GB2474831A - Adjusting the impedance of an electrochemical sensor - Google Patents
Adjusting the impedance of an electrochemical sensor Download PDFInfo
- Publication number
- GB2474831A GB2474831A GB0915162A GB0915162A GB2474831A GB 2474831 A GB2474831 A GB 2474831A GB 0915162 A GB0915162 A GB 0915162A GB 0915162 A GB0915162 A GB 0915162A GB 2474831 A GB2474831 A GB 2474831A
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- United Kingdom
- Prior art keywords
- impedance
- sensor
- glass frit
- electrochemical sensor
- thick
- 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- Withdrawn
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- 239000011521 glass Substances 0.000 claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000010304 firing Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000007650 screen-printing Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 3
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims abstract description 3
- 239000012044 organic layer Substances 0.000 claims abstract 2
- 239000013047 polymeric layer Substances 0.000 claims abstract 2
- 239000011248 coating agent Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 12
- 229920000557 Nafion® Polymers 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 229920000554 ionomer Polymers 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 4
- 238000009472 formulation Methods 0.000 claims description 3
- 206010004966 Bite Diseases 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 239000000976 ink Substances 0.000 description 17
- 230000000694 effects Effects 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000005305 interferometry Methods 0.000 description 1
- 238000007567 mass-production technique Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/403—Cells and electrode assemblies
- G01N27/406—Cells and probes with solid electrolytes
- G01N27/407—Cells and probes with solid electrolytes for investigating or analysing gases
- G01N27/4075—Composition or fabrication of the electrodes and coatings thereon, e.g. catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
Method of adjusting the impedance of an electrochemical sensor with interdigitated electrodes 302, 303, 304 of the type made by screen printing on a ceramic substrate 305 a thick-film ink composed of metal or metal oxide powder or particles, glass frit, a temporary organic binder and a temporary solvent; drying to remove the solvent, and firing the composition to fuse the glass frit and burn off the binder. A chemically sensitive organic or polymeric layer 301 is over-coated on the electrodes, which can be tuned to the detection of one or a number of target molecules. The impedance between the electrodes is determined and the chemical composition of the glass frit can be adjusted during the manufacturing process in order to obtain a desired impedance value for the sensor. The sensor may be used to detect gases, such as water vapour in exhaled breath.
Description
ELECTROCHEMICAL SENSOR
The present invention relates to electrochemical sensors and a method for their preparation. The electrochemical sensors are of particular use in gas sensors.
One type of thick-film electrochemical sensor may be made by thick-film screen-printing interdigitated patterns of a suitable thick film ink on a ceramic substrate, and then firing the thick-film ink pattern to form thick film electrical conductors. The thick film ink may be made from a composition comprising metal particles, glass frit, a temporary organic (resin) binder and a temporary solvent. The thick film inks which are used for each type of electrical component are specially formulated so that the final (fired) composition will have pre-determined electronic properties. For example, the thick film inks used to form conductor lines typically comprise 65% to 90% of a highly conductive, finely divided, powdered material, such as powdered copper, silver or gold.
The invention can be practiced with any screen-printable metallic component: inks containing gold, silver, platinum, palladium, ruthenium or thallium will also work. a.. * . a
::..: Glass is usually added to the formulation in order to improve the adhesion of the ink to the substrate. Added as a frit, the screen-printed ink patterns are subjected to *:::29 a temperature just below the thermal degradation temperature for a time sufficient to remove the organic binder. The resultant prints are then heated at or above the glass transition temperature until the glass frit fuses and forms a composite with the *: particulate material within the ink. Glass can also used as an overglaze, to mechanically protect electronic circuit structures, It will be readily appreciated that the glass should not react to a significant extent with any part of the circuit on the substrate.
In use, a sensor may typically be exposed to a gaseous atmosphere, wherein the impedance may be used to determine the concentration of one (or a mixture) of the gaseous components within the atmosphere. We have found that the electronic background signature can be significantly affected by the impedance caused by the presence of the glass.
It would therefore be advantageous to provide an improved method of manufacturing screen-printed electrode patterns which will control the impedance of the resultant electrochemical sensors.
Further, it would be advantageous to provide an improved method of adjusting the impedance values of screen-printed sensors during the manufacturing process, which method is compatible with mass production techniques and is low in cost.
According to the present invention, there is provided a method of making a thick-film screen-printed electrochemical sensor by screen printing on a heat resistant, electrically-insulating substrate, a thick-film ink composition comprising a mixture of metal or metal oxide particles, a glass frit, a temporary organic binder and a temporary solvent, and firing said composition to fuse the glass frit and burn off the organic binder, the method comprising the steps of: manufacturing geometric patterns of one or a series of electrodes, used for various electrochemical applications, on the substrate; S...
* over-coating the resultant electrode pattern with an organic or polymeric *:::: layer used as a chemically-sensitive material; * determining the impedance between the interdigitated electrodes by adjusting the chemical composition of the glass frit so as to obtain the S...
: desired impedance.
We have found that the chemical composition of the glass affects the electrical properties of interdigitated electrodes used as electrochemical sensors, especially if the sensor is subsequently over-coated with another layer, a chemically sensitive layer, used to enhance the sensitivity and or selectivity of the sensor towards gaseous target molecules. Surprisingly, we have found that the properties are significantly affected if the coating were to be an ionic exchange material. The glass in the printing ink can supply ions to the added electrolyte coating such that the electrode output for a given detection gas is greatly enhanced. We believe that the glass, and perhaps the substrate of the electrode, can be tailored to maximise this effect yielding very high sensitivity electrodes, possibly caused by an avalanching effect of the leached ions.
Furthermore, this effect might be magnified by printing' the glass or other ion donor between the electrodes using a conventional substrate. This would have the effect of making the effective gap much smaller and better than be achieved by the printing technique.
The dimension and shape of the printed electrodes and the ink composition determines the impedance of the completed sensor, Some of the factors that also affect the ultimate impedance of the completed sensor are: 1. Exact composition of the glass, and metallic ink, 2. The pattern and geometry of the interdigitated electrodes, 3. Variations in thickness of the interdigitated electrodes, 4. Variations in coating, superimposed over the thick-film screen-printed electrodes. S... * S S
I *.
There are many inter-related factors which enter into the exact value of the *:::: impedance which will be ultimately obtained in any one sensor. The manufacturing control of impedance values, within acceptably close tolerances, previously has been extremely difficult. Because of these and other variables that are always present in the *: manufacturing of screen-printed electrochemical sensors, this method permits the impedance to be controllably (and reproducibly) increased or decreased.
Small variations in percentage composition of components within the ink cause considerable variations in impedance of the product. The ionic composition of the glass affects the conductivity of any layer coated over the surface of the sensor, especially if that coating is an ionic exchange material.
Before drying and firing, the inks also contain a solvent, usually about 15 to 30% by weight of the printed-on composition. This may be butyl or ethyl carbitol acetate. The inks also contain an organic binder, usually ethyl cellulose. The binder usually comprises about 2-6% of the dry weight (after solvent removal) of the composition.
The method of the present invention preferably includes the further steps of monitoring the impedance of the sensors as they are produced and, as the impedance changes from a desired value, adjusting the proportion of glass frit within the thick-film ink formulation to change the impedance of subsequent sensors to a desired value.
The method may further comprises the steps of monitoring the impedance of the sensors as they are produced and, as the impedance changes from a desired value, adjusting the amount (thickness) of coated material to change the impedance of subsequent sensors to a desired value.
The coating may be prepared with any suitable materials. In one preferred embodiment, the coating is prepared to comprise an ionomer, more preferably a a sulfonated tetrafluoroethylene based fluoropolymer-copolymer. Nafion is a particularly preferred ionomer for inclusion in the coating of the sensor. * * a...
In a further aspect, the present invention provides an electrochemical sensor 2t prepared by the method as hereinbefore described. The electrochemical sensor finds general use. In particular, the sensor has been found to be particularly useful in an electrochemical gas sensor, to detect and determine the concentration of components in a gas stream that is allowed to contact the surface of the sensor. The electrochemical sensor finds particular use in determining the presence of components in a gas stream exhaled by a subject, in particular water, typically present as water vapour.
The present invention will be further described, by way of example only, having reference to the accompanying figures, in which: Figure 1 shows examples of mechanical height (cross-sectional) profiles of a typical thick-film screen-printed (uncoated) sensor in the latitudinal (X Profile, or red line) and longitudinal (Y Profile, or blue line) axes; Figure 2 shows examples of mechanical height (cross-sectional) profiles of a thick-film screen-printed sensor that was subsequently coated with approximately 2um layer of Nafion; Figure 3 is a schematic cross-section through a sensor prepared according to the present invention; Figure 4 shows typical results of using the sensor (coated with Nafion) and measuring the conductivity of exhaled water vapour against time; and Figure 5 is a representation of a cross-section through an electrode of a sensor prepared according to the method of the present invention. * * ****
Referring to Figure 1, there is shown mechanical height (cross-sectional) 1.* : profiles of a typical thick-film screen-printed (uncoated) sensor in the latitudinal (X Profile, or red line) and longitudinal (Y Profile, or blue line) axes. The latitudinal section shows that the fingers are approximately 9um in height and 220um in width. The walls' 0SS* : of the printed sensor however are not necessarily vertical, showing a considerable variation in width as a function of height: the sensors are narrower at the top and thicker at the bottom. The longitudinal section shows that the ceramic substrate has a granular' surface, and is not absolutely flat.
The glass frit is not thought to be homogenous throughout the printed sensor -being more concentrated' at the bottom than at the top. This implies that the additional contribution of the glass to any measured signal (impedance) between the electrodes will be more significant at the base.
Vertical measurements are taken using HDVSI (high density vertical scanning interferometry), which possesses sub-nanometer vertical resolution.
Turning to Figure 2, there is shown mechanical height (cross-sectional) profiles of a thick-film screen-printed sensor that was subsequently coated with approximately 2uni layer of Nafion. There is insufficient detail within either the latitudinal and longitudinal sections to reveal the presence of the Nafion coating.
Figure 3 shows a schematic cross-section through a sensor prepared according to the present invention, showing the Nafion coating (301) covering the entire surface of the working (303) and counter (302, 304) electrodes, on a ceramic substrate (305).
Any flow of electrons (current signal) between the working (303) and counter (302, 304) electrodes will traverse through the narrow section in the gap ("valley floor") between the electrodes. *... * * * ** S * .5*
Typical results of using the sensor (coated with Nafion) and measuring the *::: conductivity of exhaled water vapour against time are shown in Figure 4. Curve a) is a coated sensor (containing no glass frit) with no background sensitivity, curve b) shows a higher signal in the exhaled profiles for a coated sensor (containing glass), together : with an elevated background signal due to the increased impedance of the glass A cross-sectional schematic illustration through an electrode is shown in Figure 5. The electrode, indicated as (501) is screen-printed onto a substrate (502), showing the concentration of glass (503) as a function of height within an electrode finger.
The proportion (or concentration) of glass increases down towards the substrate, following firing at elevated temperatures, thought to be a result of the glass adhering to the substrate.
Claims (12)
- CLAIMS1. A method of making a thick-film screen-printed electrochemical sensor by screen printing on a heat resistant, electrically-insulating substrate, a thick-film ink composition comprising a mixture of metal or metal oxide particles, a glass frit, a temporary organic binder and a temporary solvent, and firing said composition to fuse the glass frit and burn off the organic binder, the method comprising the steps of: * manufacturing geometric patterns of one or a series of electrodes, used for various electrochemical applications, on the surface of the substrate; * over-coating the resultant electrode pattern with an organic or polymeric layer used as a chemically-sensitive material; and * determining the impedance between the interdigitated electrodes by adjusting the chemical composition of the glass frit so as to obtain the desired impedance.*::::
- 2. The method according to claim 1, further comprising the steps of monitoring the impedance of the sensors as they are produced and, as the impedance changes from a desired value, adjusting the proportion of glass frit within the * thick-film ink formulation to change the impedance of subsequent sensors to a desired value.
- 3. The method according to either of claims 1 012, further comprising the steps of monitoring the impedance of the sensors as they are produced and, as the impedance changes from a desired value, adjusting the amount (thickness) of coated material to change the impedance of subsequent sensors to a desired value.
- 4. The method according to any preceding claim, wherein the coating is prepared using an ionomer.
- 5. The method according to claim 4, wherein the ionomer is Nafion.
- 6. An electrochemical sensor prepared using a method according to any preceding claim.
- 7. A gas sensor comprising an electrochemical sensor according to claim 6.
- 8. The use of an electrochemical sensor according to claim 6 as a gas sensor.
- 9. The use according to claim 8, wherein the gas sensor is employed to detect a component of a gas stream exhaled by a subject.
- 10. The use according to claim 9, wherein the component is water.
- Il. A method of preparing an electrochemical sensor substantially as hereinbefore described having reference to the accompanying figures. * ** ** I
- 12. An electrochemical sensor substantially as hereinbefore described having I.'-.reference to the accompanying figures. *I*S * S ** bISS * * * S. I
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB0915162A GB2474831A (en) | 2009-09-01 | 2009-09-01 | Adjusting the impedance of an electrochemical sensor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB0915162A GB2474831A (en) | 2009-09-01 | 2009-09-01 | Adjusting the impedance of an electrochemical sensor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB0915162D0 GB0915162D0 (en) | 2009-10-07 |
| GB2474831A true GB2474831A (en) | 2011-05-04 |
Family
ID=41202944
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB0915162A Withdrawn GB2474831A (en) | 2009-09-01 | 2009-09-01 | Adjusting the impedance of an electrochemical sensor |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB2474831A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015161353A1 (en) * | 2014-04-24 | 2015-10-29 | Centro Nacional De Pesquisa Em Energia E Materiais - Cnpem | Sensor device for determining the concentration of analytes in a liquid phase, preferably alcohol and/or water, and method for constructing the sensor device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6365036B1 (en) * | 2000-03-06 | 2002-04-02 | Delphi Technologies, Inc. | Electrode ink formulation for oxygen sensor |
| US20070202012A1 (en) * | 2003-11-12 | 2007-08-30 | Steichen John C | System and method for sensing and analyzing gases |
-
2009
- 2009-09-01 GB GB0915162A patent/GB2474831A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6365036B1 (en) * | 2000-03-06 | 2002-04-02 | Delphi Technologies, Inc. | Electrode ink formulation for oxygen sensor |
| US20070202012A1 (en) * | 2003-11-12 | 2007-08-30 | Steichen John C | System and method for sensing and analyzing gases |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015161353A1 (en) * | 2014-04-24 | 2015-10-29 | Centro Nacional De Pesquisa Em Energia E Materiais - Cnpem | Sensor device for determining the concentration of analytes in a liquid phase, preferably alcohol and/or water, and method for constructing the sensor device |
Also Published As
| Publication number | Publication date |
|---|---|
| GB0915162D0 (en) | 2009-10-07 |
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| Date | Code | Title | Description |
|---|---|---|---|
| WAP | Application withdrawn, taken to be withdrawn or refused ** after publication under section 16(1) |