Inficon RQCM - Quartz Crystal Microbalance Research System Manuel d'utilisateur

OPERATION AND SERVICE MANUALResearch Quartz Crystal MicrobalancePN 603800 Rev.KRQCM

v3.5 ADJUSTING CAPACITANCE CANCELLATION TRIMMER & SWITCH... 3-5 3.5.1 AS A GENERAL RULE...

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE REFERENCES 12-2

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE REFERENCES 12-3

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE REFERENCES 12-4

vi 5.3 THICKNESS CALCULATION ... 5-3 5.4 LIQUID MEASU

viiTable of Figures FIGURE 1 CRYSTAL FACE MATING CONNECTOR ...

viii List of Tables TABLE 5-1 MATERIAL DENSITY AND ACOUSTIC IMPEDANCE VALUE... 5-4 TABLE 7-1 D

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE GENERAL DESCRIPTION 1-11 GENERAL DESCRIPTION The RQCM is designed for many types of research applications

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE GENERAL DESCRIPTION 1-2 1.1.4 MULTIPLE CRYSTAL MEASUREMENT CHANNELS The RQCM can be configured to measure

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE GENERAL DESCRIPTION 1-31.2 SPECIFICATIONS 1.2.1 CRYSTAL MEASUREMENT Crystal measurement channels: One

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE GENERAL DESCRIPTION 1-4 1.2.2.2 Thermocouple Input Type: Type “T” thermocouple Temperature range: 0 to 37

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE GENERAL DESCRIPTION 1-51.3 ACCESSORIES Part Number Description 172205 CHT-100 Crystal Holder, Teflon®, SM

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE GETTING STARTED 2-12 GETTING STARTED 2.1 UNPACKING Your RQCM was released to the carrier in good condition

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE GETTING STARTED 2-2 IEEE-488 communication option, install the proper cable. Refer to Section 7.1 to insta

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE GETTING STARTED 2-32.3.1.2 In Water Submerge the crystal holder into room temperature water (20°C) and adj

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-13 OPERATION The heart of the RQCM is the crystal measurement methodology. It is important th

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-2 3.2 UNDERSTANDING AND SETTING UP A CRYSTAL MEASUREMENT CHANNEL The RQCM can have up to thr

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-33.3.6.1 Crystal Face Mating Connector The mating connector to the Crystal Face Connector i

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-4 Figure 2 Crystal Channel Description

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-53.4 ADJUSTING THE CAPACITANCE CANCELLATION Proper adjustment of the Capacitance Cancellati

OPERATION AND SERVICE MANUALRQCMResearch Quartz Crystal MicrobalanceIPN 603800 Rev.Kwww.inficon.com [email protected] to our continuing progr

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-6 the SMB connector labeled Crystal but don’t install a crystal. If the Sweep LED is flashi

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-7films. ♦ Use a shortest cable possible for connection from the Crystal Holder to the RQCM.

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-8 Face Connector on the RQCM is connected to the potentiostat’s “working electrode” port. A

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-9 Figure 5 Typical Voltammogram Plot Obtained Using the RQCM 3.9 OPERATION GUIDELINES This

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-10 drift is temperature. Review section 4.1.9 for more information on the crystal’s respons

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-113.9.4.4 Prepare Your Solutions Carefully To avoid effects due to changes in the propertie

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-12Figure 6 RQCM Front Panel

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE OPERATION 3-13 Figure 7 RQCM Rear Panel

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-14 CRYSTALS, HOLDERS AND FLOW CELL An essential part of the RQCM syst

TrademarksThe trademarks of the products mentioned in this manual are held by the companies that produce them.All other brand and product names are tr

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-2 Figure 8 INFICON 1-Inch Diameter Crystals – Electrode Configuration

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-34.1.3 CRYSTAL SURFACE FINISH Studies have shown that electrode surface

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-4 The minimum detectable mass change is typically a few ng/cm2 and limit

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-5♦ The acoustic losses in the deposited material♦ The design of the osci

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-6 always good practice to wait at least 30 minutes before performing any

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-7Freq Change vs. TempINFICON AT cut for 25C-2502550751001251501752002252

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-8 4.2.1 CRYSTAL CLEANING The surface properties of the sensor crystal de

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-9organic solvents prior to oxidative cleaning. Polymers that are very

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-10 4.3 CRYSTAL HOLDERS Figure 12 shows a INFICON CHC-100 Crystal Holde

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-11 Figure 13 Crystal Installation 3. Place the Retainer Ring over th

DECLARATION OF CONFORMITY This is to certify that this equipment, designed and manufactured by: INFICON Inc. Two Technology Place East Syrac

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-12 4.3.2 HOLDER CARE AND HANDLING With a robust design, INFICON crys

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE CRYSTALS, HOLDERS AND FLOW CELL 4-13o Remove the crystal to expose the crystal cavity. o Remove both P

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-15 THEORY OF OPERATION Sauerbrey was the first to recognize the ability of the Qu

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-2 It is important to note that under these assumptions, the change in frequency i

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-35.3 THICKNESS CALCULATION Film thickness is often the parameter of interest in many

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-4 Table 5-1 Material Density and Acoustic Impedance Value Material Symbol Density

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-5Palladium Pd 12.00 24.73 Platinum Pt 21.40 36.04 Potassium Chloride KC 1.98 4.

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-6 When the QCM comes in contact with a liquid, there is a decrease in frequency that

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-7illustrated by Figure 14 and Figure 15, respectively. Note that some of the disc

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-8 Resistance Change vs. Wt % Glycerol0100020003000400050000 20406080100Wt % Glycerol

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-9Sω = Angular frequency at series resonance ( fπ2 ) For example, the decay length

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-10 Because a crystal’s impedance is minimum at resonance it is convenient to chara

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-11 Figure 18 Admittance vs. Frequency, Magnitude and Phase of High Q Crystal Figu

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-12 When the above complex conductance is plotted in polar coordinates, one obtains

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-13Figure 21 Polar Admittance Plot of Low Q Crystal Figure 22 Admittance vs. Frequenc

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-14 mechanism for canceling out the imaginary current effectively putting the cente

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-15 Figure 24 Non-zero Phase Lock Figure 24 shows the result of a non-zero phase

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-16 the crystal’s resonant frequency the current leads the voltage and the phase go

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-175.7.3 FREQUENCY ERROR DUE TO IMPERFECT CAPACITANCE CANCELLATION The effect of i

INFICON warrants the product to be free of functional defects in material and workmanship and that it will perform in accordance with its published sp

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-18 5.8 FREQUENCY ERRORS DUE TO IMPERFECT CAPACITANCE CANCELLATION There are two

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-19only 0.018 degrees when measuring a ten-ohm crystal. However, when measuring a

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE THEORY OF OPERATION 5-20 Voc = Open Circuit crystal drive voltage = 125 mV Rs = Crystal drive source re

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE APPLICATIONS 6-16 APPLICATIONS The RQCM will respond very sensitively to minute stress changes on its vi

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE APPLICATIONS 6-2 Q = integrated charge during the reduction in Coulombs, n = number of electrons transfe

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE APPLICATIONS 6-3investigation and/or monitoring of biochemcially significant processes60. Sensitive, se

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE COMPUTER INTERFACE 7-17 COMPUTER INTERFACE Three different interfaces are available to connect the RQCM

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE COMPUTER INTERFACE 7-2 The RQCM acts as DTE, and accordingly the 9-pin connector has ‘plug’ pins. It c

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE COMPUTER INTERFACE 7-37.7 IEEE-488 PARALLEL INTERFACE The optional IEEE-488 interface provides the RQCM

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE COMPUTER INTERFACE 7-4 Table 7-2 IEEE-488 Pin Assignments 7.8 PROTOCOL All communications between the c

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE COMPUTER INTERFACE 7-5Length=2 Instruction Code Receive code Checksum A value of 253 for the instruction

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE COMPUTER INTERFACE 7-6 1. Send RQCM hardware configuration (Code #0) Instructs the RQCM to send its con

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE COMPUTER INTERFACE 7-731,255,109,53 This equals (31*256^3 + 255*256^2 + 109*256 + 53) = 536,833,333 To

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE COMPUTER INTERFACE 7-8 Byte # Description Length bytes Range 1 Input #1 Range 1 0 to 7 2 Input #2 Ra

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE COMPUTER INTERFACE 7-98. Internal Command 9. Set RQCM Interface Address (Code #8) This instruction all

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE DATA ACQUISITION CARD (OPTIONAL) 8-18 DATA ACQUISITION CARD (OPTIONAL) The RQCM has one rear panel slot

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE DATA ACQUISITION CARD (OPTIONAL) 8-2 8.2 TEMPERATURE INPUTS Three temperature inputs are included to sup

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE DATA ACQUISITION CARD (OPTIONAL) 8-38.3 GROUNDING CONSIDERATION Proper grounding and shield terminatio

iv TABLE OF CONTENTS1 GENERAL DESCRIPTION ... 1-1 1.1

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE I/O CARD (OPTIONAL) 9-19 I/O CARD (OPTIONAL) The RQCM has one rear panel slot for the optional I/O card

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE TROUBLESHOOTING GUIDE 10-110 TROUBLESHOOTING GUIDE This section is intended primarily as an aid in underst

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE TROUBLESHOOTING GUIDE 10-2 “Unbalanced” or damaged coaxial cable. Check cable for any signs of damage suc

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE GLOSSARY 11-111 GLOSSARY Conductance The ability to conduct. Conductance is the inverse of resistance. C

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE GLOSSARY 11-2 Viton® DuPont Dow Elastomers’ registered trademark of Fluoroelastomer, offers superior mech

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE GLOSSARY 11-3 Plasma Cleaning A method that utilizes plasma reaction at the surface of the sample and v

RQCM – RESEARCH QUARTZ CRYSTAL MICROBALANCE REFERENCES 12-112 REFERENCES 1 Martin, Step