# Presentation: 330420

## Sample Encapsulation Considerations In DesigningHigh Temperature Neutron Diffraction Experimentspresented at Sample Environment for Neutron Scattering ExperimentsSENSE WorkshopTallahassee, FL USASeptember 26, 2003byKenneth J. VolinIntense Pulsed Neutron SourceArgonne National Laboratory

**Sample Encapsulation Considerations In Designing****High Temperature Neutron Diffraction Experiments***presented at* **S**ample **E**nvironment for **N**eutron **S**cattering **E**xperimentsSENSE WorkshopTallahassee, FL USASeptember 26, 2003*by*Kenneth J. VolinIntense Pulsed Neutron SourceArgonne National Laboratory

**Notes:**
Kenneth J. Volin
Shared Services Manager
Intense Pulsed Neutron Source

Argonne National Laboratory
9700 South Cass Ave.
Argonne, IL 60439-4814

TEL	630-252-6092
FAX	630-252-4163
PAGE	630-722-3332
EMAIL	kjvolin@anl.gov

## Science Driven Sample Environments

**Sample environments serve the neutron scientist in two ways:**
**1) They mimic the harsh environment ****of the real world**
**2) They span the parameter range of ****applicable condensed matter theory**

- [Your Presentation Title]

## Science Pushing The Upper Limits of Temperature

**High Temperature Compound Synthesis **
- High Tc Superconductors
- Catalysts
**High Strength/High Temperature Materials**
- Nitride, Carbide, and Oxide Based Ceramics
- Intermetallic Superalloys
**Fast Ionic Conductors**
- Ca-stabilized ZrO2
**Geologically Relevant Molten Oxides**
- Molten Silica and Magnesium Silicate
**Molecular Dynamics and Monte Carlo Simulations**

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## The Sample Environments Are Available

**Cartridge Heater Furnaces****	****~500****°C**
**Vanadium Foil Furnaces****	****~1200****°C**
**Tantalum Ribbon Furnaces****	****~1450****°C**
**Halogen Lamp Furnaces****	****~1650°C**
**Laser Furnaces****	****>2800°C**

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**Notes:**
Furnace	Heat Source	TMAX [°C]
Coffee Can Furnace 	Cartridge Heaters	300°C		
Hot Stage Displex	Cartridge Heaters	528°C
Small Angle Furnace		900°C
Howe/LUCYFE Furnace	Vanadium Foil	1200°C
Single Xtal Furnace	Platinum Foil	1200°C
Miller I & II Furnces	Tantalum Ribbon	1450°C
Halogen Lamp Furnace	Halogen Lamp	1650°C
Laser Furnace	250W CW Laser	>2800°C

## But What To Hold The Sample?

**Ultimately – Nothing!**
** **
**As the science drives the required temperatures higher and higher, there are fewer and fewer refractory materials available with the proper combination of high temperature structural integrity and chemical compatibility.  Containerless schemes for measuring high temperature molten materials have been developed but cannot be used for all the diverse materials that the material scientist may want to study at high temperatures.**
** **

- Containerless Research Inc. (CRI)
- Evanston, IL

- [Your Presentation Title]

**Notes:**
Rick Webber
Containerless Research Inc. (CRI)
Envanston, IL

## Designing a High Temperature Neutron Experiment

**What is the temperature range that covers the science that your are interested in?**
**What high temperature sample environment equipment is available at the neutron source facility and is compatible with the instrument that the experiment will be run on?**
**What sample containers are available from the instrument or facility?  What other sample containers have been used in the past with the particular sample environment?**
**Are any of the above sample containers chemically compatible with your sample material?  If not, what can you do to contain your sample at temperature?**

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## Sample Encapsulation Considerations

**Choosing a containment material**
- Low Scattering Background
*Aluminum, Vanadium and Tantalum*
*Null-Alloys *
*Fused Silica, Sapphire, Vitreous Carbon*
- Good Physical Properties
*High Melting Point*
*Retention of Structural Properties*
- Chemical Compatibility with Sample Material at Temperature
*Knowledgeable resources*
*Published information either in scientific literature or reference material*
*Experimental results*

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**Notes:**
Refractory Metals: W(4310C), Ta(2996C), Mo(
> Does anyone have recommendations for null scattering
> alloys that can be easily machined for ambient temp
> and pressure neutron powder diffraction sample cans?
Lachlan M. D. Cranswick
Neutron Program for Materials Research (NPMR),
National Research Council (NRC),
Chalk River Laboratories, Chalk River, Ontario, Canada

## Sample Encapsulation Options

**Aluminum**
**Low coherent scattering length**
**High melting point: 625°C**
**Thin wall closed one end cans commercially available in a variety of diameters and wall thicknesses. **
**Pure aluminum [1100 series] bar stock commercially available in a variety of diameters and lengths**
**Can be easily worked using common machine shop tools**
**Can be e-beam or TIG welded to other metals forming flanges or end-caps**

- QENS Instrument
- ANL/IPNS Facility, Argonne, IL

- [Your Presentation Title]

## Sample Encapsulation Options

**Vanadium**
**Low coherent scattering length**
**Refractory Metal **
**High melting point: 1917°C**
**Thin wall closed one end cans commercially available in a variety of metric and SAE diameters**
**E-beam consolidated bar stock commercially available in a variety of diameters and lengths**
**Can be easily worked using common machine shop tools**
**Can be e-beam welded to other metals forming flanges or end-caps**

- Metal Technologies Inc., Albany, OR

- [Your Presentation Title]

**Notes:**
Metals Technology Inc.
(formerly BJ Scientific Inc.)
Albany, OR

## Sample Encapsulation Options

- Modified 316 Stainless Steel Swagelok Seal
- [3/8” diameter thin wall vanadium can]
- ANL/IPNS Facility, Argonne, IL

- [Your Presentation Title]

**Notes:**
A new sample cell for neutron scattering at high and low temperature 
S. Susman, Rev Sci Inst, 64(2), 1993. 

## Sample Encapsulation Options

**Titanium-Zirconium (TiZr)**
**Null alloy**
**High melting point: 3300°C**
**Commercially available from specialist foundries in billet form**
**Can be semi-easily worked using common machine shop tools**
**Can be e-beam welded to other metals forming flanges or end-caps**

- GLAD Instrument
- ANL/IPNS Facility, Argonne IL
- [RAL/ISIS Facility, Oxfordshire, UK]

- [Your Presentation Title]

## Sample Encapsulation Options

**Fused Silica or**
**Silicon Oxide [SiO****2****]**
**Low coherent scattering length**
**Chemically inert to most materials  **
**High melting point: 1425°C****Softening point: ~1200°C**
**Commercially available in rod, tube, plate forms **
**Easy to work into ampoule form and then to seal off under a low pressure of inert gas such as helium.  Can be worked into complex designed by a skilled glassblower.**

- GLAD Instrument
- ANL/IPNS Facility, Argonne, IL

- [Your Presentation Title]

## Sample Encapsulation Options

**Alumina or **
**Aluminum Oxide [Al****2****O****3****]**
**Chemically inert to most materials  **
**High melting point: 2054°C**
**Commercially available in rod, tube, plate forms and a range of purities**
**Difficult to machine but can be ground or ultrasonically milled by a skilled ceramics worker**
**Difficult to seal adequately**

- ILL Facility, Grenoble, FR
- ANL/IPNS Facility, Argonne, IL

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## The Chemical Compatibility Question

**Knowledgeable Resources**
- Chemistry Departments or Material Science Divisions
**Published Literature**
- Compound Synthesis
- Phase Diagrams
- Other high temperature measurements
**Experimental Results**
- Corrosion Tests
- Mass Loss	 Measurements

- http://web.met.kth.se/dct/pd/element/Al-V.html

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## Some Parting Thoughts

**The selection of a proper sample container for a high temperature neutron experiment is a compromise between the ideal neutron experiment, where the neutrons see nothing but the sample, and the ideal container, which holds but does not contaminate the sample material.  Often the compromise leans more towards the ideal container than the ideal neutron experiment.  The neutron scientist then must use his ingenuity in properly analyzing his data.**
**It is the responsibility of the experimenter, not the user facility, to ensure that the sample is safely contained throughout the experiment.**

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## Acknowledgments

**IPNS Neutron Operations Group**
*S. Short*
*R. Connatser*
*J. Siewenie*
**IPNS Sample Environment Group**
*J. Fieramosca – Group Leader*
*R. Como*
*J. Baldwin*
**IPNS Shared Services Group**
*D. Leach*
*R. Kleb*
- Argonne National Laboratory, a U.S. Department of Energy
- Office of Science laboratory, is operated by The University of Chicago under contract W-31-109-Eng-38.

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