N.L. Tran , J.Z. Sexton, T.J. Grassman, B. Fruhberger, A.C. Kummel

1
N.L. Tran , J.Z. Sexton, T.J. Grassman, B. Fruhberger, A.C. Kummel University of California, San Diego S.V. Patel, T.E. Mlsna Seacoast Science AFOSR MURI# F49620-02-1-0288 Test Chamber Mass Flow Control Temperature Controlled Enclosure Heat Exchanger Flow Meter Data Acquisition And Control PC 4-Way Valve Temperature Controlled Bubblers Carrier Gas Exhaust Goal Determination of Material Growth and Analyte Interaction Evaluation of Sensor Performance DFT Computation Phthalocyanine Deposition Current Capabilities: In Preparation: Develop Instruments to: (a) Fabricate Metallo-Phthalocyanine (MPC) Chemically Sensitive Field Effect Transistor (ChemFet) (b) Test MPC ChemFETs (c) Image Sensor Materials 1 3 2 E binding of Cl 2 using GGA-DFT Binding Site [eV] 1. -1.40 2. -1.05 3. -1.41 DFT simulations can aid in the assignment of observed STM features Computation suggest multiple possible binding sites for Cl 2 (Cu and the organic ligand) • Custom designed MBE cell for MPc deposition • MBE cell capabilities include: • fast introduction of different MPcs • differential pumping H 2 O cooled Cu heat shield to minimize heat transfer and protect UHV instrumentation • plate valve allowing separation between MBE cell and UHV chamber Low T effusion cell Linear & Linear/Rotary feedthroughs control plate valve Cu cooling shield braised onto SS can Two mounted tees to connect shafts to feedthroughs Two side ports for mounting turbo pump and ion gauge Effusion cell shutter Plate valve Cu spacers for heat transfer – also act as hard stops Linear feedthrough Cu plate Linear/rotary feedthrough Viton o-ring for sealing Closed to UHV Open to UHV And for depositi on Low Temperature STM for Single Molecule Studies: funded by NSF • Scanner: Beetle type with x-,y- coarse movement • Cooling: Liquid He bath cryostat; Scanner 100% surrounded by a 4K shield • Vibration isolation: Internal spring system with eddy current damping and external isolation with pneumatic isolation leg • Additional shutter to control in-situ gas dosing at low temperature onto STM mounted sample • Temperature variation either by heating the complete STM scanner or just the sample The Createc STM-SY-014-2 combines a low-temperature STM (LT-STM) with three chambers: load-lock, sample preparation, and analysis. High Resolution Images of Complex Molecules At Low Temperature due to Extremely Stable Environment Instrument Features: - Additional He gas cooled radiation shield in between to improve the thermal isolation - Eddy current vibration damping of the pendulum motion of the inner cryostat - STM is completely isolated (thermally and electrically) when tunneling (a) 8K STM image of TBPP (porphyrin) on Cu(100), (b) STM simulation of TBPP/Cu(100); (c) structure of TBPP on Cu(100). Note the excellent submolecular resolution at the good agreement with the simulation. From Moresco et al LHe dewar (4 l) shutter for sample & tip transfer radiation shields (LN 2 , LHe) eddy current damping for the LHe cryostat STM head He gas cooled radiation shield linear feedtrough 4” (to pull down the STM) rotary feedtrough (transfer shutter) electrical feedtroughs STM-contacts (37-pin plug) Cabling (stainless steel) baffles LN 2 dewar (14 l) • 50 electrical feedthroughs • Closed-loop temperature control: 0 - 100 ± 0.05° C; 20 minute response time • Closed-loop relative humidity control: 0 - 100% ± 2% RH; 10 minute response time • Open-loop permanent gas concentration control: 0 - 40000 ± 4 ppm; 4 minute response time; or, • Open-loop volatile organics concentration control: up to 8 volatile organics from temperature-controlled bubblers in any one experiment, 4 minute response time • Temperature and humidity sensors inside chamber • Outer enclosure with closed-loop temperature control: 25 ± 0.5°C • Test runs are fully automated Room temperature STM • Filled state image of CuPc on Au(111) at monolayer coverage • Metal center of adsorbed CuPc appears dark, consistent with unfilled Cu-dz 2 orbitals • Conditions: -1 V sample bias, 0.3 nA tunneling current 60 Å x 60 Å Future Plans Plate valve mechanics: Use STM to image growth modes and analyte binding sites for Metallo-Phthalocyanines Test sensors for ppb sensitivity and selectivity to Chemical Warfare Agent (CWA) simulants

description

Data Acquisition And Control PC. Mass Flow Control. Exhaust. Temperature Controlled Enclosure. Test Chamber. Heat Exchanger. Flow Meter. 4-Way Valve. Temperature Controlled Bubblers. Carrier Gas. 1. 2. 3. rotary feedtrough (transfer shutter). electrical feedtroughs. Cabling - PowerPoint PPT Presentation

Transcript of N.L. Tran , J.Z. Sexton, T.J. Grassman, B. Fruhberger, A.C. Kummel

Page 1: N.L. Tran , J.Z. Sexton, T.J. Grassman, B. Fruhberger, A.C. Kummel

N.L. Tran, J.Z. Sexton, T.J. Grassman, B. Fruhberger, A.C. Kummel

University of California, San DiegoS.V. Patel, T.E. Mlsna

Seacoast Science AFOSR MURI# F49620-02-1-0288

TestChamber

Mass Flow Control

Temperature ControlledEnclosure

HeatExchanger Flow

Meter

Data AcquisitionAnd Control PC

4-WayValve

TemperatureControlled BubblersCarrier

Gas

Exhaust

Goal Determination of Material Growth and Analyte Interaction

Evaluation of Sensor Performance

DFT Computation

Phthalocyanine Deposition

Current Capabilities:

In Preparation:

Develop Instruments to:

(a) Fabricate Metallo-Phthalocyanine (MPC) Chemically Sensitive Field Effect Transistor (ChemFet)

(b) Test MPC ChemFETs

(c) Image Sensor Materials

1

3

2

Ebinding of Cl2 using GGA-DFT

Binding Site [eV]1. -1.402. -1.053. -1.41

DFT simulations can aid in the assignment of observed STM features

Computation suggest multiple possible binding sites for Cl2 (Cu and the organic ligand)

• Custom designed MBE cell for MPc deposition

• MBE cell capabilities include:• fast introduction of different MPcs• differential pumping• H2O cooled Cu heat shield to minimize heat transfer and protect UHV instrumentation• plate valve allowing separation between MBE cell and UHV chamber

Low T effusion cell

Linear & Linear/Rotary feedthroughs control plate valve

Cu cooling shieldbraised onto SS

can

Two mounted tees to connect shafts to

feedthroughs

Two side ports for mounting turbo pump

and ion gauge

Effusion cell shutter

Plate valve

Cu spacers for heat transfer – also act as hard stops

Linear feedthrough

Cu plate

Linear/rotary feedthrough

Viton o-ring for sealing

Closedto UHV

Opento UHVAnd for

deposition

Low Temperature STM for Single Molecule Studies: funded by NSF

• Scanner: Beetle type with x-,y-coarse movement • Cooling: Liquid He bath cryostat; Scanner 100% surrounded by a 4K shield• Vibration isolation: Internal spring system with eddy current damping and external isolation with pneumatic isolation leg• Additional shutter to control in-situ gas dosing at low temperature onto STM mounted sample• Temperature variation either by heating the complete STM scanner or just the sample

The Createc STM-SY-014-2 combines a low-temperature STM (LT-STM) with three chambers: load-lock, sample preparation, and analysis.

High Resolution Images of Complex Molecules At Low Temperature due to Extremely Stable Environment

Instrument Features:

- Additional He gas cooled radiation shield inbetween to improve the thermal isolation

- Eddy current vibration damping of thependulum motion of the inner cryostat

- STM is completely isolated (thermally andelectrically) when tunneling

(a) 8K STM image of TBPP (porphyrin) on Cu(100), (b) STM simulation of TBPP/Cu(100); (c) structure of TBPP on Cu(100). Note the excellent submolecular resolution at the good agreement with the simulation. From Moresco et al

LHe dewar(4 l)

shutter for sample& tip transfer

radiation shields(LN2, LHe)

eddy current dampingfor the LHe cryostat

STM head

He gas cooledradiation shield

linear feedtrough 4”(to pull down the STM)

rotary feedtrough(transfer shutter)

electrical feedtroughs

STM-contacts(37-pin plug)

Cabling(stainless steel)

baffles

LN2 dewar(14 l)

• 50 electrical feedthroughs • Closed-loop temperature control: 0 - 100 ± 0.05° C; 20 minute response time • Closed-loop relative humidity control: 0 - 100% ± 2% RH; 10 minute response time • Open-loop permanent gas concentration control: 0 - 40000 ± 4 ppm; 4 minute response time; or,• Open-loop volatile organics concentration control: up to 8 volatile organics from temperature-controlled bubblers in any one experiment, 4 minute response time• Temperature and humidity sensors inside chamber • Outer enclosure with closed-loop temperature control: 25 ± 0.5°C • Test runs are fully automated

Room temperature STM• Filled state image of CuPc on Au(111) at monolayer coverage• Metal center of adsorbed CuPc appears dark, consistent with unfilled Cu-dz2 orbitals• Conditions: -1 V sample bias, 0.3 nA tunneling current

60 Å x 60 Å

Future Plans

Plate valve mechanics:

•Use STM to image growth modes and analyte binding sites for Metallo-Phthalocyanines•Test sensors for ppb sensitivity and selectivity to Chemical Warfare Agent (CWA) simulants