Gas Adsorption Controll Systems (WP 21.4)

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1 Gas Adsorption Controll Systems (WP 21.4) WP Adsorption Isotherm Sample Preparation System - OF-Adsorption-Insert (1.5K - 600K, 300bar) with sample cells - Cyogenfree Sorption System (50K 600K, 50bar) with sample cells - Automated Gas-dosing System (500K, 300bar) with dynamic flow option WP Gravimetric Measurement System 9/9/ NMI3 1

2 WP 21.4 Gas Adsorpion Systems WP REMOTE CONTROLLED GAS ADSORPTION SYSTEMS Cryo-Furnace Inserts Temperature Environment Closed Cycle Systems (stand alone) Gas Handling Volumetric Gas Dosing Capillaries/Tubes Flow Option WP GRAVIMETRIC MEASUREMENT SYSTEM Suspension Balance Vapour Mixing Cryostat 9/9/ NMI3 2

3 In-situ gas adsorption measurements Orange cryostat CO 2 Gas handling Gas-capillary Amount of Absorbed Gas N Sorption Isotherm Pressure P Neutron beam Sample container Neutron Intensity Small Angle Neutron scattering Pressure P Momentum Transfer Q

4 WP REMOTE CONTROLLED GAS ADSORPTION SYSTEMS Temperature Environment 1.5K 600K, p < 300 bar Cryo-Furnace Inserts (Samplestick) Gas circulator (magnetic coupled) Adjustable 900+/-20 mm 2 capillaries (3mm) for gas circulation Sample Themometer (Gardner Denver GK-M 02) System pressure: 150 bar Pressure difference: 75 mbar Gas flow: 2.5 L/min Capillary heating necessary from 77K to 295K!

5 Aluminium (AW 7075) Sample Cells Tensile Strength: 450 MPa at 295K Sealing: 1mm In- or Pb- wire da (mm) 300 K 400 K 500 K 600K bar 100 bar 10 bar 1 bar bar 200 bar 50 bar 20 bar bar 300 bar 300 bar 300 bar

6 In-situ stress-strain-analysis 296K da = 12 mm, p = 100bar 340K 420K

7 WP REMOTE CONTROLLED GAS ADSORPTION SYSTEMS Accessories for Air Protected Sample Preparation Sample-Stick sluice in Helium Glovebox Cell Locking Device Seals: In, Pb, Cu Pre-Seal: Rubber

8 Temperature Environment 1.5K 600K, p < 300 bar Closed Cycle Systems crygen free no cold spot Pulse Tube 55K.. 350K Gifford McMahon 6K.. 600K

9 WP REMOTE CONTROLLED GAS ADSORPTION SYSTEMS Temperature Environment 1.5K 600K, p < 300 bar Closed Cycle Systems (Mini Pulse Tube Cooler) 2 optinal capillaries floating shield and copper link 400 mm

10 High Temperatures ARS-Saphire Adapter (600K) for Gifford McMahon Redisigned 800K-Adapter for Pulse Tube System

11 WP REMOTE CONTROLLED GAS ADSORPTION SYSTEMS Gashandling System 300 bar, 500 K Volumetric Gas Dosing Pump PV4 PV15 PV3 MV1 EV1 PV7 20% 0% NV1 MV2 350 ccm MV3 350 ccm PV12 EV2 MV4 NV2 PV2 PV6 PV8 PV9 PV11 PV13 Gas 1 Gas 2 PV1 PV5 PV10 PV14 Sample T = 60.1 C SP = 60.0 C MV5 MV6 MV7 MV8 MV9 MV10 PG1 PG

12 Temperature dependend calibration of pressure gauches finished Software for automized Adsorption measurements is under construction

13 WP Gravimetric Measurement System Magnetic Suspension Balance for Neutron Scattering Measuring Position Zero Point Position balance CAL Balance CAL magnetic coupling gas inlet Measuring Position Electromagnet Permanent Manget Position Sensor Zero Point Position sample position Load Decoupling gas outlet Sample 1-10 µg accuracy of weighing under extreme conditions 9/9/ NMI3 13

14 Sample Repositioning for non powder samples Membrane Diffraktometer V1 at HZB Sample has to be in fixed Zero Position when the balance is rotating, e.g. in a rocking scan! Sample has to come back in reproduceable beam position after lifting and weighing!

15 Adapter for Humidity Control by Saturated Salt Solutions T=20 C 1.0bar 6.3 sample weigth (g) humidity (

16 Thanks for your attention and to my Coworkers Nico Grimm (Engineer) Mario Bochnia (Technician)

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