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11111\Q /1111 0 9 “2” 0 W2 I 111 J 106 Patent Application Publication Oct US 20120247186A1 (19) United States (12) Patent Application Publication (10) Pub. No.: US 2012/0247186 A1 Sanjeeb et al. (43) Pub. Date: Oct. 4, 2012 (54) NOX GAS SENSOR INCLUDING NICKEL Publication Classi?cation OXIDE (51) Int. Cl. (75) Inventors: Tripathy Sanj eeb, Bangalore (IN); G01N 27/00 (2006.01) Abhilasha Srivastava, Bangalore B05D 3/02 (2006.01) (IN); Raju Raghurama, Bangalore B05D 5/12 (2006.01) (IN); Reddappa Reddy (52) us. c1. ................................... .. 73/3105; 427/1266 Kumbarageri, Bangalore (IN); Srinivas S.N. Mutukuri, Bangalore (57) ABSTRACT (1N) One example includes a sensor for sensing NOX, including an electrically insulating substrate, a ?rst electrode and a second (73) Assignee: Honeywell International Inc., electrode, each disposed onto the substrate, Wherein each of MorristoWn, N] (U S) the ?rst electrode and the second electrode has a ?rst end con?gured to receive a current and a second end and a sensor (21) Appl. No.: 13/407,453 element formed of nickel oxide poWder, the sensor element disposed on the substrate in electrical communication With Filed: Feb. 28, 2012 (22) the second ends of the ?rst electrode and the second electrode. In some examples, electronics are used to measure the change Related US. Application Data in electrical resistance of a sensor in association With NOx (60) Provisional application No. 61/447,351, ?led on Feb. concentration near the sensor. In some examples, the sensor is 28, 2011. maintained at 575° C. /m /1111 A20 HEAHNG NOX CKT CIRCUIT 11111\Q /1111 0 9 “2” 0 W2 I 111 j 106 Patent Application Publication Oct. 4, 2012 Sheet 1 0f 10 US 2012/0247186 A1 21 02:5: E616 Patent Application Publication Oct. 4, 2012 Sheet 2 0f 10 US 2012/0247186 A1 26 24 22 WW -'2.% 1%" "1?. \ ‘2A \—\4 ‘2.2 FIG. 2 3% W“ ‘16 1?.“ 3m FIG. 3 (a? 3“ WW \ o o o o o 0 <5 \A‘ O O O O O O O O 28 i Patent Application Publication Oct. 4, 2012 Sheet 3 0f 10 US 2012/0247186 A1 Patent Application Publication Oct. 4, 2012 Sheet 4 0f 10 US 2012/0247186 A1 m fOOA SYNTHESIZING A NIO POWDER T Ass MIXING A PASTE INCLUDING THE NiO POWDER AND A BINDER T fm DEPOSITING THE PASTE ONTO A SUBSTRATE, SUCH AS ONTO A CTL SENSOR-HEATER SUBSTRATE T fmII SINTERING THE SENSOR T /6\2 CONNECTING ELECTRICAL CONTACTS TO THE SENSOR T /%\A PACKAGING THE SENSOR, SUCH AS BY POTTING WITH M203, BONDING THE SENSOR T0 WIRE AND PACKAGING THE SENSOR IN A HOUSING l- — — — — — — — — —T — — — — — — — — [m_| I VERIFYING THE SENSOR, SUCH AS BY TESTING IN A GAS I | FORMED 0F N2, 300 PPM 00, 20% e02, 200 PPM NH3, | | 15 PPM S02 AND 20% 02 AT 5750 | |_ _________ 5m J FIG. 6 Patent Application Publication Oct. 4, 2012 Sheet 5 0f 10 US 2012/0247186 A1 START /'IDA NICKEL SALT BASE, SUCH AS 25 CRAMS, COMBINED WITH ACETONE INTO MIX I f'TDB GRIND MIX, SUCH AS FOR 20 MINUTES VIA MORTAR AND PESTLE HEAT MIX, SUCH AS AT IZD'C FOR 15 MIN I /'IID GRIND MIX, SUCH AS WITH MORTAR AND PESTLE I /'II2 HEAT MIX, SUCH AS AT 2500 FOR 30 MIN CALCINATIONSEQUENCE I [TIA GRIND MIX, SUCH AS WITH MORTAR AND PESTLE I /'TI6 HEAT MIX, SUCH AS AT 6500 FOR 30 MIN I /'TIS GRIND MIX, SUCH AS WITH MORTAR AND PESTLE ‘72D END FIG. 7 Patent Application Publication Oct. 4, 2012 Sheet 6 0f 10 US 2012/0247186 A1 ‘7/ BBC BB2 fm NiO POWDER MIXED WITH COMMERCIAL VEHICLE, SUCH AS AT 30% COMMERCIAL VEHICLE BY WEIGHT I fms BALL MILL MIX, SUCH AS AT I HOUR AT 450 RPM USING 5MM ZIRCONIA BALLS AND ZIRCONIA CONTAINER I EBIIB . 8 Patent Application Publication Oct. 4, 2012 Sheet 7 0f 10 US 2012/0247186 A1 SW2. fQQA NIO PASTE MAINTAINED AT SELECTED VISCOSITY, SUCH AS BETWEEN 180-220 POISE I Kw‘) NiO FILM CREATED, SUCH AS AT A THICKNESS 0F AROUND I20 MICRONS I 5%% PG, 9 Patent Application Publication Oct. 4, 2012 Sheet 8 0f 10 US 2012/0247186 A1 Am NiO SINTERED, SUCH AS AT TZU'C FOR 45 MIN IN A MUFFLE FURNACE T fms NiO SINTERED, SUCH AS AT 500'C FOR 30 MIN IN A MUFFLE FURNACE T Am Ni0 SINTERED, SUCH AS AT 700'C FOR 5 MIN IN A MUFFLE FURNACE T Am COOLING THE NiO A SAUCE. 1a 0 Patent Application Publication Oct. 4, 2012 Sheet 9 0f 10 US 2012/0247186 A1 Emmi; 0100112geaogiwoogxs812Jags @EN asa:GaO20 25585caN02 am _ Has 8: as Patent Application Publication Oct. 4, 2012 Sheet 10 0f 10 US 2012/0247186 A1 mzi¢m85:8 _ 2E mmmzsz$5 6QMN 82 E82| 82| 82| E828Q72X02 $0550zazmm US 2012/0247186 A1 Oct. 4, 2012 NOX GAS SENSOR INCLUDING NICKEL [0013] FIG. 8 is a How chart ofa method for mixing a paste OXIDE including nickel oxide poWder such as nanopoWder, accord ing to some examples. CROSS REFERENCE TO RELATED [0014] FIG. 9 is a How chart of a method for applying a APPLICATIONS paste to a substrate, according to some examples. [0001] The present application claims priority under 119(e) [0015] FIG. 10 is a How chart of a method for sintering a to US. Provisional Application No. 61/447,351, ?led Feb. 28, sensor element, according to some examples. 2011, Which is related to US Patent Application Publication [0016] FIG. 11 ShoWs the performance evaluation of the No. US2008002050 and US Patent Publication No. sensor by measuring the resistance change With gas concen US20090020422, the entire speci?cation of each of Which is tration, and is made up of a nickel oxide sensor example, incorporated by reference in its entirety. including nickel oxide poWder such as nanopoWder, exposed to a cocktail gases at 575° C., shoWing sensitivity to NO and BACKGROUND NO2 according to some examples. [0017] FIG. 12 shoWs the performance evaluation of the [0002] The generic term “NOx” describes oxides of nitro sensor by measuring the resistance change With gas concen gen, such as nitrogen monoxide (“NO”) and nitrogen dioxide tration, and is engine response at different operational steps (“N02”). NOx is produced as a by-product of combustion in some engines. Aircraft engines, automobile engines, and and sensor sensitivity to NOx, according to some examples. poWer generators, for example, utiliZe combustion processes that produce NOx. DETAILED DESCRIPTION [0003] NOx is believed to contribute to the production of [0018] In the folloWing description, reference is made to acid rain, smog, and the depletion of the oZone layer. For the accompanying draWings that form a part hereof, and in example, reactions including volatile organic compounds and Which is shoWn by Way of illustration speci?c embodiments NOx, occurring in sunlight, are believed to form oZone. that are practiced. These embodiments are described in suf Ground-level oZone is believed to contribute to throat irrita ?cient detail to enable those skilled in the art to practice the tion, congestion, chest pains, nausea and labored breathing. embodiments, and it is to be understood that other embodi Such oZone is believed to aggravate respiratory conditions ments is utiliZed and that structural, logical and electrical like chronic lung and heart diseases, allergies and asthma. changes is made. The folloWing description of example OZone is believed to effectively “age” lungs and may contrib embodiments is, therefore, not to be taken in a limited sense, ute to lung disease. With an increase in the number of With the scope being de?ned by the appended claims. vehicles, the amount of NOx produced is increasing, and is believed to exacerbate environmental harm. [0019] NOx is sometimes estimated from measured NO, based on an assumption that total NOx is 5% NO2 and 95% [0004] For at least these reasons, it is desirable to monitor NOx gas concentrations in emissions. In fact, NOx sensing, NO. This assumption is generally acceptable When combus tion exhaust gases are measured at the outlet of the combus such as for emission control, is a requirement of regulations governing the operation of some diesel and spark ignition tion system, and the oxygen concentration is loW. If the mea engines. Regions applying such regulations include countries surement is made at the exhaust outlet or in the atmosphere, in North America and Europe. As an example, in 2010, the hoWever, the NO2 percentage is likely higher than 5% of the total production of emission-regulated heavy-duty trucks, total NOx. For at least this reason, measurement of both NO and NO2 is recommended for accurate total NOx concentra Which Will be required to monitor NOx, Will be at least 1.5 million. Similar emission standards are being proposed for tion. Accordingly, the present subject matter provides sensors other internal combustion engines (i.e., passenger cars, boats, that measure both NO and N02, rather than deriving one measurement from the other. sport vehicles, etc.). Accordingly, there is a need for a reliable NOx sensor to monitor and control emissions. [0020] The present subject matter provides several advan tages. The sensors disclosed herein provide exemplary syn BRIEF DESCRIPTION OF THE DRAWINGS theses of NiO poWder such as nanopoWder capable of pro ducing increasing conductivity (i.e., decreasing resistance [0005] FIG. 1 illustrates an engine system including a sen measured at a sensor) in the presence of both NO and NO2 sor assembly coupled to an exhaust system, according to gases. Various examples provide equal sensitivity to NO and some examples. N02, hence, reliable measurement of the total NOx content [0006] FIG.
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