Powder XRD Core Facility

 
 

Next dates available


We will be turning the XRD on in the following weeks, if there are enough users interested. Please contact us expressing your interest, or for urgent cases.


6 - 10 June 2016

1 - 5 August 2016

5 - 9 September 2016

3 - 7 October 2016

7 - 11 November

5 - 9 December



Overview


The Power X-Ray Diffraction Core Facility was established in 2011 with funding from the FY 2011 – Core Facility Support Program of the OSU Vice President for Research Office to support materials research at OSU through a cost-effective and sustainable model.


Unfortunately  the equipment does not have additional support from the University for a maintenance contract - the facility is supposed to be supported by users through fees collected from all users. We strongly encourage users of the facility to request funds to maintain the instrument in their grant proposals. This is a fundamental technique for many fields of research on campus, but it will be difficult to keep the instrument operational without more support from the users or the administration.


Based on historical data on the usage of the instrument, we estimate the cost of maintenance and running the instrument at ~$ 75/h (see the usage report here). We hope that this cost will be reduced with time if the equipment does not present problems. After discussion with users, however, we decided that a rate of $50 per hour of equipment time is a good compromise, although it is not sufficient to cover the costs of major repairs.


We remind the users that the equipment has a high throughput and is automated - for most users a 5 min scan per sample is sufficient to obtain quality data for phase identification. Typically users do not require more than 1-2 h, except when analyzing a very large number of samples.The equipment is configured for efficient characterization of powder samples, equipped with a robot that can automatically load up to 90 samples, placed in up to 6 sample “towers” of 15 samples each (see photo below), for analysis.


We also emphasize that all funds collected as part of this instrument are deposited in a stores account for future repairs and maintenance.
















Equipment timeline


Sep. 2011 - Equipment installed and accepted.

Dec. 2011 – Lynxeye detector exhibited high background (high counts). Background decreased after equipment had been powered down for the holidays. Problem was not identified by Bruker.

Mar. 2012 – Lynxeye was not recognized by the system. Equipment had to be reinitialized.

Apr. 2012 – 1st preventive maintenance visit (included in equipment acquisition). Water and filter in chiller were changed. No problem detected.

Sep. 2012 – End of one year warranty. One year PM contract was purchased ($4,800).

Jun. 2013 – Lynxeye background is high again. It was determined that the background is reduced by leaving the Lynxeye detector off overnight, but the background increases slowly as the detector remains on. This was probably why the problem was not detected before, since the equipment has been used sparely. Measurement can be run, but detector must remain off overnight.

Jun. 2013 – 2nd preventive maintenance visit (included in the one-year PM contract). Problem in Lynxeye was verified, but nothing could be done. No other problem detected.

Jul. 2013 – Driver problem in secondary goniometer track (detector), causing measurement to be interrupted. Measurements are not possible.

Oct. 2013 - Preventive maintenance performed. LynxEye detector and detector goniometer were replaced. Instrument is operational again.

Jul. 2014 - Instrument presented several problems related to the robot and the sample lift.

Nov. 2014 - The instrument was repaired and it is operational again.


Equipment details


  1. Bruker D8-A25-ADVANCE (DAVINCI design)

  2. Vertical goniometer, Bragg-Brentano geometry (theta-theta arrangement)

  3. LYNXEYE detector (1-dimensional "compound silicon strip" detector)

  4. Cu-anode, long fine focus, 2.2 kW, ceramic insulation body. Focus size: 0.04 x 12 mm.

  5. Variable primary and secondary slits

  6. 90-position sample changer

  7. DIFFRAC.EVA software for X-ray powder diffraction data evaluation and presentation

  8. DIFFRACplus TOPAS graphics-based, non-linear least squares profile analysis program

  9. ICDD/PDF-2

  10. Sample holders: PMMA specimen holders with sample reception diameter 25mm (C79298A3244D82), PMMA back loading specimen holders (C79298A3244D88), and a few Si low background holders (C79298A3244B261). The sample holders available are indicated in red in this file.

  11. Corundum standard sample supplied by NIST (A13B77).


How much material is required?


  1. We have several (~100) PMMA specimen holders with sample reception diameter 25mm (C79298A3244D82). These hold ~0.7-0.9 cm3 of compacted material. For example, for table salt (2.16 g/cm3) we need 1.5-2 g of material.

  2. We have a smaller number of PMMA back loading specimen holders (C79298A3244D88), which hold less material, probably a half of the holder above.

  3. For very small amounts, we have a few Si low background holders (C79298A3244B261).

  4. Holders available are indicated in red in this file.

Users responsibilities


  1. Users are responsible for preparing their samples. In special circumstances, we can prepare the samples, but the technical assistance charge applies (see below).

  2. Users are responsible for cleaning up the sample holders and leave them ready for the next users.

  3. Users are responsible for taking note of the measurement sequences and measurement conditions.

  4. Very important: Users are responsible for the overall scientific quality of the data and experiments. We make the equipment available for users in many areas and we cannot be responsible for misinterpretation of the data or misuse of the technique. Calibration data obtained in standard conditions using a Corundum standard sample supplied by NIST (A13B77) will be made available every session.


How to schedule equipment time: Please contact the facility manager listed on top of the page. (Use of the computer dedicated to data analysis is free and does not require scheduling.)


Fees:


OSU users: $ 50/h (equipment time)

Other academic users: $ 75/h (equipment time)

Industry: $ 100/h (equipment time)

Technical assistance (1h minimum): $ 50/h


Manuals: All equipment and software manuals can be made available to users in a Dropbox folder. Please e-mail me if you would like access to those.


Notes


  1. First time users must take 1-2h of training (see fee above).

  2. We have EVA and TOPAS installed in a computer dedicated to data analysis, which can be used anytime free of charge and with no need to schedule.

  3. Fees may change depending on maintenance needs.


Radiation Safety Requirements

  1. All users must have OSU’s Radiation Safety Training, badge and ring dosimeter, otherwise data should be acquired by the facility technical person.


Recommended references

  1. B. D. Cullity and S. R. Stock. “Elements of X-ray Diffraction”. Prentice Hall.

  2. R. E. Dinnebier and S. J. L. Billinge (Editors). “Powder Diffraction: Theory and Practice”. RSC Publishing.


Useful links

  1. Bruker website: http://www.bruker-axs.com/d8_advance.html

  2. List of other facilities available at OSU: http://research.okstate.edu/index.php/research-centers

  3. OSU Microscopy Laboratory: http://microscopy.okstate.edu/


Principal Investigators in 2011 Core Facility Proposal

  1. Allen Apblett (Chemistry)

  2. Don A. Lucca (Mechanical and Aerospace Engineering)

  3. Donghua Zhou (Physics)

  4. Eduardo G. Yukihara (Physics)

  5. Jay Gregg (Geology)

  6. Jim Puckette (Geology)

  7. Regina DeWitt (Physics)

  8. Sandip Harimkar (Mechanical and Aerospace Engineering)

  9. Tyler Ley (Civil and Environmental Engineering)

  10. Yu (Jessie) Mao (Biosystems and Agricultural Engineering)

Funding

Location

OSU Labs at Venture I

Oklahoma Technology and Research Park

1110 S. Innovation Way Dr.

  1. (405)744-1111

See map


To schedule time, contact:

eduardo.yukihara@okstate.edu


Fee summary (see more below)

OSU: $ 50/h equipment + $50/h for 1h technical assistance