CN101149354B - Gas sensitization array sensor and its manufacture method - Google Patents
Gas sensitization array sensor and its manufacture method Download PDFInfo
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- CN101149354B CN101149354B CN2007100536521A CN200710053652A CN101149354B CN 101149354 B CN101149354 B CN 101149354B CN 2007100536521 A CN2007100536521 A CN 2007100536521A CN 200710053652 A CN200710053652 A CN 200710053652A CN 101149354 B CN101149354 B CN 101149354B
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Abstract
The invention discloses a kind of array sensor for gas and the preparing method. The sensor uses the aurum, platinum or argentum as electrode; the RuO2, MoSi2, W or Pt is as heating membrane material; the random one or several kinds of the ZnO, SnO2 or Fe2O, or ZnO, SnO2 or Fe2O3 and Pt0.1wt%-3wt%, Pd0.1wt%-3wt%, Ni1wt%-30wt%, TiO21wt%-30wt%, WO31wt%-40wt%, Co2O3 1wt%-15wt%, V2O51wt%-30wt%, Al2O31wt%-20wt%, MnO21wt%-30wt% is as the sensing layer material. It gets the gas sensing array on the alumina, aluminium nitride or silicon base sheet with anti high temperature, electric insulating and heat conducting by the screen printing technology. The gas sensing array is fixed on the basal seat by the axis to form the gas sensing array sensor by ultrasonic hot press welding electrode leg wire. The sensor has the low production cost, low power cost, good mechanism stability. Each unit has the good gas sensing character and the process is proper for the big batch production.
Description
Technical field
The invention belongs to the gas sensitization array sensor technical field, be specifically related to a kind of gas sensitization array sensor and preparation method thereof.
Background technology
Gas sensor has been widely used in environmental monitoring, fireproof alarming, chemical industry, food-processing industry field, in all gases sensor, metal oxide sensor obtains with its simple in structure, cheap characteristics paying close attention to, because most of metal oxide gas sensitive (SnO
2, ZnO, Fe
2O
3Deng) need be 300-400 ℃ temperature work, the device power consumption made from conventional art is very big, and volume is also big, and single-sensor can only be realized simple the warning to gas.Use micro-electromechanical system (MEMS) process technology (Kraig D.Mitzner, Jason Sternhagen, David W.Galipeau, Development of a micromachined hazardous gas sensor array, Sensors andActuators B 93 (2003) 92-99), with the monocrystalline silicon piece is substrate, the gas sensitization array sensor of the microelectronics manufacturing of employing standard and post-processing technology preparation, though can prepare the gas sensor and the array thereof of low-power consumption, the stability of sensor and array thereof and consistance thereof remain the deadly defect of this technology.And this technology also is difficult to satisfy each element in the sensor array and possesses the requirement that different chemical is formed.Simultaneously, the production equipment of micro-electromechanical system (MEMS) processing is very expensive, the working condition harshness.And the encapsulation or the employing of the array substrate of thick film technology preparation are mounted on the pedestal, or the hanging type (I.Czech that adopts contact conductor to support, J.Manca, J.Roggen et al.ElectricalCharacterisation and Reliability Studies of Thick Film Gas Sensor Structures.Proceedings of the 1996 IEEE International Conference on Microelectronic TestStructures, Vol.9, March 1996), the former array substrate heats up with pedestal, energy consumption is very big, a little less than the unsettled support strength of latter's contact conductor, the device mechanical stability is very poor.These factors have seriously hindered promoting the use of of sensor array.Especially at present at Aero-Space, environmental monitoring, building safety, food is false proof and the Automation of Manufacturing Process controlling party has very eager needs in the face of low-power consumption, stable microstructure gas sensitization array sensor.
Summary of the invention
The purpose of this invention is to provide a kind of gas sensitization array sensor, this gas sensitization array sensor production cost is low, low in energy consumption, good mechanical stability; The present invention also provides the preparation method of this gas sensitization array sensor.
Gas sensitization array sensor provided by the invention, it is characterized in that: first, second test electrode is positioned at same side, three, the 4th test electrode is positioned at same side, they lay respectively on two relative limits of substrate, and array well heater positive electrode and loop electrode thereof lay respectively on other two relative limits of substrate; The loop electrode of the loop electrode of first, second test electrode and the 3rd, the 4th test electrode is between first, second test electrode and the 3rd, the 4th test electrode, and it is parallel with first, second test electrode respectively with test electrode, the loop electrode and the 3rd of the loop electrode of first, second test electrode, array well heater positive electrode, the loop electrode of the 4th test electrode ' ㄈ ' shape that is formed by connecting is as public electrode; On the substrate between the loop electrode of array well heater positive electrode and array well heater positive electrode, be printed with heating film, on the substrate between each test electrode public electrode corresponding, be printed with the metal oxide sensitive layer respectively with it, center at substrate is equipped with axle, axle passes heating film, and be fixed on the center of pedestal, leave the gap between substrate and the pedestal; Also be provided with at least six binding posts on the pedestal, be connected with each test electrode, array well heater positive electrode and public electrode by contact conductor respectively.
The preparation method of above-mentioned gas sensitization array sensor, its step comprises:
(1) serigraphy array well heater positive electrode, first to the 4th test electrode and the public electrode on the substrate after the cleaning, substrate thickness be smaller or equal to 1 millimeter, and dry back was 700～850 ℃ of following sintering 5～20 minutes;
(2) serigraphy one deck heating film between heating of substrate device electrode and corresponding public electrode, dry back was 500～850 ℃ of following sintering 5～20 minutes;
(3) screen-printed metal oxide sensitive layer between test electrode and corresponding public electrode, dry back was at 500～850 ℃ of following sintering 1-4 hours;
(4) repeating step (3) prepares the metal oxide sensitive layer of each unit of array successively, obtains gas sensitization array;
(5) on the heating film of gas sensitization array, bore a hole;
(6) adopt axle substrate to be fixed on the pedestal by the hole of gas sensitization array, and fixed each contact conductor of nation, burin-in process makes gas sensitization array sensor.
The present invention is with the material of multiple gas with various sensitivity characteristic, adopt screen printing technique to prepare sensitive layer and constitute gas sensitization array, gas sensitization array is fixed on the pedestal by single shaft, constitute gas sensitization array sensor through ultrasonic thermocompression welding electrode lead-in wire, overcome the deficiency of existing gas sensitization array sensor effectively, realized low-power consumption, low cost, helped to produce in enormous quantities.
Compare with micro-electromechanical system (MEMS) process technology, the preparation technology of gas sensitization array sensor of the present invention requires lower to production equipment, production environment, each sensor array has better consistance, each unit sensitive layer of array has better air-sensitive stability.Gas sensitization array sensor binding pattern recognition technology is formed electric nasus system can be in real time, fast tested gas is realized qualitative identification and quantitative test, overcome that the single-sensor air-sensitive is optionally limited to and the stability of the shortcoming of the large volume of a plurality of sensor combinations, high energy consumption and micro-electromechanical system (MEMS) processing gas sensitization array sensor and consistance is poor, production equipment is very expensive, the shortcoming of working condition harshness.Adopt screen printing technique, in conjunction with brand-new nano material system, the gas sensitization array sensor structure that design is unique provides assurance for realizing low-power consumption, low cost, the gas sensitization array sensor that air-sensitive is stable.
Description of drawings
Fig. 1 is the structural representation that contains the gas sensitization array sensor of four gas sensor units, and wherein Fig. 1 (a) is a vertical view; Fig. 1 (b) is the AB sectional front view of Fig. 1 (a);
Fig. 2 is heating electrode, test electrode and the public electrode layout structure synoptic diagram of gas sensitization array sensor of the present invention, and wherein Fig. 2 (a) is the prepared in batches synoptic diagram; Fig. 2 (b) is a synoptic diagram on the array substrate;
Fig. 3 has printed layout structure synoptic diagram, wherein Fig. 3 (a) vertical view behind the heating film for gas sensitization array substrate of the present invention; The half tone pattern of Fig. 3 (b) printing heating film.
Fig. 4 has printed layout structure synoptic diagram, wherein Fig. 4 (a) vertical view behind the unit sensitive layer for gas sensitization array sensor substrate of the present invention; The half tone pattern (b) of Fig. 4 (b) printing sensitive membrane;
Fig. 5 has printed vertical view behind two unit sensitive layers for gas sensitization array sensor substrate of the present invention;
Fig. 6 has printed vertical view behind three unit sensitive layers for gas sensitization array sensor substrate of the present invention;
Fig. 7 has printed vertical view behind four unit sensitive layers for gas sensitization array sensor substrate of the present invention;
Fig. 8 is gas sensitization array sensor substrate center perforation of the present invention back vertical view;
Fig. 9 is the equilibrium temperature and the energy consumption graph of a relation of gas sensitization array sensor of the present invention;
Figure 10 is the alcohol air-sensitive response curve of the preferred embodiment of the present invention four unitary gas sensitization array sensors.
Embodiment
The present invention is further detailed explanation below in conjunction with accompanying drawing and example.
As shown in Figure 1, the structure of gas sensitization array sensor of the present invention is: first, second test electrode 9,11 and the 3rd, the 4th test electrode 12,13 lay respectively on the opposite side of substrate 3, and array well heater positive electrode 7 and loop electrode 10 thereof lay respectively on another opposite side of substrate 3.The loop electrode 15 of the loop electrode 14 and the 3rd of first, second test electrode 9,11, the 4th test electrode 12,13 is between first, second test electrode 9,11 and the 3rd, the 4th test electrode 12,13, and it is parallel with test electrode 12,13 with first, second test electrode 9,11, the loop electrode 15 of the loop electrode 10 and the 3rd of the loop electrode 14 of first, second test electrode 9,11, array well heater positive electrode 7, the 4th test electrode 12,13 is formed by connecting ' ㄈ ' shape as public electrode, as Fig. 2 (b).Be printed with heating film 4 on substrate 3 planes between the loop electrode 10 of array well heater positive electrode 7 and array well heater positive electrode 7, as Fig. 3 (a), Fig. 3 (b) is printing screen plate figure.Type metal oxide sensitive layer 8 respectively on substrate 3 planes between test electrode 9,11,12,13 public electrode corresponding with it constitutes one or more gas sensor units, as Fig. 4,5,6,7.At the center of substrate 3 axle 5 is installed, axle 5 passes heating film 4, and is fixed on the center of pedestal 2, as Fig. 8, and makes substrate 3 and pedestal 2 leave gap (being generally 1-3mm), as Fig. 1 (b).Pedestal 2 is provided with at least 6 binding posts 1, is connected with public electrode with test electrode 9,11,12,13 and array well heater positive electrode 7 by contact conductor 6 respectively.
The above-mentioned gas sensitization array sensor adopts screen printing technique to make, and its step comprises:
(1) serigraphy array well heater positive electrode 7, test electrode 9,11,12,13 and public electrode on the substrate after the cleaning 3, substrate thickness be smaller or equal to 1 millimeter, and dry back was 700～850 ℃ of following sintering 5～20 minutes; Electrode material can be conductive materials such as gold, platinum or silver; Substrate material can be resistant to elevated temperatures electrically insulating materials such as aluminium oxide, aluminium nitride or silicon, as Fig. 2.
(2) serigraphy one deck heating film 4 between heating of substrate device electrode 7 and corresponding public electrode, dry back was 500～850 ℃ of following sintering 5～20 minutes; As Fig. 3.
(3) screen-printed metal oxide sensitive layer 8 between test electrode 9 and corresponding public electrode, as Fig. 4, dry back was at 500～850 ℃ of following sintering 1-4 hours;
(4) repeating step (3) prepares the metal oxide sensitive layer 8 of each unit of array successively, obtains gas sensitization array, as Fig. 5,6,7.(3), can print the highest sensitive layer of sintering temperature earlier according to the height of sensitive layer sintering temperature in (4) step, print the sensitive layer of lower sintering temperature behind drying, the sintering more successively.The sensitive layer of identical sintering temperature and time is dry earlier, and intact back to be printed is once sintered.
(5) on the heating film of the gas sensitization array that step (4) is obtained, bore a hole, as Fig. 8 with laser or jig drill.
(6) the perforation gas sensitization array that is obtained in the step (5) is fixed on the pedestal 2 by axle 5, fixed each contact conductor 6 of ultrasound wave hot pressing gold wire bonder nation, burin-in process makes the gas sensitization array sensor of structure as shown in Figure 1.
Heating film can be RuO
2, MoSi
2, W or Pt the slurry serigraphy be prepared from, as Fig. 3.
The material of metal oxide sensitive layer 8 can be ZnO, SnO
2Or Fe
2O
3, perhaps ZnO, SnO
2Or Fe
2O
3With arbitrary or several doping in following each component:
Pt (0.1wt%-3wt%), Pd (0.1wt%-3wt%), Ni (1wt%-30wt%), TiO
2(1wt%-30wt%), WO
3(1wt%-40wt%), Co
2O
3(1wt%-15wt%), V
2O
5(1wt%-30wt%), Al
2O
3(1wt%-20wt%), MnO
2(1wt%-30wt%) wait the doped and compounded thing material that forms.
Example:
Below with reference to each accompanying drawing example in detail the preferred embodiments of the present invention:
Embodiment one:
(1) system of the substrate of belt electrode and well heater.With the thick Al of 0.4mm
2O
3Pottery is a substrate 3, by serigraphy gold paste material, and the slurry film of the public electrode that disposable preparation array well heater positive electrode 7, first, second, third, fourth test electrode 9,11,12,13 and loop electrode 10,14,15 thereof are formed.After the drying, 900 ℃ of sintering are 10 minutes in the air, and furnace cooling obtains electroded substrate as shown in Figure 2 to room temperature.Adopting the half tone serigraphy RuO shown in Fig. 3 (b)
2The slurry film, 850 ℃ of sintering are 15 minutes in the air of dry back, and furnace cooling is to room temperature, obtains the belt electrode shown in Fig. 3 (a) and the substrate of well heater.
(2) preparation of the sensitive layer 8 of gas array.With four-acicular nanometer ZnO, 10wt%TiO
2Doping four-acicular nanometer ZnO, 5wt%Co
2O
3Doping four-acicular nanometer ZnO, 15wt%MnO
2Doping four-acicular nanometer ZnO is a sensitive material, adds the 30wt% organic bond respectively and mixes, and makes stable printable slurry in 6 hours with the bowl mill ball milling.Print the sensitive layer of Unit four respectively with half tone shown in Fig. 4 (b), after every printing Unit one is to be dried, at the printing next unit.In 700 ℃ of sintering of sintering furnace 3 hours, obtain four unitary gas sensitization array sheets as shown in Figure 7 at last.
(3) gas array package.The 3 center laser beam perforations of the array substrate with four unitary gas sensitive layers 8 to as shown in Figure 7 are fixed on four unitary gas sensitive layer array chips on the pedestal 2 by axle 5, and and pedestal 2 between stay the 2mm gap.Ultrasound wave spun gold ball hot welding press is nation's fixed electrode lead-in wire 6 between 6 binding posts on the array well heater positive electrode 7 on the array chip, test electrode 9,11,12,13 and public electrode and the pedestal 2.Make the gas sensitization array sensor of structure as shown in Figure 1.
(4) test.Gas sensitization array sensor is made energy consumption and gas sensitivity tests through 400 ℃ after aging 3 days.Fig. 9 is the equilibrium temperature and the energy consumption graph of a relation of gas sensitization array sensor example of the present invention, and energy consumption is the energy consumption of whole array, and temperature is the temperature in sensitive layer 8 zones; Figure 10 is the alcohol air-sensitive response curve of four unitary gas sensitization array sensors of the preferred embodiment of the present invention.
Embodiment two:
In embodiment one between the 9th, 11 test electrode of four cell arrays, increase the gas sensor array that a test electrode just can get Unit six between the 12nd, 13 test electrode respectively.Preparation process together
Embodiment one, gas sensor array substrate, heating film, electrode and sensitive layer material, sintering process such as table 1.Can obtain having the gas sensor array of Unit six of gas with various sensitivity characteristic.
Table 1: six unitary gas sensor array substrates, heating film, electrode and sensitive layer material, sintering process
| ? | Array substrate: aluminium nitride | Heating film: MoSi2 | Electrode: Pt |
| Gas sensor unit | The sensitive layer material | Sintering temperature | Sintering time (hour) |
| ?1? | SnO2 doping 0.1wt%Pt | 550℃? | 2.5? |
| ?2? | ZnO doping 10wt%WO3 | 650℃? | 2? |
| ?3? | SnO2 doping 7wt%Co2O3 | 700℃? | 2.5? |
| ?4? | ZnO doping 0.2wt%Pd | 600℃? | 2? |
| ?5? | ZnO doping 5wt%Al2O3 and 5wt%TiO2 | 650℃? | 3? |
| ?6? | ZnO doping 10wt%Ni | 700℃? | 2.5? |
The present invention not only is confined to the foregoing description, by between first, second test electrode and the 3rd, the 4th test electrode set up the test electrode of different numbers, and printing heating film and metal oxide sensitive layer, can obtain containing the gas sensor array of the gas sensor unit of any number more than 4.The material of each gas sensor unit can be identical or different, and persons skilled in the art can adopt other multiple specific implementation to implement the present invention according to content disclosed by the invention.
Claims (5)
1. gas sensitization array sensor, it is characterized in that: first, second test electrode (9,11) is positioned at same side, and the 3rd, the 4th test electrode (12,13) is positioned at same side, and they lay respectively on two relative limits of substrate (3); Array well heater positive electrode (7) and loop electrode (10) thereof lay respectively on other two relative limits of substrate (3); First, second test electrode (9,11) loop electrode (14) is positioned at first, second test electrode (9,11) between, the 3rd, the 4th test electrode (12,13) loop electrode (15) is positioned at the 3rd, the 4th test electrode (12,13) between, first, second test electrode (9,11) loop electrode (14) and first, second test electrode (9,11) parallel, the 3rd, the 4th test electrode (12,13) loop electrode (15) and the 3rd, the 4th test electrode (12,13) parallel, first, second test electrode (9,11) loop electrode (14), the loop electrode (10) and the 3rd of array well heater positive electrode (7), the 4th test electrode (12,13) loop electrode (15) is formed by connecting ' ㄈ ' shape as public electrode; On the substrate (3) between the loop electrode (10) of array well heater positive electrode (7) and array well heater positive electrode (7), be printed with heating film (4), on the substrate (3) between each test electrode public electrode corresponding, be printed with metal oxide sensitive layer (8) respectively with it, axle (5) is installed at the center of substrate (3), axle (5) passes heating film (4), and be fixed on the center of pedestal (2), leave the gap between substrate (3) and the pedestal (2); Also be provided with at least 6 binding posts (1) on the pedestal (2), be connected with each test electrode, array well heater positive electrode (7) and public electrode by contact conductor (6) respectively.
2. gas sensitization array sensor according to claim 1 is characterized in that: be respectively arranged with at least one test electrode between first, second test electrode (9,11) and between the 3rd, the 4th test electrode (12,13).
3. the preparation method of the described gas sensitization array sensor of claim 1, its step comprises:
(1) serigraphy array well heater positive electrode, first to the 4th test electrode and the public electrode on the substrate after the cleaning, substrate thickness be smaller or equal to 1 millimeter, and dry back was 700～850 ℃ of following sintering 5～20 minutes;
(2) serigraphy one deck heating film between heating of substrate device electrode and corresponding public electrode, dry back was 500～850 ℃ of following sintering 5～20 minutes;
(3) screen-printed metal oxide sensitive layer between test electrode and corresponding public electrode, dry back was at 500～850 ℃ of following sintering 1-4 hours;
(4) repeating step (3) prepares the metal oxide sensitive layer of each unit of array successively, obtains gas sensitization array;
(5) on the heating film of gas sensitization array, bore a hole;
(6) adopt axle substrate to be fixed on the pedestal by the hole of gas sensitization array, and fixed each contact conductor of nation, burin-in process makes gas sensitization array sensor.
4. method according to claim 3 is characterized in that: the material of heating film (4) is RuO
2, MoSi
2, W or Pt.
5. according to claim 3 or 4 described methods, it is characterized in that: the material of metal oxide sensitive layer (8) is ZnO, SnO
2Or Fe
2O
3, perhaps ZnO, SnO
2Or Fe
2O
3With arbitrary or several doping in following each component:
Pt?0.1wt％-3wt％，Pd?0.1wt％-3wt％，Ni?1wt％-30wt％，TiO
21wt％-30wt％，WO
31wt％-40wt％，Co
2O
31wt％-15wt％，V
2O
51wt％-30wt％，Al
2O
31wt％-20wt％，MnO
21wt％-30wt％。
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