Nanoprobe endstation

The Development of Hard X-ray Nanoprobe

by Montel Mirrors

Gung-Chian Yin 9/12/2014 at NSRRC 20th users’ meeting

Workshop IV

41A Soft RIXS

23A Nano-probe

25A Coherent Scattering

09A Temporally Coherent XRD

45A Submicron soft X-ray

21A Submicron XRD

24A Soft X-ray tomography

05A Protein Microrystallography

TPS

24-cell DBA

ID: 12m X 6, 7 m X 18

Plan of phase-I TPS Beamline

3

X-ray Nanoprobe at TPS

Beyond Si CMOS, Beyond Moore’s and More

Energy range：4 - 15 keV

Photon flux：1010 ~1011 photons/sec

Energy resolution：< 2×10-4 with Si(111) crystals

Beam size： ~ 40 nm at 10 keV (H × V, FWHM)

High-order harmonic contamination：≦1 × 10-3

Energy scanning capabilities.

Vacuum close to 10-7 torr

Adapted to 2 inch /standard Omicron holder

•Nano-electronics

•Fast speed logics

•Mass storage

•Optoelectronic

macromolecules (also

photo-voltaics)

•Energy

•Quantum computing

•Uniqueness of the research

activities

X-ray Methods

Beyond sub-ten-nm resolution (coherent)

With tens-nm resolution (incoherent)

• nano-XRF (x-ray fluorescence) – Element-specific nano-imaging

• nano-XAFS (x-ray absorption fine structures) – Local electronic structure – Local chemical environments – Element-specific, averaged over nano-area

• nano-XEOL (x-ray excited optical luminescence)

– X-ray-to-visible down-conversion efficiency in nano phosphor • nano-PXM (projection x-ray microscopy)

– Absorption and phase contrast x-ray images

• nano-CXDI (coherent x-ray diffraction imaging) • Bragg-ptychography

– strain dynamics in nano-devices

Other than X-rays

•SEM (SE, EDS, CL with high resolution) •Fly scanning •Nanomotors (optional) •Sample environment (optional)

XNP at TPS

Ee (GeV) IU22

3

Photon energy (keV) HP 3.52-20

VP

Ring current (A) 0.5

Period length, λ(mm) 22

Number of period, Nperiod 140

Peak field, By (T) 1.05

Peak field, Bx (T)

Deflection parameter, Kymax 2.15

Deflection parameter, Kxmax 0.00

Total magnetic length, L (m) 3.1

Minimum magnet gap (mm) 5

0 5 10 15 20 2510

17

1018

1019

1020

1021

IU22

22 mm, L = 3 m,

Kmax

= 2.15 with gap 5 mm

Bril

lian

ce (

ph

s/s/

mr2

/mm

2/0

.1%

bw

)

Photon Energy (keV)

0 5 10 15 20 2510

12

1013

1014

1015

1016

IU22

22 mm, L = 3 m,

Kmax

= 2.15 with gap 5 mm

Flu

x (

ph

/s/0

.1%

bw

)

Photon Energy (keV)

IU22 Insertion Devices（Gap of 5mm）

Source size

Horizontal source size :

282 μm (FWHM) @ 10 KeV

Vertical source size:

12.5μm (FWHM) @ 10 kev

Source divergence

Horizontal source divergence :

46 μrad (FWHM) @ 10 KeV

Vertical source divergence:

24 μrad (FWHM ) @ 10 KeV

Nano-Focusing optics K-B Mirrors Zone Plate Refractive Lens Montel KB

Mirror Chromatic dependence low-pass 1/λ 1/λ2 low-pass

Flux delivery high medium Energy depend high

Energy range critical angle limited < 12 keV up to hundreds of keV critical angle limited

Focal size 20 nm-1000 nm 20 nm-300 nm 50nm-1000 nm 20 nm-1000 nm

Theoretical limit < 10 nm, limited by NA < 10 nm ~ 5 nm Montel KB has larger

NA than normal KB.

Geometry reflective in-line in-line reflective

Diffraction Application ideal for polychromatic

and monochromatic

micro/nano- diffraction

limited access to

reciprocal space

for high energy

applications

Fluorescent analysis high flux using KB

multilayer

High resolution, low

cost, easy operation high flux using KB

multilayer

Imaging Application ok highest resolution; Proposed

Spectroscopy allowing large and

rapid energy changes

need to move the

zoneplate

(need fine alignment)

allowing large and

rapid energy changes

1. Focus beam 2. Only one mirror reflection

3. No cross

Illustration of the Montel KB Mirror

3

2 Vm only

2 Hm only

1

Focus length = 11 cm

Mirror length = 11 cm

Slope error < 0.05 μrad

Objective distance is 69 m

Incident angle =4 mrad

With Rh coating

Montel optics (nested KB)

Minimum radius

for this mirror: 20 m

40nm

5.656 mrad

4.0 mrad

Simulation of Focus Spot & divergence Simulation at 10 keV, average reflection=0.802, by ray tracing

Effective Source size 12.5 μm x 12.5 μm

Source divergence 6μrad x 6μrad

FHWM 32nm x 32nm,

Simulated

Focus spot size

Simulated

Divergence

Montel Mirrors holder/aligner

Axis name Travel Range

Resolution

(minimum

movement)

Stability

1 X 10 mm 0.1um 10 nm*

2 Y 24 mm 0.1um 1um

3 Z 10 mm 0.1um 10 nm*

4 Pitch 40 mrad 0.01 urad 0.1urad*

5 Roll 40 mrad 0.1 urad 0.1urad*

6 Yaw 40 mard 0.01 urad 0.1urad*

7 Top-Y 1mm 1 um 1um

8 Top-Z 1mm 1 um 10 nm*

9 Top-Pitch (X) 1mrad 0.05 urad 0.1urad*

10 Top-Roll (Y) 1mrad 1 urad 0.1urad*

Top-4 axis (for Alignment of Montel Mirror)

Bottom-6 axis (for total mirror set)

* Holder design has not finished yet-

Prototype of the Montel Mirrors

September 2013 at JTEC

Substrate of prototype of 7cm Montel mirrors.

12

283 μm (FWHM)

Optical Scheme of KB mirror focusing

L4 = 69 m

object

Horizontal direction

s h

0.5l/ s v

L1 = 27 m

L2 = 33 m

s h

HFM1

L5 =0.11 m

d=6.25 μm

6 μrad/90μrad

261μm

12.5μm × 110/ 69000 = 20.0nm

~12.5μm (FWHM) object

Vertical direction

Double Crystal Monochromator

s v 0.5l/ s v

L1 = 69 m

6 μrad/24μrad

L2 =0.11 m

261μm 12.5μm × 110 / 69000 = 20.0nm

Demagnification Ratio:

627

Demagnification Ratio:

Stage 1: 4.5

Stage 2: -0.5

(re-define the source)

Stage 3: 627

L3 = 66 m

Slit3

Beamline 2-stage focusing

Horizontal DCM

Short in length ( <70 m )

Windowless

Vertically coherent

Montel optics

Ultimate focal spot ~ 30-40 nm

photon flux 1010-1011/sec

Shih-Hung Chang

From user’s requirements

Targeting pressure: <10-6 torr

Temp. : 10k~ 873k (Red not implement low temperature yet)

Sample Size: 1cm2~ “2” wafer

Spot Size:<40nm

Sample perpetration: Heater ~873K

(degas/decap)

Use with 2” portable sample transfer

Conceptual layout for the X-ray nanoprobe

IU22

Focusing Optics

Bragg-Ptychography

/Diffraction

SEM

Fluorescence

SS1

Preparation Chamber

Projection CCD

XEOL

Laser interferometer

The current design of the endstation 1. KB mirror 2. Sample Stage 3. Laser interferometer 4. XEOL 5. SEM 6. XRF(EDS) 7. Sample Preparation system 8. Portable sample transfer 9. Projection CCD 10. Diffraction detector 11. (system is in vacuum)

1

2

3

4 5

6

7

8

9

10

xray

Design of mirror holder and sample stage

Montel KB mirror XFR

Flexure stage,XYZ

3 axis-Rotation stage

SEM

Piezo-stage, XYZ

Laser interferometer

Beam direction

The design with nanomotor

The consideration of Preparation Chamber

Portable chamber To transfer from MBE system

Switch to standard sample holder Heating stage, Surface clean, Ion gun, e gun.

To main Chamber

Switch from 2-inch To standard omicron holder

Endstation Schedule

Beamline ready

2014 2015 2016 2017

Finish test chamber Main chamber

& support design

user requirement

KB mirror & holder

Main chamber fabrication

Stage design

CCD Detector

Optical table, support

Procurement of stage

Stage test

Air conditions

In-situ system (optional)

Test of Montel KB

Procurement of Pilatus diffraction detector

Software development

Electronics& interferometer system development

Diffraction detector

holder design

Procurement of holder

Now Commissioning

Project Leader: Prof. J. Raynien Kwo (郭瑞年教授)

Construction Team

Leader

Mau-Tsu Tang (湯茂竹)

Beamline-

Shih-Hung Chang (張世汯)and Beamline Group

Endstation-

Gung-Chian Yin*,(殷廣鈐) optical design and overall system integration.

Bo-Yi Chen(陳伯毅) Mechanical engineer.

Chian-Yao Lee, (李建佑) Electronic engineer.

Huang-Yeh Chen (陳皇曄) Mechanical design and exeperiment.

Shao-Chin Tseng (曾紹欽) Sample preparation, experiment design.

Bi-Shuan Lin (林碧軒) Experiment design, XEOL, diffraction.

Shao-Yun Wu (吳紹筠) Experiment design, Diffraction

Construction Team

Progress of Testing Chamber

Vacuum:

After baking <10-7 torr

Operation at low 10-6 torr

SEM:

x100,000 (OK)

EDS:

Vortex me4 test (OK)

Interferometer: test OK

Temperature control:+- 0.02 C

Test Chamber

SEM

Turbo pump

SE Vortex ME4 detector

Granite base for

sample and mirror stages

Hi-Wedge mount

Cast iron frame

for chamber

Testing Chamber in progress

Flexure stage

Y Axis

Z Axis

SEM

EDS

SE

Turbo Pump

Laser Interferometer

Laser Path & Sample Stage

In details

Testing of integrated SEM

x10000

x50,000 x100,000

x31

Thank you for your attention !!!

The MBE system from user

Advanced Nano Epitaxy Lab, ITRI

Portable UHV

chamber for

transfer 2”wafers

in 3x10-10 torr for

X-ray and STM

analysis

Standard 2’’ wafer

Transported by

portable chamber

Consideration of diffraction Diffraction: By S2D2 method: Most of the Bragg angle Position can be found at 10 keV.

70 deg

45 deg

Si (5.431 Å )

Gamma delta

(002) 26.392 0

(004) 54.333 0

(202) 27.955 26.35

(204) 57.750

26.186

(224)

62.03 36.992

gamma

delta

J.Appl.Crystl(1995)28,318

29

List of Detectors

Type of experiment Detector Possible Brand

Fluorescence Multi-elements detectors (SDD/ Maia)

Vortex me4.

XEOL Spectrum Princeton instrument /Andor

•CDI/Bragg-ptychography CCD / photon counting area detector

Pilatus3 1M

Projection Microscope CCD Princeton instrument XO series

How Image is formed

Laser interferometer

Sample stage

address

signal

EDS/readout circuit test

Customize IO

Mercury-4

Customize IO test – 4k MCA @Ag

• Vortex Me4 is tested, and customized circuit is designed and tested. The circuit to

combine the signal and interferometer is finished and wait the real signal for

optimization. Bellow, slider and electrical isolation are finished.

• Vortex Me4 will be installed into the vacuum system soon.

Interferometer will also be installed soon.

2014 2015 2016

01 02 03 04 05 06 07 08 09 10 11 12 01 02 03 04 05 06 07 08 09 10 11 12 01 02 03 04 05 06 07 08 09 10 11 12

Hutch with utility

DCM with LN2

Mirrors

Mirror chambers

Vacuum components

Beamline components

Interlock system

Control system

Installation, sub-system

commissioning and

integration

Beamline commissioning

Design Prchase Utility Construction - - Hutch Temp.

Control

Specification Purchase Installation manufacture

Specification Purchase Installation manufacture

Specification Purchase Installation manufacture

Purchase

Leak Check Purchase Purchase Leak Check

manufacture

manufacture manufacture Installation

Design Purchase

manufacture Installation

Design manufacture

Installation Purchase

Commissioning

Installation, sub-system commissioning

and integration

Beamline Construction Schedule

33

Source size

3.52 - 20 keV

Horizontal source size :

282 μm (FWHM) @ 10 KeV

Vertical source size:

13μm (FWHM) @ 10 kev

Source divergence

3.52 - 20 keV

Horizontal source divergence :

46 μrad (FWHM) @ 10 KeV

Vertical source divergence:

24 μrad (FWHM ) @ 10 KeV

278

280

282

284

286

0 5 10 15 20 25

12

13

14

15

16

So

urc

e si

ze (

m)

Photon Energy (keV)

Horizontcal, FWHM

Vertical, FWHM

40

44

48

52

0 5 10 15 20 25

15

20

25

30

35

So

urc

e an

gu

lar

div

erg

ence

(

rad

)Photon Energy (keV)

Horizontcal, FWHM

Vertical, FWHM

IU22 Source Size and Divergence（Gap of 5mm）

34

X-ray Methods With tens-nm resolution (incoherent)

•nano-XRF (x-ray fluorescence)

•Element-specific nanoimaging

•nano-XAFS (x-ray absorption fine structures)

•Local electronic structure

•Local chemical environments

•Element-specific, averaged over nanozied area

•nano-XEOL (x-ray excited optical luminescence)

•X-ray-to-visible down-conversion efficiency in nano phosphor

•nano-PXM (projection x-ray microscopy)

•Absorption and phase contrast x-ray images

•nano-CXDI (coherent x-ray diffraction imaging)

•Bragg-ptychograpgy •strain dynamics in nanodevices

Beyond sub-ten-nm resolution (coherent)

35

Estimation of the Data Rate

Type of experiment Maximum data rate (Bytes/second)

Explain

Fluorescence 8M Bytes/sec 1ms per pixel, 4096 channels with multi-element detector. 16 bits for each channel.

X-ray absorption 20 KBytes/sec 0.1ms per pixel 1 channel 16 bits for each pixel

•CDI/Bragg-ptychography 100M Bytes/sec

0.1 s per frame 2048x2048 16 bits for each pixel

Projection Microscope 100M Bytes/sec 20ms per frame @ 1024x1024 pixel number 16 bits for each pixel

1.+-0.01K archived at control point 1.Air cool fan

No addition vibration observed

The temperature control

The consideration of XEOL

Scheme of the X-ray nanoprobe instruments

IU22

Focusing optics

Bragg-ptychography

Fluorescence

Detector

Projection CCD Sample

SEM

Laser interferometer

Sample Preparation Chamber

XEOL

39

Simulation of Beam Size

2 4 6 8 10 12 14 16 18 20

20

30

40

50

60

70

80

90

100

Foca

l sp

ot

(nm

)( F

WH

M)

Energy (keV)

diffraction-limit

geometrical

slope error = 0 rad

slope error = 0.05 rad

slope error = 0.10 rad

Diffraction limit

ε = 0.8895 λq/D

ε：resolvable image size

λ ：wave length

q：image distance

D：projection of reflective surface on z-axis

40

Flux estimation of different focusing optics

4 5 6 7 8 9 10 11 12 13 14 1510

8

109

1010

1011

1012

1013

1014

1015

1016

1017

Source(ph/s/0.1w)

HFM 0.7 m, Zone plate

K-B Mirrors

HFM 0.7 m, Nested K-B mirrors

F

lux

(P

ho

ton

s/se

c)

Photon Energy (keV)

Pitch of 2nd

crystal-flexure

coupling

Coarse motion

Fine motion

Range

Resolution

Repeatability

Drive

Range

Resolution

Repeatability

Drive

± 1°

< 2 μrad

< 5 μrad

In-vacuum stepping motor,

encoded

300 μrad

< 0.01 μrad

< 0.05 μrad

In-vacuum piezo

Perpendicular translate of 2nd

crystal

Range

Resolution

Repeatability

Drive

10 mm

< 0.5 μm

< 1 μm

In-vacuum stepping motor,

encoded

Angular stability

Drift

< 0.05 μrad

< 0.1 μrad/5hr

Bragg angle

Roll for

1st crystal

pitch

Roll for

2nd crystal

Perpendicular

Translation

Motion Parameter Specification

Bragg angle (i.e. rotation of

the crystal cage)

Range

Resolution

Repeatability

Eccentricity

Wobble

Speed

-1° to 35° (Feasible range)

6.3 ° to 34.4° (Operational)

< 1 μrad (full-step mode)

< 1 μrad

3 μm

10 μrad

0.5 °/sec

Horizontal translation (of the

whole assembly)

Note: will also provide pitch and roll

alignment for the whole DCM

assembly via independent motion of

the jacks

Range

Resolution

Repeatability

Drive

± 5 mm

< 10 μm

< 10 μm

Possibly manual; otherwise 3 -

4 stepping motors (jacks)

preferably encoded

Roll of 1st crystal-flexure

coupling

Range

Resolution

Repeatability

Drive

± 1°

< 2 μrad

< 5 μrad

In-vacuum stepping motor,

encoded

Roll of 2nd

crystal-flexure

coupling

Range

Resolution

Repeatability

Drive

± 1°

< 2 μrad

< 5 μrad

In-vacuum stepping motor,

encoded

Design Parameters of DCM

Crystal : Si (111)