Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si...

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Cornell X-ray Experiment Details

Transcript of Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si...

Page 1: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

Cornell X-ray Experiment Details

Page 2: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

Unload the chamber

Page 3: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

Source holder in detail Front view

Backside view, Connections

Sb

K

Cs

Picture was taken before the change, sources are from previous run, Sb bead was used already.

Page 4: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

Chamber inside in detail

QCM, directly attached on sample holder, no water cooling

Movable anode, also served as source blocker

Sample holder

RF graphene evaporator

Page 5: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

Chamber inside in detail

RF graphene evaporator

Page 6: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

Source exchange

Sb sources wired on copper pins and inserted in to holes to be fixed on the holder.

K, Cs sources, clamped at both sides and bended to insert into the holder

The two holes, made of macor tubes

Page 7: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

Source company- Cs, K Phase diagram (Bi-Cs)

Alkali and alkali earth metals form many stable, high melting intermetallic compounds with nontoxic metals (bismuth).

s

http://www.alvatec.com/products/

Page 8: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

GISAXS: Grazing Incidence Small Angle X-ray Scattering XRR: X-ray Reflectivity

GIXRD: Grazing Incidence X-ray Diffraction

In XRR scan, incidence angle (αi) = exit angle (αf), scan range: 0 - 4o In GISAXS and GIXRD, αi =1.8o, fringes due to x-ray scattering was recorded.

X-ray Techniques used for Bi-alkali Photocathode Study

Experiment performed at: NSLS X21 (BNL) & CHESS G3 (Cornell)

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Page 9: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

CHESS Cathode Growth Process (Yo-Yo)

9 Silicon Substrate (p-type)

Sb (5 nm) (150 oC)

K (15 nm) (150 oC)

Cs (100 nm) (150 oC)

Sb (5 nm) (150 oC)

K (50 nm) (150 oC)

Silicon Substrate (p-type)

Sb (5 nm) (25 oC)

K (16 nm) (150 oC)

Cs (6 nm) (150 oC)

Sb (6 nm) (25 oC)

K (53 nm) (150 oC)

Cs (26 nm) (150 oC)

Sb (3 nm) (25 oC)

B33 Glass Substrate

Sb (5 nm) (25 oC)

K (16 nm) (150 oC)

Cs (6 nm) (150 oC)

Sb (6 nm) (25 oC)

K (53 nm) (150 oC)

Cs (26 nm) (150 oC)

Sb (3 nm) (25 oC)

Cathode 2 Cathode 3 Cathode 1

Sb, K, Cs deposited at 150 oC Sb deposited at Room Temperature, K & Cs at 150 oC

* All thicknesses are from QCM estimation, the K,

Cs deposition thicknesses are determined by QE

Page 10: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

Cathode 1: K-Sb deposition on Si substrate

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X-ray reflectivity Electron density profile

αi (degree)

I (a.

u.)

Thickness (Å)

ρ p

rofi

le (

Å-3

)

0 0.5 1 1.5 2 2.5 3 3.5 410

-7

10-6

10-5

10-4

10-3

10-2

10-1

100

101

Inte

nsity (

a.u

.)

Angle (deg)

-30 -20 -10 0 10 20 30 40 50 60 700

0.2

0.4

0.6

0.8

1

1.2

1.4

depth (A)

ele

ctr

on d

ensity (

A-3

)

0 0.5 1 1.5 2 2.5 310

-7

10-6

10-5

10-4

10-3

10-2

10-1

100

101

Inte

nsity (

a.u

.)

Angle (deg)

-50 0 50 100 150 200 2500

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

depth (A)

ele

ctr

on d

ensity (

A-3

)

Silicon Substrate (p-type)

Sb (5 nm) (150 oC)

Silicon Substrate (p-type)

Sb (5 nm) (150 oC)

K (15 nm) (150 oC)

Uniform KxSb on Si

Page 11: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

0 0.5 1 1.5 2 2.5 310

-7

10-6

10-5

10-4

10-3

10-2

10-1

100

101

Inte

nsity (

a.u

.)

Angle (deg)-50 0 50 100 150 200 250 3000

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

depth (A)

ele

ctr

on d

ensity (

A-3

)0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8

10-7

10-6

10-5

10-4

10-3

10-2

10-1

100

Inte

nsity (

a.u

.)

Angle (deg)

-100 0 100 200 300 400 500 600 7000

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

depth (A)ele

ctr

on d

ensity (

A-3

)

Cathode 1: K-Sb deposition on Si substrate (continued)

X-ray reflectivity Electron density profile

αi (degree) Thickness (Å)

Uniform KxSb on Si

I (a.

u.)

ρ p

rofi

le (

Å-3

)

Silicon Substrate (p-type)

Sb (5 nm) (150 oC)

K (15 nm) (150 oC)

Sb (5 nm) (150 oC)

Silicon Substrate (p-type)

Sb (5 nm) (150 oC)

K (15 nm) (150 oC)

Sb (5 nm) (150 oC)

K (50 nm) (150 oC)

Uniform KxSb? Sb also diffuses in to the compound?

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Page 12: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

Cathode 2: K-Sb deposition on Si substrate

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0 0.5 1 1.5 2 2.5 310

-6

10-4

10-2

100

102

104

Inte

nsity (

a.u

.)

Angle (deg)

-60 -40 -20 0 20 40 600

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

depth (A)

ele

ctr

on d

ensity (

A-3

)

0 0.5 1 1.5 2 2.5 3 3.5 410

-6

10-4

10-2

100

102

104

Inte

nsity (

a.u

.)

Angle (deg)

-50 0 50 1000

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

depth (A)

ele

ctr

on d

ensity (

A-3

)

0 0.5 1 1.5 2 2.5 3 3.5 410

-6

10-4

10-2

100

102

104

Inte

nsity (

a.u

.)

Angle (deg)

-50 0 50 100 1500

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

depth (A)

ele

ctr

on d

ensity (

A-3

)

X-ray reflectivity Electron density profile

αi (degree) I (

a.u

.)

Thickness (Å)

ρ p

rofi

le (

Å-3

)

Silicon Substrate (p-type)

Silicon Substrate (p-type)

Sb (5 nm) (25 oC)

Silicon Substrate (p-type)

Sb (5 nm) (25 oC)

K (16 nm) (150 oC)

Uniform KxSb on Si

Page 13: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

0 0.5 1 1.5 2 2.5 310

-7

10-6

10-5

10-4

10-3

10-2

10-1

100

101

Inte

nsity (

a.u

.)

Angle (deg)

-50 0 50 100 150 200 2500

0.2

0.4

0.6

0.8

1

1.2

1.4

depth (A)

ele

ctr

on d

ensity (

A-3

)

Cathode 2: K-Sb deposition on Si substrate (continued)

X-ray reflectivity Electron density profile

αi (degree) Thickness (Å)

I (a.

u.)

ρ p

rofi

le (

Å-3

)

Silicon Substrate (p-type)

Sb (5 nm) (25 oC)

K (16 nm) (150 oC)

Sb (6 nm) (25 oC)

Silicon Substrate (p-type)

Sb (5 nm) (25 oC)

K (16 nm) (150 oC)

Sb (6 nm) (25 oC)

K (53 nm) (150 oC)

0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 210

-6

10-5

10-4

10-3

10-2

10-1

100

Inte

nsity (

a.u

.)

Angle (deg)

-100 0 100 200 300 400 500 6000

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

depth (A)

ele

ctr

on d

ensity (

A-3

)

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Page 14: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

-60 -40 -20 0 20 40 600

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

depth (A)

ele

ctr

on d

ensity (

A-3

)

0 0.5 1 1.5 2 2.5 310

-6

10-4

10-2

100

102

104

Inte

nsity (

a.u

.)

Angle (deg)

Cathode 3: K-Sb deposition on B33 glass substrate

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X-ray reflectivity Electron density profile

αi (degree) I (

a.u

.)

Thickness (Å)

ρ p

rofi

le (

Å-3

)

0 0.5 1 1.5 2 2.5 3 3.5 410

-6

10-4

10-2

100

102

104

Inte

nsity (

a.u

.)

Angle (deg)

-60 -40 -20 0 20 40 60 80 1000

0.2

0.4

0.6

0.8

1

1.2

1.4

1.6

depth (A)

ele

ctr

on d

ensity (

A-3

)

0 0.5 1 1.5 2 2.5 3 3.5 410

-6

10-4

10-2

100

102

104

Inte

nsity (

a.u

.)

Angle (deg)

-100 -50 0 50 100 150 2000

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

depth (A)

ele

ctr

on d

ensity (

A-3

)

Uniform KxSb on glass

B33 glass Substrate (p-type)

B33 glass Substrate

Sb (5 nm) (25 oC)

B33 glass Substrate

Sb (5 nm) (25 oC)

K (16 nm) (150 oC)

Page 15: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

0 0.5 1 1.5 2 2.5 310

-7

10-6

10-5

10-4

10-3

10-2

10-1

100

101

Inte

nsity (

a.u

.)

Angle (deg)

-100 -50 0 50 100 150 200 2500

0.2

0.4

0.6

0.8

1

1.2

1.4

depth (A)

ele

ctr

on d

ensity (

A-3

)

Cathode 3: K-Sb deposition on glass substrate (continued)

X-ray reflectivity Electron density profile

αi (degree) Thickness (Å)

I (a.

u.)

ρ p

rofi

le (

Å-3

)

B33 glass Substrate

Sb (5 nm) (25 oC)

K (16 nm) (150 oC)

Sb (6 nm) (25 oC)

B33 glass Substrate

Sb (5 nm) (25 oC)

K (16 nm) (150 oC)

Sb (6 nm) (25 oC)

K (53 nm) (150 oC)

0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.810

-5

10-4

10-3

10-2

10-1

100

101

Inte

nsity (

a.u

.)

Angle (deg)

-100 0 100 200 300 400 500 6000

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

depth (A)

ele

ctr

on d

ensity (

A-3

)

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Page 16: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

XRR Preliminary Results (continue updating)

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Sb, K, Cs deposited at 150 oC Sb deposited at Room Temperature, K & Cs at 150 oC

Silicon Silicon Glass

Thickness (Å) Roughness (Å) Thickness (Å) Roughness (Å) Thickness (Å) Roughness (Å)

Substrate - 4.04±0.67 - 4.84±0.02 - 4.94±0.02

Sb on Substrate 49.76±0.22 1.90±0.12 50.53±0.21 3.37±0.03 52. 39±0.28 3.40±0.03

K-Sb on Substrate 163.73±0.78 4.83±0.11 110.41±0.41 3.67±0.04 116.55±0.56 3.80±0.03

Sb-K-Sb on Substrate

225.08±0.59 4.60±0.09 165.47±0.53 4.11±0.09 175.97±0.77 4.21±0.08

K-Sb-K-Sb on Substrate

544.18±1.16 7.63±0.06 543.13±2.25 5.17±0.15 530.66±2.33 2.82±0.35

Cs-K-Sb-K-Sb on Substrate

Sb-Cs-K-Sb-K-Sb on Substrate

- -

Cs-Sb-Cs-K-Sb-K-Sb on Substrate

- -

Page 17: Cornell X-ray Experiment Details - University of Chicago...Cathode 1: K-Sb deposition on Si substrate (continued) X-ray reflectivity Electron density profile α i (degree) Thickness

XRR Preliminary Summary

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All the simulation is based on one homogeneous Sb or KxSb layer code. Similar thickness and roughness indicates the growth of K-Sb/substrate on Si and glass may follow the same growth mechanism. During first KxSb deposition, cathode 1 has thicker KXSb film than cathode 2 and 3; at the end, cathode 1 has the same KXSb film thickness as cathode 2 and 3. They have the same thickness Sb deposition, the final thickness seems to be determined solely by Sb thickness. Uniform electron density profile indicates the formation of pure alkali antimonide (KxSb) compound. The absolute electron density value may be not very accurate. Further understanding and optimization of the code is under going. Electron density value is strongly determined by the accuracy of the critical angle. In the future, the alignment may be addressed. Electron density of bulk K (19e) is 0.26/A3, Electron density of bulk Sb (51e) is 1.69 /A3, electron density of bulk Si (14e) is 0.70/A3, it is possible that the KxSb (with rich K) electron density is lower than Si. XRR roughness is different from AFM roughness. During XRR experiment in our experiment, the 2-cm long surface was covered with X-ray at small angle.