Specific Process Knowledge/Characterization/XRD/XRD Powder: Difference between revisions

From LabAdviser
Reet (talk | contribs)
mNo edit summary
Reet (talk | contribs)
 
(11 intermediate revisions by 2 users not shown)
Line 1: Line 1:
'''Feedback to this page''': '''[mailto:labadviser@nanolab.dtu.dk?Subject=Feed%20back%20from%20page%20http://labadviser.nanolab.dtu.dk/index.php/Specific_Process_Knowledge/Characterization/XRD/XRD_Powder click here]'''
'''Feedback to this page''': '''[mailto:labadviser@nanolab.dtu.dk?Subject=Feed%20back%20from%20page%20http://labadviser.nanolab.dtu.dk/index.php/Specific_Process_Knowledge/Characterization/XRD/XRD_Powder click here]'''
<i> Unless otherwise stated, this page is written by <b>DTU Nanolab internal</b><br>
All images and photos on this page belongs to <b>DTU Nanolab</b></i>


=The XRD Powder setup=
=The XRD Powder setup=
[[Image:machine front with on-off button.JPG|right|thumb|300px|The XRD Powder located in the basement of building 346 at Nanolab, Room 904.]]
[[Image:machine front with on-off button.JPG|right|thumb|300px|The XRD Powder located in the basement of building 346 at Nanolab, Room 904.]]
The "XRD powder" is an Aeris Research edition benchtop X-ray diffractometer from Malvern Panalytical. It is meant for phase analysis of powders, is easy to use, and offers the option of making measurements while heating the sample in a N<sub><sub>2</sub></sub> atmosphere. The setup allows X-ray diffraction measurements in Bragg-Brentano mode (i.e., Theta-2Theta measurements where the incident and diffraction arms of the goniometer are coupled). We have a very limited selection of optics for this instrument, so there is little that the user can adjust.
The "XRD powder" is an Aeris Research edition benchtop X-ray diffractometer from Malvern Panalytical. It is meant for phase analysis of powders, is easy to use, and offers the option of making measurements while heating the sample in a N<sub><sub>2</sub></sub> atmosphere. The setup allows X-ray diffraction measurements with a Cu source in Bragg-Brentano mode (i.e., Theta-2Theta measurements where the incident and diffraction arms of the goniometer are coupled). We have a very limited selection of optics for this instrument, so there is little that the user can adjust.
The instrument has a 1D strip detector, which makes data acquisition very efficient, so you can measure your samples relatively quickly. The detector also has a fluorescence suppression option, so you can measure samples containing  for instance iron with the copper radiation.


Please contact the equipment responsible if you would like to mount the special sample holder for heating during the measurement.  
Please contact the equipment responsible if you would like to mount the special sample holder for heating during the measurement.  
Line 9: Line 13:
'''The user manual(s), user APV(s), technical information, and contact information can be found in LabManager:'''  
'''The user manual(s), user APV(s), technical information, and contact information can be found in LabManager:'''  


[http://labmanager.dtu.dk/function.php?module=Machine&view=view&mach=463 XRD Powder in LabManager]
[http://labmanager.dtu.dk/function.php?module=Machine&view=view&mach=463 XRD Powder in LabManager] - requires login




==Process information==
==Process information==


*A detailed manual on the Aeris XRD is found on the [https://wiki.iodp.tamu.edu/display/LMUG/Aeris+Advanced+User+Guide| wiki of the International Ocean Discovery Project].
*Tips for choosing among the scan and hardware parameters including fluorescence suppression: [[/Measurement tips| XRD Powder measurement tips]]
 
Malvern Panalytical has a large collection of webinars on XRD. You have to register to view them but the amount of email you receive afterwards is modest, so it's worth it in my opinion (Rebecca, July 2022). Some useful webinars include:


*[https://www.malvernpanalytical.com/en/learn/events-and-training/webinars/W20200604XRD.html| Better XRD data quality with good sample preparation]
*Malvern Panalytical has a large collection of webinars on XRD. You have to register to view them but the amount of email you receive afterwards is modest, so it's worth it in my opinion (Rebecca, July 2022). Some useful webinars include:
**[https://www.malvernpanalytical.com/en/learn/events-and-training/webinars/W20200604XRD.html Better XRD data quality with good sample preparation]
*A [https://www.malvernpanalytical.com/en/learn/events-and-training/webinars/W20210330XRD.html| beginner’s tutorial] which also mentions sample preparation about half-way through and explains very briefly some of the issues that can arise from displaced samples, not having a thick enough sample layer, odd sized sample particles, etc.
**A [https://www.malvernpanalytical.com/en/learn/events-and-training/webinars/W20210330XRD.html beginner’s tutorial] which also mentions sample preparation about half-way through and explains very briefly some of the issues that can arise from displaced samples, not having a thick enough sample layer, odd sized sample particles, etc.
   
   
===Software===
===Software===
Line 33: Line 35:
|-
|-
!style="background:silver; color:black;" align="center" width="60"|Purpose  
!style="background:silver; color:black;" align="center" width="60"|Purpose  
|style="background:LightGrey; color:black"| Crystal structure analysis and thin film thickness measurement
|style="background:LightGrey; color:black"| Crystal structure analysis
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
*Phase ID
*Phase ID
Line 70: Line 72:
0.4 mm x 12 mm (Line)
0.4 mm x 12 mm (Line)
|-
|-
!style="background:silver; color:black" align="center" valign="center" rowspan="5"|Goniometer
!style="background:silver; color:black" align="center" valign="center" rowspan="4"|Goniometer
|style="background:LightGrey; color:black"|
|style="background:LightGrey; color:black"|
Scanning mode
Scanning mode
Line 91: Line 93:
Fixed with rotation
Fixed with rotation
|-
|-
|style="background:LightGrey; color:black"|
 
Sample size
|style="background:WhiteSmoke; color:black"|
Powders
|-
!style="background:silver; color:black" align="center" valign="center" rowspan="2"|Optics
!style="background:silver; color:black" align="center" valign="center" rowspan="2"|Optics
|style="background:LightGrey; color:black"|Incident side
|style="background:LightGrey; color:black"|Incident side

Latest revision as of 15:59, 13 May 2024

Feedback to this page: click here

Unless otherwise stated, this page is written by DTU Nanolab internal
All images and photos on this page belongs to DTU Nanolab

The XRD Powder setup

The XRD Powder located in the basement of building 346 at Nanolab, Room 904.

The "XRD powder" is an Aeris Research edition benchtop X-ray diffractometer from Malvern Panalytical. It is meant for phase analysis of powders, is easy to use, and offers the option of making measurements while heating the sample in a N2 atmosphere. The setup allows X-ray diffraction measurements with a Cu source in Bragg-Brentano mode (i.e., Theta-2Theta measurements where the incident and diffraction arms of the goniometer are coupled). We have a very limited selection of optics for this instrument, so there is little that the user can adjust. The instrument has a 1D strip detector, which makes data acquisition very efficient, so you can measure your samples relatively quickly. The detector also has a fluorescence suppression option, so you can measure samples containing for instance iron with the copper radiation.

Please contact the equipment responsible if you would like to mount the special sample holder for heating during the measurement.

The user manual(s), user APV(s), technical information, and contact information can be found in LabManager:

XRD Powder in LabManager - requires login


Process information

  • Malvern Panalytical has a large collection of webinars on XRD. You have to register to view them but the amount of email you receive afterwards is modest, so it's worth it in my opinion (Rebecca, July 2022). Some useful webinars include:

Software

To adjust measurement parameters and analyze the data, you will need dedicated software which is described here: XRD Powder software

Equipment performance and process related parameters

Equipment XRD Powder
Purpose Crystal structure analysis
  • Phase ID
  • Crystal Size
  • Crystallinity
X-ray generator

Maximum rated output

600 W

Rated tube voltage

40 kV

Rated tube current

15 mA

Type

Sealed tube

Target

Cu

Focus size

0.4 mm x 12 mm (Line)

Goniometer

Scanning mode

incident / receiver coupled

Goniomenter radius

145 mm

Minimum step size

0.001° (3.6")

Sample stage

Fixed with rotation

Optics Incident side
  • 0.04° soller slit
  • Ni and Cu filter
  • Divergence slits
  • Beam mask
Receiver side
  • 0.04° soller slit
  • Ni filter
Substrates Measurement temperature

May be heated in N2 up to 500 °C

Substrate size

Only for powders

Allowed materials

All materials have to be approved