Specific Process Knowledge/Characterization/XRD: Difference between revisions

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We have two X-ray diffraction setups in building 346:
We have two X-ray diffraction setups in building 346:
*The [[/XRD_SmartLab|XRD SmartLab]] primarily for thin film analysis inside the cleanroom.
*The [[/XRD_SmartLab|XRD SmartLab]] primarily for thin film analysis inside the cleanroom.
*The [[/XRD SmartLab 9kW Rotating Anode|XRD SmartLab 9kW Rotating Anode]] multipurpose system outside the cleanroom.
*The [[/XRD_Powder|XRD Powder]] for phase analysis of powders outside the cleanroom.
*The [[/XRD_Powder|XRD Powder]] for phase analysis of powders outside the cleanroom.


==Experiments performed with XRD==
==Experiments performed with XRD==
*[[/Process Info|List and description of possible XRD measurements with typical setup requirements]]
*[[/Process Info|List and description of possible XRD measurements with typical setup requirements]] Note mostly relevant for XRD Smartlab


==Data analysis==
==Data analysis==
For data analysis, we recommend using Rigaku SmartLab Studio for both thinfilms and basic powder analysis.
For data analysis, we recommend using Rigaku SmartLab Studio for both thinfilms and basic powder analysis.
If more advanced powder analysis is needed a remote desktop with a licens for the Malvern Panalytical software, HighScore is available.
If more advanced powder analysis is needed we provide access to a remote desktop with a licence for the excellent Malvern Panalytical software, HighScore.


*[[/software|Installing SmartLab Studio II]]
*[[/software|Installing SmartLab Studio II]]
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*[[/SLSII_analysis|Guide for using SmartLab Studio II for data analysis]]
*[[/SLSII_analysis|Guide for using SmartLab Studio II for data analysis]]
*[[/HighScore_analysis|Guide for using HighScore Plus for advanced powder data analysis]]
*[[/HighScore_analysis|Guide for using HighScore Plus for advanced powder data analysis]]
Apart from this commercial software a wide range of free software is available online for data analysis. [https://xrd.mit.edu/xrd-software Here are some suggestions from MIT].


==Comparison of the XRDs at Nanolab==
==Comparison of the XRDs at Nanolab==
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!colspan="2" border="none" style="background:silver; color:black;" align="center"|Equipment  
!colspan="2" border="none" style="background:silver; color:black;" align="center"|Equipment  
|style="background:WhiteSmoke; color:black"|<b>XRD SmartLab</b>
|style="background:WhiteSmoke; color:black"|<b>XRD SmartLab</b>
|style="background:WhiteSmoke; color:black"|<b>XRD SmartLab 9kW Rotating Anode</b>
|style="background:WhiteSmoke; color:black"|<b>XRD Powder</b>
|style="background:WhiteSmoke; color:black"|<b>XRD Powder</b>
|-
|-
!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  
 
and thin film thickness measurement
|style="background:WhiteSmoke; color:black"|
*Phase ID
*Crystal Size
*Crystallinity
*Quality and degree of orientation
*3D orientation
*Latice strain
*Composition
*Twist
*3D lattice constant
*Thickness
*Roughness
*Density
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
*Phase ID
*Phase ID
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|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
3 kW
3 kW
|style="background:WhiteSmoke; color:black"|
9 kW
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
600 W
600 W
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|style="background:LightGrey; color:black"|
|style="background:LightGrey; color:black"|
Rated tube voltage
Rated tube voltage
|style="background:WhiteSmoke; color:black"|
20 to 45 kV
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
20 to 45 kV
20 to 45 kV
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|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
2 to 60 mA
2 to 60 mA
|style="background:WhiteSmoke; color:black"|
2 to 200 mA
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
15 mA
15 mA
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|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
Sealed tube
Sealed tube
|style="background:WhiteSmoke; color:black"|
Rotating Anode
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
Sealed tube
Sealed tube
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|style="background:LightGrey; color:black"|
|style="background:LightGrey; color:black"|
Target
Target
|style="background:WhiteSmoke; color:black"|
Cu
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
Cu
Cu
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|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
0.4 mm x 8 mm (Line/Point)
0.4 mm x 8 mm (Line/Point)
|style="background:WhiteSmoke; color:black"|
0.1-0.5 mm x 8 mm (Line/Point)
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
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
|style="background:WhiteSmoke; color:black"|
incident / receiver coupled or independent
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
incident / receiver coupled or independent
incident / receiver coupled or independent
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|style="background:LightGrey; color:black"|
|style="background:LightGrey; color:black"|
Goniomenter radius
Goniomenter radius
|style="background:WhiteSmoke; color:black"|
300 mm
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
300 mm
300 mm
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|style="background:LightGrey; color:black"|
|style="background:LightGrey; color:black"|
Minimum step size
Minimum step size
|style="background:WhiteSmoke; color:black"|
0.0001° (0.36")
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
0.0001° (0.36")
0.0001° (0.36")
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|style="background:LightGrey; color:black"|
|style="background:LightGrey; color:black"|
Sample stage motion
Sample stage motion
|style="background:WhiteSmoke; color:black"|
*&chi;:-5~+95°
*&phi;:0~360°
*Z:-4~+1 mm
*X,Y:&plusmn;50 mm for a 100 mm wafer
*Rx,Ry:-5~+5°
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
*&chi;:-5~+95°
*&chi;:-5~+95°
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|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
Fixed with rotation
Fixed with rotation
|-
 
|style="background:LightGrey; color:black"|
Sample size
|style="background:WhiteSmoke; color:black"|
Diameter: 150 mm
Thickness: 0~21 mm
|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
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*Cross Beam Optics(CBO)
*Cross Beam Optics(CBO)
*Ge(220)x2 monochromator
*Ge(220)x2 monochromator
*In-Plane Parallel Slit Collimator (PSC)
*Soller slit
*Automatic variable divergence slit
*Length limiting slits
|style="background:WhiteSmoke; color:black"|
*Cross Beam Optics(CBO)
*Ge(400)x2 monochromator
*In-Plane Parallel Slit Collimator (PSC)
*In-Plane Parallel Slit Collimator (PSC)
*Soller slit
*Soller slit
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*Parallel slit analysers (PSA)
*Parallel slit analysers (PSA)
*Ge(220)x2 analyser
*Ge(220)x2 analyser
|style="background:WhiteSmoke; color:black"|
*Automatic variable scattering slit
*Automatic variable receiver slit
*Parallel slit analysers (PSA)
*Ge(400)x2 analyser
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
*0.04° soller slit
*0.04° soller slit
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!style="background:silver; color:black" align="center" valign="center" rowspan="3"|Substrates
!style="background:silver; color:black" align="center" valign="center" rowspan="3"|Substrates
|style="background:LightGrey; color:black"|Measurement temperature
|style="background:LightGrey; color:black"|Measurement temperature
|style="background:WhiteSmoke; color:black"|
Room temperature
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
Room temperature
Room temperature
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|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
up to 150 mm wafers
up to 150 mm wafers
Thickness max 21 mm
|style="background:WhiteSmoke; color:black"|
up to 150 mm wafers
Thickness max 21 mm
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
Only for powders
Only for powders
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| style="background:LightGrey; color:black"|Allowed materials
| style="background:LightGrey; color:black"|Allowed materials
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
All materials approved in the cleanroom. No powders or dusty materials.
All materials approved in the cleanroom.  
 
No powders or dusty materials.
|style="background:WhiteSmoke; color:black"|
All materials have to be approved
|style="background:WhiteSmoke; color:black"|
|style="background:WhiteSmoke; color:black"|
All materials have to be approved
All materials have to be approved

Latest revision as of 18:09, 25 September 2024

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Unless otherwise stated, this page is written by DTU Nanolab internal


XRD at DTU Nanolab

We have two X-ray diffraction setups in building 346:

Experiments performed with XRD

Data analysis

For data analysis, we recommend using Rigaku SmartLab Studio for both thinfilms and basic powder analysis. If more advanced powder analysis is needed we provide access to a remote desktop with a licence for the excellent Malvern Panalytical software, HighScore.

Apart from this commercial software a wide range of free software is available online for data analysis. Here are some suggestions from MIT.

Comparison of the XRDs at Nanolab

Equipment XRD SmartLab XRD SmartLab 9kW Rotating Anode XRD Powder
Purpose Crystal structure analysis

and thin film thickness measurement

  • Phase ID
  • Crystal Size
  • Crystallinity
  • Quality and degree of orientation
  • 3D orientation
  • Latice strain
  • Composition
  • Twist
  • 3D lattice constant
  • Thickness
  • Roughness
  • Density
  • Phase ID
  • Crystal Size
  • Crystallinity
  • Quality and degree of orientation
  • 3D orientation
  • Latice strain
  • Composition
  • Twist
  • 3D lattice constant
  • Thickness
  • Roughness
  • Density
  • Phase ID
  • Crystal Size
  • Crystallinity
X-ray generator

Maximum rated output

3 kW

9 kW

600 W

Rated tube voltage

20 to 45 kV

20 to 45 kV

40 kV

Rated tube current

2 to 60 mA

2 to 200 mA

15 mA

Type

Sealed tube

Rotating Anode

Sealed tube

Target

Cu

Cu

Cu

Focus size

0.4 mm x 8 mm (Line/Point)

0.1-0.5 mm x 8 mm (Line/Point)

0.4 mm x 12 mm (Line)

Goniometer

Scanning mode

incident / receiver coupled or independent

incident / receiver coupled or independent

incident / receiver coupled

Goniomenter radius

300 mm

300 mm

145 mm

Minimum step size

0.0001° (0.36")

0.0001° (0.36")

0.001° (3.6")

Sample stage motion

  • χ:-5~+95°
  • φ:0~360°
  • Z:-4~+1 mm
  • X,Y:±50 mm for a 100 mm wafer
  • Rx,Ry:-5~+5°
  • χ:-5~+95°
  • φ:0~360°
  • Z:-4~+1 mm
  • X,Y:±50 mm for a 100 mm wafer
  • Rx,Ry:-5~+5°

Fixed with rotation

Optics Incident side
  • Cross Beam Optics(CBO)
  • Ge(220)x2 monochromator
  • In-Plane Parallel Slit Collimator (PSC)
  • Soller slit
  • Automatic variable divergence slit
  • Length limiting slits
  • Cross Beam Optics(CBO)
  • Ge(400)x2 monochromator
  • In-Plane Parallel Slit Collimator (PSC)
  • Soller slit
  • Automatic variable divergence slit
  • Length limiting slits
  • 0.04° soller slit
  • Ni and Cu filter
  • Divergence slits
  • Beam masks
Receiver side
  • Automatic variable scattering slit
  • Automatic variable receiver slit
  • Parallel slit analysers (PSA)
  • Ge(220)x2 analyser
  • Automatic variable scattering slit
  • Automatic variable receiver slit
  • Parallel slit analysers (PSA)
  • Ge(400)x2 analyser
  • 0.04° soller slit
  • Ni filter
Substrates Measurement temperature

Room temperature

Room temperature

May be heated in N2 up to 500°C

Substrate size

up to 150 mm wafers

Thickness max 21 mm

up to 150 mm wafers

Thickness max 21 mm

Only for powders

Allowed materials

All materials approved in the cleanroom.

No powders or dusty materials.

All materials have to be approved

All materials have to be approved