystals to increase strength in composites. “Cellulose crystals are stronger than steel and stiffer than aluminum. And they’re renewable. That’s probably why nature uses them for trees,” he says.

Just as important for researchers, cellulose chemistry is well known, and, compared to many other nanoparticles, easy to work with. In his lab, Simonsen makes cellulose nanocrystals by grinding standard filter paper, then hydrolyzing it with acid. A simplified version of the process goes like this: Add acid, spin the solution in a centrifuge, then pass it through an ultrafilter to concentrate the cellulose and remove the impurities. The resulting liquid looks like watered-down milk. For show-and-tell, he keeps a vial of the cloudy liquid on his desk, telling visitors that the cellulose has remained suspended in solution for more than a year.

Simonsen uses the material in several areas of research: improving the performance of membranes, such as those in kidney dialysis filters; improving the properties of barrier films to keep out toxic industrial chemicals; and making novel materials by combining the nanocrystalline cellulose with other polymers.

Initial findings from a dialysis membrane study by Simonsen, Sundar Atre (Industrial and Manufacturing Engineering) and Sweda Noorani, a graduate student, showed that by adding only 2 percent cellulose to the membrane, they increased both stiffness and water vapor transport, a property that should foster the ability of the filter to cleanse the blood.

In addition to his research, Simonsen is working with OSU faculty members on a nanotechnology curriculum in the Materials Science Program. A Nanotechnology Processes Option is also available in Chemical Engineering.

Nanofactories

While new materials are driving product development, Brian Paul is putting his money on “nanomanufacturing,” the ability to economically structure matter on the nanometer scale. Paul received his Ph.D. from Penn State and is a professor in the OSU Department of Industrial and Manufacturing Engineering. He specializes in bulk microfluidics, a technology that uses channels no wider than a human hair to improve the quality of chemical reactions and heat transfer.

With this technology, close proximity is key; forced into tight quarters, chemicals react quickly and uniformly. Paul and his colleagues in OSU’s Microproducts Breakthrough Institute (MBI) have found ways to sequence systems of chemical mixers, separators and heat exchangers within microchannels. In MBI research, bulk microfluidic technology has already shown promise in making biodiesel and hydrogen and in filtering blood for kidney dialysis. These microsystems are tested in labs on campus and fabricated at the ONAMI Nano/Micro Fabrication Facility on the Hewlett-Packard campus.

But what makes Paul’s eyes really light up is the microchannel synthesis of nanomaterials, such as nanoparticles called “dendrimers.” Named for their tree-like branching structure, these spherical molecules have spacious interiors and functional exteriors that can be tailored to selectively attach to surfaces. They can carry an anti-cancer drug to a tumor or lock onto the HIV virus, thus making it incapable of infecting a human cell.

Trouble is, dendrimers may take weeks to months to manufacture, and they are priced accordingly, from hundreds to hundreds of thousands of dollars per gram. Using bulk microfluidics, Paul says his OSU colleagues Chih-hung Chang (Chemical Engineering) and Vince Remcho (Chemistry) are continuously producing multiple pounds per hour of dendrimer molecules using much less expensive capital equipment, significantly lowering the chemical cost. Moreover, the team can achieve a level of purity unmatched by industrial batch processing.

Arrays of microchannels can also address another concern that is not so nano, says Paul: safety. “Many nanoparticles are readily absorbed through the skin, and their health affects are not yet well understood. Do we really want a supply chain that is transporting them on the highways and rails? Better to transport reagents and produce the particles at the point of use to minimize exposure,” he says.

That would mean manufacturing nanoparticles in distributed reactors instead of centralized chemical plants. “What we’re talking about is distributed and portable production. We’re talking about a new paradigm, manufacturing models that blow away existing industrial scale models of production,” he adds. The challenge is finding ways to build cheap distributed systems to replace expensive centralized facilities.

With a $650,000 grant from the W. M. Keck Foundation, Paul, Chang and Remcho are studying microsystem-enabled dendrimer production, hoping to find new and efficient ways to apply it to a commercial scale.

“I come from a manufacturing mindset. You can’t wait months tying up expensive capital equipment and expect to make a difference. The objective is to deploy,” says Paul.

Other OSU researchers working on nanoscale projects include Greg Rorrer, Goran Jovanovic and Christine Kelly in chemical engineering. And ONAMI is bringing them together with counterparts at the University of Oregon’s Center for Advanced Materials Characterization in Oregon and Portland State University’s Center for Nanoscience and Nanotechnology. Their private-sector colleagues include Oregon-based FEI, Inc., a world leader in electron microscopy, which enables researchers to see at the nanometer scale and even below, into the spaces between subatomic particles.

Together, they are contributing to an economic sector that could be valued at between $1.4 trillion and $2.6 trillion by 2015, according to recent estimates by Lux Research and the National Science Foundation.