GB2236855A - Piezoelectric microbalance and method of using the same - Google Patents

Piezoelectric microbalance and method of using the same Download PDF

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Publication number
GB2236855A
GB2236855A GB9018815A GB9018815A GB2236855A GB 2236855 A GB2236855 A GB 2236855A GB 9018815 A GB9018815 A GB 9018815A GB 9018815 A GB9018815 A GB 9018815A GB 2236855 A GB2236855 A GB 2236855A
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GB
United Kingdom
Prior art keywords
piezoelectric
crystal
microbalance
piezoelectric microbalance
substrate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
GB9018815A
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GB9018815D0 (en
Inventor
Kevin Ian Worthington
Stuart Philip Bullock
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Rolls Royce PLC
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Rolls Royce PLC
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Filing date
Publication date
Application filed by Rolls Royce PLC filed Critical Rolls Royce PLC
Publication of GB9018815D0 publication Critical patent/GB9018815D0/en
Publication of GB2236855A publication Critical patent/GB2236855A/en
Withdrawn legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01GWEIGHING
    • G01G3/00Weighing apparatus characterised by the use of elastically-deformable members, e.g. spring balances
    • G01G3/12Weighing apparatus characterised by the use of elastically-deformable members, e.g. spring balances wherein the weighing element is in the form of a solid body stressed by pressure or tension during weighing
    • G01G3/13Weighing apparatus characterised by the use of elastically-deformable members, e.g. spring balances wherein the weighing element is in the form of a solid body stressed by pressure or tension during weighing having piezoelectric or piezoresistive properties

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)

Abstract

A piezoelectric microbalance 10 is described and a method of using such a microbalance 10 for the detection of reaction products deposited thereon as a result of the interaction between a layer of material 10d deposited onto the microbalance 10 with a fluid or substance in which it is immersed. The piezoelectric microbalance 10 comprises a piezoelectric crystal 10a having a known frequency of vibration. Two metallic electrodes 10b are located on opposed faces of the crystal 10a. Above one of the electrodes 10b is an insulating layer 10c which isolates the metallic electrode 10b from a layer of material 10d. In operation the piezoelectric microbalance is immersed into a fluid. The layer 10d interacts with the fluid into which it is immersed and the reaction produces are deposited onto the piezoelectric microbalance. The quartz crystal 10a then experiences a change in its vibration frequency which is directly proportional to the mass of the reaction products deposited onto the piezoelectric crystal. <IMAGE>

Description

PIEZOELECTRIC MICROBALANCE AND METHOD OF USING THE SAME The present invention relates to a piezoelectric microbalance and to a method of using such a microbalance for the detection of reaction products deposited thereon as a result of an interaction between the piezoelectric microbalance and the fluid or substance in which it is immersed.
It is known to use piezoelectric materials as microbalances to detect the proportion of different constituents in fluid mixtures. Piezoelectric materials such as quartz, tourmaline, rochelle salt and the like, are mechanically deformed when subjected to an electrical current and vibrate when a voltage is applied across them.
The frequency of the vibration experienced by a piezoelectric material is dependant upon its mass and will therefore change when a further mass is deposited onto it.
This change in the frequency of vibration of the piezoelectric material is proportional to the mass deposited. The piezoelectric material can therefore be used as a microbalance, the change experienced in its vibration frequency indicating the proportion of a particular constituent in the fluid mixture that has been deposited onto the piezoelectric material.
The present invention seeks to provide an improved piezoelectric microbalance which is capable of evaluating the compatibility of different materials with a fluid or substance in which the piezoelectric microbalance is immersed.
According to the present invention, a piezoelectric microbalance comprises a piezoelectric crystal provided with means for applying a potential difference across the crystal to cause it to vibrate and means for connecting the piezoelectric crystal to an electrical circuit for measurement of the vibration frequency of the piezoelectric crystal, the piezoelectric crystal having on at least one electrically insulating layer deposited thereon to isolate the means for applying a potential difference across the crystal and the means for connecting the crystal to an electrical circuit from an at least one further layer of material deposited thereon for interaction with a substance in which in operation the piezoelectric microbalance is immersed.
Preferably the piezoelectric crystal has integral heating means which may be an at least one substrate coated onto the piezoelectric crystal. The substrate is of a material which will conduct an electrical current and generates heat due to the resistance of the material to the electrical current. The at least one substrate is preferably a coating of nickel or platinum.
In one embodiment the means for applying a potential difference across the crystal to cause it to vibrate and the means for connecting the crystal to an electrical circuit for measurement of the vibration frequency of the piezoelectric crystal are a pair of electrically conductive electrodes on opposite faces of the piezoelectric crystal.
In a further embodiment the means for applying a potential difference across the crystal to cause it to vibrate and the means for connecting the crystal to an electrical circuit for measurement of the vibration frequency of the piezoelectric crystal is an electrically conductive electrode on one face of the crystal and the integral heating means on the opposing face.
The present invention will now be described by way of example and with reference to the accompanying drawings in which, Figure 1 is an exploded view of a piezoelectric microbalance in accordance with one embodiment of the present invention, Figure 2 is a diagrammatic view of a piezoelectric microbalance and its associated circuitry for use in accordance with the present invention.
Figure 3 is an exploded view of a thermal piezoelectric microbalance in accordance with a second embodiment of the present invention, Figure 4 is a diagrammatic view of a thermal piezoelectric microbalance and its associated circuitry for use in accordance with the second embodiment of the present invention.
Figure 5 is an exploded view of a thermal piezoelectric microbalance in accordance with a third embodiment of the present invention.
Figure 6 is an exploded view of a thermal piezoelectric microbalance in accordance with a fourth embodiment of the present invention.
Referring to Figure 1, a piezoelectric microbalance generally indicated at 10, comprises a quartz crystal lOa which has two- metal electrodes lOb. The two metal electrodes lOb are located on opposite faces of and are in electrical contact with the quartz crystal lOa. On one side of the quartz crystal lOa a layer of insulating material lOc, such as alumina borosilicate glass or any other electrically insulating material, is located on top of one of the metal electrodes lOb. The insulating material 10e isolates the metallic electrode lOb from a layer of material lOd. The layer lOd consists of a material whose interaction with a fluid or other substance in which it is immersed is to be investigated.The layer of material lOd may be a layer of metallic alloy, a layer of ion-impregnated material or a catalytic layer which will initiate a reaction with the fluid or substance in which it is immersed.
The layers of different materials, lOb-lOd, on the quartz crystal lOa can be deposited by a variety of techniques such as chemical vapour deposition, vacuum evaporation or sputtering. The technique required will depend upon the material selected for deposition onto the quartz crystal 10a. Each of the layers of different materials, lOb-lOd, are deposited to a thickness typically of the order of 50nm.
In operation the piezoelectric microbalance 10 is immersed in a fluid. The fluid 18 may be static as shown in Figure 2 or dynamic as in a pipe line.
Referring to Figure 2, the piezoelectric microbalance 10 is mounted on a holder 20. Electrical connections between the piezoelectric microbalance 10 and its associated circuitry are made via the pins 22 of the holder 20.
The metal electrodes lOb of the piezoelectric microbalance 10 are connected to an oscillating circuit 24. The oscillating circuit 24 operates to provide a voltage difference across the two electrodes lOb. By applying a voltage difference across the two electrodes lOb the quartz crystal 10a is mechanically deformed and vibrates. The frequency of the vibration experienced by the quartz crystal 10a is dependent upon its mass and is detected by the frequency counter 26.
Having determined the vibration frequency of the quartz crystal l0a, the piezoelectric microbalance is immersed into a fluid 18.
The fluid 18 interacts with the layer of material lOd deposited onto the piezoelectric microbalance.
Decomposition of the fluid 18 produces reaction products which are deposited onto the surfaces of the piezoelectric microbalance 10. The vibration frequency of the quartz crystal l0a changes and is monitored by the frequency counter 26. The piezoelectric microbalance 10 is removed from the fluid 18 in which it is immersed and any residual fluid 18 is washed away prior to monitoring the change in its vibration frequency. The change in the vibration frequency of the quartz crystal l0a is directly proportional to the mass of the reaction products deposited onto the piezoelectric microbalance 10.
It will be appreciated to those skilled in the art that although in the method described the quartz crystal 10a is removed from the fluid 18 to monitor the change in its vibration frequency that this change in its vibration frequency may be monitored with the quartz crystal l0a in situ in the fluid 18.
In a second embodiment of the present invention, shown in Figure 3, the piezoelectric microbalance is provided with an integral heating means.
Referring to Figure 3, a thermal piezoelectric microbalance generally indicated at 11 comprises a quartz crystal ila which has two metal electrodes llb. The two metal electrodes lib are located on opposite faces of and are in electrical contact with the quartz crystal gila.
The insulating material llc isolates the metallic electrodes lib from a thermocouple lie. The thermocouple lie consists of two strips of dissimilar material such as nickel and platinum which overlap one another. Above the thermocouple lie is located a further layer of insulating material lif which isolates the thermocouple lie from an electrical resistance heater llg, The electrical resistance heater lig is formed from a material that will conduct an electrical current but which will generate heat due to the resistance of the material to the flow of electricity. The electrical resistance heat can be formed from metallic elements such as nickel, platinum or gold.
a further insulating layer llh isolates the electrical resistance heater 11g from the layer lid.
In operation the thermal piezoelectric microbalance 11 is immersed in a fluid. Referring to Figure 4 the frequency of the vibration experienced by the quartz crystal ila when a voltage difference is applied across the two electrodes lib is detected by a frequency counter 26. Having determined the vibration frequency of the quartz crystal lia, an electrical current is applied to the electrical resistance heater 11g from a heat supply 28. The electrical resistance heater 119, heats the piezoelectric microbalance 11 which in turn heats the fluid 18. Heating of the thermal piezoelectric microbalance 11 causes a voltage to be generated at the function of the two dissimilar metals of the thermocouple lie which is displayed on a temperature display 30.The temperature display 30 is connected to the heater supply 26 to control the current to the electrical resistance heater 11g.
The fluid 18 is heated by the resistance heater 11g under the control of the thermocouple lie to a temperature at which thermal decomposition of the fluid occurs. The effect of the material layer lid on the thermal decomposition of the fluid 18 can be monitored by the change in the vibration frequency of the quartz crystal ila which is directly proportional to the mass of the reaction products deposited onto the thermal piezoelectric microbalance.
As the vibration frequency of the quartz crystal iOa is dependant upon the applied mass, the sensitivity of the thermal piezoelectric microbalance 11 can be enhanced by reducing the number of layers of material, llb-llf, on the quartz crystal lia.
In a third embodiment of the present invention, shown in Figure 5, a thermal piezoelectric microbalance 12 comprises a quartz crystal 12a with two metal electrodes 12b. The two metal electrodes 12b are in electrical contact with and are located on opposite faces of the quartz crystal 12a. A layer of material 12e, such as platinum or nickel, is deposited onto one side of the crystal 12a directly on top of one of the electrodes 12b.
This layer of material 12e functions as both the electrical resistance heater llg and the thermocouple lie shown in Figure 3. The electrical resistance of the layer 12e causes the thermal piezoelectric microbalance 12 to heat up. The temperature of the thermal piezoelectric microbalance 12 is measured by monitoring the change in the electrical resistance of the layer of material 12e.
In a further embodiment of the present invention, shown in Figure 6, a thermal piezoelectric microbalance 13 comprises a quartz crystal 13a which has a single metallic electrode 13b on one of its faces. On the opposite face of the quartz crystal 13a a layer of material 13e such as nickel or platinum is deposited such that it is in electrical contact with the quartz crystal 12a. In this embodiment the layer 13e of platinum or nickel operates as both the electrical resistance heater and the thermocouple as previously described and also functions as one of the electrodes for connection to the oscillating circuit 24 in Figure 4.
In the two embodiments, shown in Figures 5 and 6, the number of layers on the quartz crystals 12a and 13a, have been reduced so enhancing the sensitivity of the thermal piezoelectric microbalances 12 and 13. The material layers 12d and 13d can then be deposited onto the thermal piezoelectric microbalances 12 and 13 to investigate their interaction with the fluid 18 in which they are immersed.
It will be appreciated that although in the embodiments described the layers iOd,iid,12d and 13d are deposited onto only one of the surfaces of the quartz crystals, that any number of additional layers may be deposited onto other faces of the crystals depending on the particular application.

Claims (15)

Claims:
1. A piezoelectric microbalance comprising a piezoelectric crystal provided with means for applying a potential difference across the crystal to cause it to vibrate and means for connecting the piezoelectric crystal to an electrical circuit for measurement of the vibration frequency of the piezoelectric crystal, the piezoelectric crystal having an at least one electrically insulating layer deposited thereon to isolate the means for applying a potential difference across the crystal and the means for connecting the crystal to an electrical circuit from an at least one further layer of material deposited thereon for interaction with a substance in which in operation the microbalance is immersed.
2. A piezoelectric microbalance as claimed in claim 1 in which the piezoelectric crystal has integral heating means.
3. A piezoelectric microbalance as claimed in claim 2 in which the integral heating means is an at least one substrate coated on the piezoelectric crystal.
4. A piezoelectric microbalance as claimed in claim 3 in which the integral heating means is an at least one substrate of a material which will conduct an electrical current and generate heat due to the resistance of the material to the electrical current.
5. A piezoelectric microbalance as claimed in claim 3 or 4 in which the at least one substrate is a coating of nickel.
6. A piezoelectric microbalance as claimed in claim 3 or 4 in which the at least one substrate is a coating of platinum.
7. A piezoelectric microbalance as claimed in claims 2-6 in which the means for applying a potential difference across the crystal to cause it to vibrate and the means for connecting the crystal to an electrical circuit for measurement of the vibration frequency of the piezoelectric crystal are an electrically conducting electrode on one face of the piezoelectric crystal and the integral heating means on the opposing face of the piezoelectric crystal.
8. A piezoelectric microbalance as claimed in claim 3 in which the piezoelectric crystal has a plurality of substrates including a first substrate which acts to heat the piezoelectric crystal, a second substrate to control the heating of the piezoelectric crystal said first and second substrates having insulating layers interdisposed for electrical isolation.
9. A piezoelectric microbalance as claimed in claim 8 in which the first substrate consists of a material which will conduct an electrical current and generate heat due to the resistance of the material to the electrical current.
10. A piezoelectric microbalance as claimed in claim 8 or claim 9 in which the second substrate is a coating of two dissimilar materials which form a thermocouple.
11. A piezoelectric microbalance as claimed in any preceding claim in which the means for applying a potential difference across the crystal to cause it to vibrate and the means for connecting the crystal to an electrical circuit for measurement of the vibration frequency of the piezoelectric crystal are a pair of electrically conducting electrodes on opposite faces of the piezoelectric crystal.
12. A piezoelectric microbalance as hereinbefore described with reference to and as shown in figure 1.
13. A piezoelectric microbalance as hereinbefore described with reference to and as shown in figure 3.
14. A piezoelectric microbalance as hereinbefore described with reference to and as shown in figure 5.
15. A piezoelectric microbalance as hereinbefore described with reference to and as shown in figure 6.
GB9018815A 1989-10-06 1990-08-29 Piezoelectric microbalance and method of using the same Withdrawn GB2236855A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB898922601A GB8922601D0 (en) 1989-10-06 1989-10-06 Thermal piezoelectric microbalance and method of using the same

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GB9018815D0 GB9018815D0 (en) 1990-10-10
GB2236855A true GB2236855A (en) 1991-04-17

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GB9018815A Withdrawn GB2236855A (en) 1989-10-06 1990-08-29 Piezoelectric microbalance and method of using the same

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0564780A1 (en) * 1992-04-06 1993-10-13 Shipley Company Inc. Methods and apparatus for maintaining electroless plating solutions
WO1996035103A1 (en) * 1995-05-04 1996-11-07 Michael Rodahl A piezoelectric crystal microbalance device
CN1034441C (en) * 1993-08-12 1997-04-02 武汉大学 Time identifying electrochemistry quartz crystal micro-balance
CN1035132C (en) * 1995-05-02 1997-06-11 武汉美 Small crystal-resonance digital-display electronic weigher
EP0943903A1 (en) * 1997-09-08 1999-09-22 Ngk Insulators, Ltd. Mass sensor and mass detection method
DE10050632A1 (en) * 2000-10-12 2002-04-18 Stiftung Caesar For a quantitative and qualitative detection of biological molecules, for analysis, comprises a sensor having a substrate where an analyte bonds to it to measure the total bonded mass and its molecular weight

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2149109A (en) * 1983-07-13 1985-06-05 Suisse Horlogerie Rech Lab Piezoelectric contamination detector
WO1987002134A1 (en) * 1985-09-26 1987-04-09 Nederlandse Organisatie Voor Toegepast-Natuurweten An apparatus for determining the condition of a material, in particular the adsorption of a gas or liquid on said material
GB2219858A (en) * 1988-06-15 1989-12-20 Nat Res Dev Apparatus and method for detecting small changes in attached mass on piezoelectric devices used as sensors.

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2149109A (en) * 1983-07-13 1985-06-05 Suisse Horlogerie Rech Lab Piezoelectric contamination detector
WO1987002134A1 (en) * 1985-09-26 1987-04-09 Nederlandse Organisatie Voor Toegepast-Natuurweten An apparatus for determining the condition of a material, in particular the adsorption of a gas or liquid on said material
GB2219858A (en) * 1988-06-15 1989-12-20 Nat Res Dev Apparatus and method for detecting small changes in attached mass on piezoelectric devices used as sensors.

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5484626A (en) * 1992-04-06 1996-01-16 Shipley Company L.L.C. Methods and apparatus for maintaining electroless plating solutions
EP0564780A1 (en) * 1992-04-06 1993-10-13 Shipley Company Inc. Methods and apparatus for maintaining electroless plating solutions
CN1034441C (en) * 1993-08-12 1997-04-02 武汉大学 Time identifying electrochemistry quartz crystal micro-balance
CN1035132C (en) * 1995-05-02 1997-06-11 武汉美 Small crystal-resonance digital-display electronic weigher
US6006589A (en) * 1995-05-04 1999-12-28 O-Sense Ab Piezoelectric crystal microbalance device
WO1996035103A1 (en) * 1995-05-04 1996-11-07 Michael Rodahl A piezoelectric crystal microbalance device
EP0943903A1 (en) * 1997-09-08 1999-09-22 Ngk Insulators, Ltd. Mass sensor and mass detection method
EP0943903A4 (en) * 1997-09-08 2000-03-15 Ngk Insulators Ltd Mass sensor and mass detection method
US6386053B1 (en) 1997-09-08 2002-05-14 Ngk Insulators, Ltd. Mass sensor and mass detection method
US6612190B2 (en) 1997-09-08 2003-09-02 Ngk Insulators, Ltd. Mass sensor and mass sensing method
US6840123B2 (en) 1997-09-08 2005-01-11 Ngk Insulators, Ltd. Mass sensor and mass sensing method
US6895829B2 (en) 1997-09-08 2005-05-24 Ngk Insulators, Ltd. Mass sensor and mass sensing method
US7089813B2 (en) 1997-09-08 2006-08-15 Ngk Insulators, Ltd. Mass sensor and mass sensing method
DE10050632A1 (en) * 2000-10-12 2002-04-18 Stiftung Caesar For a quantitative and qualitative detection of biological molecules, for analysis, comprises a sensor having a substrate where an analyte bonds to it to measure the total bonded mass and its molecular weight

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Publication number Publication date
GB8922601D0 (en) 1989-11-22
GB9018815D0 (en) 1990-10-10

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