CN101762623B - Semiconductor-type gas sensor with A1N heat isolation panel double-side micro structure and manufacturing method thereof - Google Patents
Semiconductor-type gas sensor with A1N heat isolation panel double-side micro structure and manufacturing method thereof Download PDFInfo
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- 238000010438 heat treatment Methods 0.000 claims abstract description 33
- 239000004065 semiconductor Substances 0.000 claims abstract description 11
- 239000000919 ceramic Substances 0.000 claims description 65
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 claims 6
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Abstract
一种AlN热隔离平板双面微结构的半导体式气体传感器及其制造方法，涉及一种自热隔离平板双面微结构气体传感器及其制造方法。解决了现有的Si材料的气体传感器存在工艺开发成本高、工艺复杂等问题。基片对角线的四个方位上刻蚀有热隔离槽，基片背面设置有加热电极和信号电极，通过通孔基片正面与背面的加热电极相连通，加热电极为蛇形排列结构，敏感膜附在信号电极上，制造方法如下：一选择基片；二传感器Pt金属薄膜信号电极制备：首先光刻，其次镀膜，最后金属膜剥离；三异面加热电极制备：首先镀膜，然后激光刻蚀；四热隔离；五退火；六附敏感膜。本发明可以作为半导体式Cl2、NOX、CO等气体传感器。
A semiconductor gas sensor with double-sided microstructure of AlN heat-isolated flat plate and a manufacturing method thereof, relating to a gas sensor with self-heating isolated flat double-sided microstructure and a manufacturing method thereof. The invention solves the problems of high process development cost, complex process and the like existing in the gas sensor of the existing Si material. There are thermal isolation grooves etched on the four directions of the diagonal of the substrate, and the heating electrodes and signal electrodes are arranged on the back of the substrate, and the front of the substrate is connected with the heating electrodes on the back through through holes. The sensitive film is attached to the signal electrode, and the manufacturing method is as follows: 1. Select the substrate; 2. Preparation of the signal electrode of the sensor Pt metal film: first, photolithography, second, coating, and finally peeling off the metal film; 3. Preparation of different-surface heating electrodes: first, coating, then laser Etching; four heat isolation; five annealing; six attached sensitive film. The invention can be used as a semiconductor gas sensor for Cl 2 , NO X , CO and the like.
Description
Technical field
The present invention relates to field of sensing technologies, be specifically related to a kind of self-heating and isolate panel double-side micro structure gas sensor and manufacturing approach thereof.
Background technology
At present; Semiconductor-type gas sensor both domestic and external is mainly used in and detects inflammable gas and toxic gas, is preventing to poison and combustion explosion plays a part to become more and more important; Semiconductor-type gas sensor is except gas detecting element; Also must dispose a well heater, be heated to required working temperature, present SnO with practicability to gas detecting element
2Inorganic semiconductor formula gas sensors such as system, zinc oxide series gas sensor generally need be heated to 300 ℃～500 ℃ just has gas-sensitive property; All need mix noble metal catalyst and improve its sensitivity and selectivity, thereby activity of such catalysts, life-span etc. are very big to the performance impact of element.So developed the organic semiconductor of low-temperature heat (150 ℃～room temperature) work again, but since natural organic semiconductor high resistance 10
-9More than the Ω, and the organic semi-conductor conductivity is always much lower than inorganic semiconductor, adopts interdigital electrode structure commonly used; Its resistance is quite big, is subject to disturb, and is unfavorable for the subsequent conditioning circuit signals collecting; Bring difficulty for acquired signal and subsequent conditioning circuit, limited its actual use.Therefore, to inorganic semiconductor formula gas sensor new thinking of development should be arranged.
The silicon coefficient of heat conductivity is 150W/mK in the time of 20 ℃, and heat conductivility is compared relatively poor with AlN, and the eighties in 20th century, aluminium nitride has higher heat-transfer capability as a kind of ceramics insulator, makes aluminium nitride be widely used in the microelectronics field.Different with beryllia is that aluminium nitride is nontoxic.Aluminium nitride is used metal treatment, can replace alumina and beryllia and be applied to a large amount of electronic devices.Aluminium nitride can prepare through the reducing action or the direct metal nitride aluminium of aluminium oxide and carbon.Aluminium nitride is a kind of material that links to each other with covalent bond, and it has the hex crystal structure, with zinc sulphide, wurtzite similar shape.AlN is highly stable in the hot environment of inertia, and in air, when temperature was higher than 700 ℃, the low-level oxidation effect can take place material surface, forms the sull of 5～10 nanometer thickness.
Along with the development of MEMS technology, substrate material performances such as non-silicon based ceramic, glass improve constantly, and are widely used in the Microstructure Sensor field, have wide application development prospect.
Summary of the invention
There are shortcomings such as heat conductivility is poor, process exploitation cost height, complex process in the present invention for the gas sensor that solves current material, propose a kind of semiconductor-type gas sensor and manufacturing approach thereof of AlN heat isolation panel double-side micro structure.
The semiconductor-type gas sensor of AlN heat isolation panel double-side micro structure; It comprises AlN ceramic substrate, two heating electrodes, front well heater, back heater, two signal electrodes, two signals collecting sheets, sensitive membrane and hot isolation channels; On cornerwise four orientation of said AlN ceramic substrate, be etched with hot isolation channel, hot isolation channel makes and respectively forms four isolated island convexities at AlN ceramic substrate front and back that the edge in four orientation of hot isolation channel, edge is etched with four through holes; AlN ceramic substrate front is provided with heating electrode, front well heater, signal electrode and signals collecting sheet; Heating electrode is applied in two through holes of AlN ceramic substrate one side, and signal electrode is applied in two other through hole, and the front well heater is the middle snakelike arrangement architecture that has breach; Two signals collecting sheets insert the middle breach of snakelike arrangement architecture of front well heater; The pin of signals collecting sheet is arranged in the hot isolation channel, and is connected with signal electrode, and two pins of front well heater are arranged in the hot isolation channel; And be connected with heating electrode 2; The part of inserting the snakelike arrangement architecture of heating electrode at the signals collecting sheet has sensitive membrane, and the back heater at the AlN ceramic substrate back side is snakelike arrangement architecture, and is arranged on the centre position at the AlN ceramic substrate back side; Two pins of back heater are arranged in the hot isolation channel, and are connected with heating electrode.
The manufacturing approach of the semiconductor-type gas sensor of AlN heat isolation panel double-side micro structure, concrete steps are following:
Step 2: sensor Pt metallic film signal electrode preparation, according to following sequentially built:
The end treating fluid that production order two a, the AlN ceramic substrate after step 1 handled are put into positive photoresist soaks 20～30min; Put into 150～180 ℃ of dryings of drying box again; Put into sol evenning machine gluing under 2500r/min～5000r/min speed again, put into baking oven then and dry 20～40min down at 80～100 ℃; With well heater pattern mask version is the plate-making figure, and 15～30s makes public on the double-sided exposure machine; Develop in the AlN ceramic substrate developer solution after the exposure 20～40s, rinsing 20～30s in the deionized water then; The AlN ceramic substrate that will scribble photoresist is at last put into drying box, toasts 30～40min under 100～120 ℃ of temperature;
Production order two b, the AlN ceramic substrate after production order two a are handled are put into many targets of ultrahigh vacuum sputter coating machine, and plated film adopts the platinum target, and purity is 99.99%, the size Φ 60 * 2.5mm of target; Plated film vacuum tightness reaches 10
-5During Pa, toward the logical argon gas of sputtering chamber, ar pressure is 1.5Pa, adopts d.c. sputtering, and sputtering power is 32W, and the time is 30min, and the flow of argon gas is 15～20ml/min;
Production order two c, the AlN ceramic substrate of plated film is put into acetone soln soak, the dissolving photoresist, and discontinuity is little ultrasonic, till metal pattern is clear;
Step 3: the preparation of antarafacial heating electrode, press following sequentially built:
Production order three a, the AlN ceramic substrate after step 2 handled are put into many targets of ultrahigh vacuum sputter coating machine, make pottery at AlN
Ceramic chip back side platinum plating film, plated film adopts the platinum target, and purity is 99.99%, the size Φ 60 * 2.5mm of target; Plated film vacuum tightness reaches 10
-5During Pa, toward the logical argon gas of sputtering chamber, ar pressure is 1.5Pa, adopts d.c. sputtering, and sputtering power is 32W, and the time is 30min, and the flow of argon gas is 15～20ml/min;
Production order three b, laser ablation goes out the grid heating electrode, etching power 1200～1500W, etch rate 0.2～0.5mm/s, resistance trimming size R on the AlN ceramic substrate of platinum plating film overleaf
0Be 25～30 Ω;
Step 4: with the AlN ceramic substrate laser ablation that step 3 was handled, 4 isolation channels of etching around AlN ceramic substrate heating electrode, laser ablation power 1500～1800W, etch rate 0.1～0.5mm/s;
Step 5: with 800～1000 ℃ of annealing of AlN ceramic substrate, the 2～3h after the step 4 processing;
Step 6: the AlN ceramic substrate after the step 5 processing is utilized silk-screen printing technique or coating process, on the gas microsensor, attach one deck gas sensitive material.
The AlN material has: (1) thermal conductivity high (about 270W/mK) near BeO and SiC, is Al
2O
3More than 5 times; (2) thermal expansivity (4.5 * 10
-6℃) and Si (3.5～4 * 10
-6℃) and GaAs (6 * 10
-6℃) coupling; (3) various electrical properties (specific inductive capacity, dielectric loss, body resistivity, dielectric strength) are good; (4) good mechanical property, rupture strength is higher than Al
2O
3With the BeO pottery, can be normal pressure-sintered; (5) purity is high; (6) light-transfer characteristic is good; (7) nontoxic; (8) can adopt casting technique to make.Be a kind of up-and-coming high power integrated circuit substrate and wrappage.Be mainly used in: do high-performance substrate material and encapsulating material in the products such as high density mixing circuit, microwave power device, power electronic devices, optoelectronic component, conductor refrigeration.AlN ceramic substrate 1 self is made electrode dielectric layer; Because the substrate coefficient of heat conductivity is high; Heating part and signals collecting partly adopt the antarafacial structure, scatter and disappear for preventing the temperature lateral transport, and AlN ceramic substrate 1 diagonal line four direction adopts hot isolation channel; Reduced the heating power consumption penalty, there is the problem of heat conductivility difference in the gas sensor that has solved current material.
The present invention adopts the AlN substrate to combine through lithography stripping technology and Laser Micro-Machining technology; Utilize the high thermoconductivity of AlN to adopt backside laser resistance trimming etching heating electrode; Utilize the hot isolation channel of laser scribing etching again, reduced the heating power consumption penalty, prepared a kind of semiconductor-type gas sensor of AlN heat isolation panel double-side micro structure; This gas sensor has Pt film temperature sensor, can carry out the temperature signal feedback; It is little, low in energy consumption that the semiconductor-type gas sensor of AlN heat isolation panel double-side micro structure of the present invention has a volume, and advantages such as technology is simple, the process exploitation cost is low, self-temperature compensating function can be used as semiconductor-type Cl
2, NO
X, gas sensor such as CO, have wide application development prospect.
Description of drawings
Fig. 1 is the semiconductor-type gas sensor Facad structure synoptic diagram of AlN heat isolation panel double-side micro structure.Fig. 2 is the semiconductor-type gas sensor structure synoptic diagram of AlN heat isolation panel double-side micro structure.
Embodiment
Embodiment one, combination Fig. 1 and Fig. 2 explain this embodiment; The semiconductor-type gas sensor of AlN heat isolation panel double-side micro structure; It comprises AlN ceramic substrate 1, two heating electrodes 2, front well heater 2-1, back heater 2-2, two signal electrodes 3, two signals collecting sheet 3-1, sensitive membrane 4 and hot isolation channels 5; On said AlN ceramic substrate 1 cornerwise four orientation, be etched with hot isolation channel 5, hot isolation channel 5 makes and respectively forms four isolated islands convexities 51 at AlN ceramic substrate 1 front and back that the edge in 5 four orientation of hot isolation channel, edge is etched with four through hole 1-1; AlN ceramic substrate 1 front is provided with heating electrode 2, front well heater 2-1, signal electrode 3 and signals collecting sheet 3-1; Heating electrode 2 is applied among two through hole 1-1 of AlN ceramic substrate 1 one sides, and signal electrode 3 is applied among two other through hole 1-1, and front well heater 21 is the middle snakelike arrangement architecture that has breach; Two signals collecting sheet 3-1 insert the middle breach of snakelike arrangement architecture of front well heater 2-1; The pin of signals collecting sheet 3-1 is arranged in the hot isolation channel 5, and is connected with signal electrode 3, and two pins of front well heater 2-1 are arranged in the hot isolation channel 5; And be connected with heating electrode 2; The part of inserting the snakelike arrangement architecture of heating electrode 2 at signals collecting sheet 3-1 has sensitive membrane 4, and the back heater 2-2 at AlN ceramic substrate 1 back side is snakelike arrangement architecture, and is arranged on the centre position at AlN ceramic substrate 1 back side; Two pins of back heater 2-2 are arranged in the hot isolation channel 5, and are connected with heating electrode 2.
Embodiment two, combination Fig. 1 and Fig. 2 explain this embodiment, and this embodiment is that with the difference of embodiment one AlN ceramic substrate 1 is square.
Embodiment three, combination Fig. 1 and Fig. 2 explain this embodiment, and this embodiment is that with embodiment one or two difference the length of side d of AlN ceramic substrate 1 is 3.1～3.3mm, and between adjacent two through hole 1-1 outer boundaries is 2.9～3.1mm apart from l; The protruding 5-1 of isolated island that is formed by hot isolation channel 5 is four isosceles trapezoids, wherein per two relative isosceles trapezoid congruences, and the upper base n1 of the protruding 5-1 isosceles trapezoid of a pair of isolated island is 0.45～0.55mm; The m1 that goes to the bottom is 1.35～1.45mm; High h1 is 0.25～0.35mm, and another upper base n2 to protruding 51 isosceles trapezoids of isolated island is 0.85～0.95mm, and the m2 that goes to the bottom is 1.55～1.65mm; High h2 is 0.45～0.55mm; The snakelike arrangement architecture length k of back heater 2-2 is 0.95～1.05mm, and spacing r is 0.045～0.055mm, and sensitive membrane 4 length e are 0.5～0.6mm; Width f is 0.2～0.25mm; The length p of the snakelike arrangement architecture of front well heater 2-1 is 1.04～1.06mm, and sensitive membrane 4 width f are less than the width of front well heater 2-1 central indentation, and through hole 1-1 is a square; Length of side w is 0.3～0.5mm, and what two signals collecting sheet 3-1 inserted barbed portion in the middle of the snakelike arrangement architecture of front well heater 2-1 is 0.09～0.11mm apart from s.
The manufacturing approach of the semiconductor-type gas sensor of embodiment four, AlN heat isolation panel double-side micro structure, concrete steps are following:
Step 2: sensor Pt metallic film signal electrode preparation, according to following sequentially built:
The end treating fluid that production order two a, the AlN ceramic substrate after step 1 handled are put into positive photoresist soaks 20～30min; Put into 150～180 ℃ of dryings of drying box again; Put into sol evenning machine gluing under 2500r/min～5000r/min speed again, put into baking oven then and dry 20～40min down at 80～100 ℃; With well heater pattern mask version is the plate-making figure, and 15～30s makes public on the double-sided exposure machine; Develop in the AlN ceramic substrate developer solution after the exposure 20～40s, rinsing 20～30s in the deionized water then; The AlN ceramic substrate that will scribble photoresist is at last put into drying box, toasts 30～40min under 100～120 ℃ of temperature;
Production order two b, the AlN ceramic substrate after production order two a are handled are put into many targets of ultrahigh vacuum sputter coating machine, and plated film adopts the platinum target, and purity is 99.99%, the size Φ 60 * 2.5mm of target; Plated film vacuum tightness reaches 10
-5During Pa, toward the logical argon gas of sputtering chamber, ar pressure is 1.5Pa, adopts d.c. sputtering, and sputtering power is 32W, and the time is 30min, and the flow of argon gas is 15～20ml/min;
Production order two c, the AlN ceramic substrate of plated film is put into acetone soln soak, the dissolving photoresist, and discontinuity is little ultrasonic, till metal pattern is clear;
Step 3: the preparation of antarafacial heating electrode, press following sequentially built:
Production order three a, the AlN ceramic substrate after step 2 handled are put into many targets of ultrahigh vacuum sputter coating machine, and at AlN ceramic substrate back side platinum plating film, plated film adopts the platinum target, and purity is 99.99%, the size Φ 60 * 2.5mm of target; Plated film vacuum tightness reaches 10
-5During Pa, toward the logical argon gas of sputtering chamber, ar pressure is 1.5Pa, adopts d.c. sputtering, and sputtering power is 32W, and the time is 30min, and the flow of argon gas is 15～20ml/min;
Production order three b, laser ablation goes out the grid heating electrode, etching power 1200～1500W, etch rate 0.2～0.5mm/s, resistance trimming size R on the AlN ceramic substrate of platinum plating film overleaf
0Be 25～30 Ω;
Step 4: with the AlN ceramic substrate laser ablation that step 3 was handled, 4 isolation channels of etching around AlN ceramic substrate heating electrode, laser ablation power 1500～1800W, etch rate 0.1～0.5mm/s;
Step 5: with 800～1000 ℃ of annealing of AlN ceramic substrate, the 2～3h after the step 4 processing;
Step 6: the AlN ceramic substrate after the step 5 processing is utilized silk-screen printing technique or coating process, on the gas microsensor, attach one deck gas sensitive material.
The AlN ceramic substrate that the AlN ceramic substrate that step 1 is chosen can adopt science and technology group 13 of China Electronics to be developed, thickness 0.3mm, thermal conductivity 180W/mk, surfaceness≤05 μ m; The thick more thermal loss of the AlN ceramic substrate of choosing is big more, and is thin more, and mechanical property is poor more; The big more heat conducting thermal loss of thermal conductivity is big more, and the more little thermal equilibrium of thermal conductivity is slow more; Surfaceness is big more, and the film continuity is poor more, and surfaceness membranelle adhesiveness more is poor more, is prone to come off.
Can adopt the end treating fluid of BP212 (CP45) the type positive photoresist that Beijing Ke Hua Microtronic A/S produces in the step 2 during production order two a pre-service formulas, the purpose of doing like this is the adhesiveness that increases photoresist; The desk-top drying box of DG/20-002A type that can adopt Chongqing milky way experimental apparatus company to produce when dry; The H52-10 type sol evenning machine that can adopt Yuhuan county Li An Electronics Equipment Co., Ltd to produce when sparing glue; Can adopt the SB-401B type double-sided exposure machine of CHINA ELECTRONICS TECHNOLOGY GROUP CORPORATION NO. 45 RESEARCH INSTITUTE's development during exposure; The BP212 developer solution that can adopt Beijing Ke Hua Microtronic A/S to produce during development;
Many targets of JGP560C type ultrahigh vacuum sputter coating machine that can adopt when production order b and production order three a plated films Shenyang science and technology instrument plant to produce in the step 2;
Adopt Beijing CW-4B of Hua Laiyin photoelectricity technology corporation, Ltd. laser scribing means in the step 3 during laser ablation of production order three b and step 4; Etching power and speed can be selected according to actual conditions, guarantee that the isolation channel etching thoroughly;
In the step 4 around the AlN ceramic substrate heating electrode 4 isolation channels of etching to obtain effect be to reduce the temperature cross conduction to scatter and disappear;
The effect of annealing in process is the continuity that improves film in the step 5, thereby has improved film resistance stability.
Claims (3)
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| CN102070118A (en) * | 2010-10-26 | 2011-05-25 | 南京工业大学 | Micro-heating plate for metal oxide semiconductor nano-thin film gas sensor |
| CN102731170A (en) * | 2011-04-06 | 2012-10-17 | 苏州鼎旺科技有限公司 | Technology for coating film on surface of ceramic substrate |
| CN102288644A (en) * | 2011-07-08 | 2011-12-21 | 中国科学院上海微系统与信息技术研究所 | Resistance gas sensor with four support cantilever beams and a four-layer structure and method |
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| CN103698359B (en) * | 2013-12-13 | 2016-06-15 | 苏州纳格光电科技有限公司 | Semiconductor gas sensor |
| JP6467173B2 (en) * | 2014-09-16 | 2019-02-06 | ヤマハファインテック株式会社 | Contact combustion type gas sensor |
| CN104698039A (en) * | 2015-03-26 | 2015-06-10 | 哈尔滨理工大学 | AlN ceramic substrate thermal insulation structure four-unit array gas sensor and manufacturing method thereof |
| KR101808239B1 (en) * | 2015-09-04 | 2017-12-13 | (주)포인트엔지니어링 | Micro heater and Micro sensor |
| TWI557527B (en) | 2015-12-28 | 2016-11-11 | 財團法人工業技術研究院 | Micro-electromechanical temperature control system with thermal reservoir |
| WO2018035468A1 (en) | 2016-08-18 | 2018-02-22 | Carrier Corporation | Isolated sensor and method of isolating a sensor |
| CN106053541B (en) * | 2016-08-25 | 2019-02-19 | 哈尔滨理工大学 | A kind of Al2O3-AlN ceramic micro-hot plate gas sensor with annular heater |
| CN108614015B (en) * | 2018-05-23 | 2020-11-13 | 哈尔滨工程大学 | Manufacturing method of catalysis and thermal conduction integrated gas sensor, sensor and working method |
| CN110182754B (en) * | 2019-05-17 | 2021-10-29 | 中国科学院上海微系统与信息技术研究所 | Micro-heater with enhanced micro-nano structure and preparation method thereof |
| CN111505210B (en) * | 2020-04-29 | 2021-07-27 | 华中科技大学 | A gas sensor chip integrated micromachining device |
-
2010
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