CN110988049A - Catalytic combustion type MEMS gas sensor and working method thereof - Google Patents
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Abstract
The invention relates to a catalytic MEMS gas sensor and a working method thereof. The first insulating support layer is arranged on the substrate, the resistance heating layer is arranged on the first insulating support layer, and the second insulating support layer covers the resistance heating layer; the temperature sensing electrode layer is arranged on the second insulating support layer, and the catalytic material layer is attached to the temperature sensing electrode layer and the upper part of the heating working area of the second insulating support layer; the microcontroller is disposed on the substrate. The method comprises the following steps: controlling the micro-controller to obtain the heating power and the heating temperature of the heating resistance layer and the temperature sensing electrode layer; controlling the working temperature of the resistance heating layer to be constant; the gas sensor periodically works at constant low temperature, constant medium temperature and constant high temperature. The catalytic combustion type MEMS gas sensor and the working method thereof have the advantages of quick response time, low power consumption and low cost.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a catalytic MEMS gas sensor and a working method thereof.
Background
Combustible gas is an important energy form as a chemical energy storage mode. Gas cookers and water heaters are widely used in household life; gasoline and diesel oil are still the main energy supply modes of automobiles at present, and hydrogen energy automobiles are probably the better scheme for solving the environmental pollution in the future. The gas leakage can cause serious fire, explosion and poisoning accidents. Gas leak detection has therefore spawned a great market demand for combustible gas sensors. In addition, in coal mining, combustible gas of mines and mine roads needs to be accurately monitored; in the petrochemical industry, petrochemical products generally have the characteristics of flammability and explosiveness, and the detection of the concentration of combustible gas is also needed. These require high quality combustible gas sensors that are fast in response and stable over time.
At present, the mature detection scheme of combustible gas is to enable the combustible gas to generate flameless combustion in a catalytic mode, and detect the concentration of the combustible gas by sensing the heat generated by combustion. As shown in fig. 1, specifically, a Pt coil 40 is generally used as a heating element, and a refractory material such as Al2O3 is wrapped around the Pt coil 40 to form a bead 50 as a temperature sensing element, the bead is impregnated with a catalyst to form an active sensing element 10, and both ends of the Pt coil 40 are connected to metal posts to realize temperature isolation. When the active sensing element 10 works, when a certain voltage is applied to the Pt coil 40 or a certain current is applied to the Pt coil 40, a high temperature of 350-. In practical use, in order to eliminate the interference of environmental temperature, humidity, air pressure, background gas thermal conductivity and other factors to the test, an inert compensation element 20 with the same structure without a catalyst is often added to form a bridge circuit to counteract the interference factors. Meanwhile, the high temperature generated during the operation of the sensor may cause ignition and explosion of the combustible gas, and it is necessary to dispose the above elements in the explosion-proof housing 30. The sensor structure has the following disadvantages in practical use: the temperature isolation structure has poor effect, which causes remarkable temperature rise of the sensor shell to the ambient temperature; the product has large size, large power consumption and poor anti-falling performance, and is difficult to apply to portable occasions; the working temperature is high, ignition and detonation are possible, and the safety is poor.
Disclosure of Invention
The invention provides a catalytic MEMS gas sensor and a working method thereof, aiming at the technical problems of poor temperature isolation structure and poor safety of a combustible gas detection sensor in the prior art.
The technical scheme for solving the technical problems is as follows:
a catalytic combustion type MEMS gas sensor comprises a substrate, a first insulating support layer, a resistance heating layer, a second insulating support layer, a temperature sensing electrode layer, a catalytic material layer and a microcontroller; the first insulating support layer is arranged on the substrate, the resistance heating layer is arranged on the first insulating support layer, and the second insulating support layer covers the resistance heating layer; the temperature sensing electrode layer is arranged on the second insulating support layer, and the catalytic material layer is attached to the temperature sensing electrode layer and the upper part of the heating working area of the second insulating support layer; the micro controller is arranged on the substrate and is electrically connected with the heating resistance layer and the temperature sensing electrode layer.
In the preferred scheme, the substrate is made of monocrystalline silicon, polycrystalline silicon, quartz, sapphire, yttrium oxide, porous anodic aluminum oxide or porous silicon.
In a preferred embodiment, the first insulating support layer and the second insulating support layer are made of silicon nitride, silicon oxide, or silicon oxynitride.
In the preferred scheme, the resistance heating layer is made of base metal, base metal alloy, doped monocrystalline silicon, doped polycrystalline silicon, conductive metal carbide, conductive metal nitride or conductive metal oxide.
In a preferred scheme, the substrate is made of doped monocrystalline silicon.
In a preferred embodiment, the temperature sensing electrode layer is made of Pt or Pt alloy material.
In a preferred scheme, the catalytic material layer adopts Si doped with one or more of noble metals Pd, Pt and Au3N4、SiO2Or Al2O3A material.
The invention also provides a working method of the catalytic combustion type MEMS gas sensor, which comprises the following steps:
controlling the micro controller to measure the resistance values of the heating resistance layer and the temperature sensing electrode layer, and obtaining the heating power and the heating temperature of the heating resistance layer and the temperature sensing electrode layer;
controlling the heating power of the resistance heating layer to realize constant working temperature; the gas sensor periodically works at constant low temperature, constant medium temperature and constant high temperature; the environmental factors are calibrated according to the heating power at constant low temperature, and the catalytic combustion effect is evaluated according to the heating power at constant medium temperature, so that the concentration of the combustible gas is obtained, and the combustible gas is rapidly ignited at constant high temperature.
In the preferable scheme, the operating temperature of the MEMS gas sensor is 100-600 ℃.
In the preferred scheme, the catalytic combustion type MEMS gas sensor periodically works at constant low temperature, constant medium temperature and constant high temperature; wherein, in a constant low temperature period, there are two or more constant medium temperature and constant high temperature periods.
The catalytic combustion type MEMS gas sensor and the working method thereof provided by the invention at least have the following beneficial effects or advantages:
the invention provides a catalytic combustion type MEMS gas sensor and a working method thereof.A microcontroller is controlled to measure the resistance values of a heating resistance layer and a temperature sensing electrode layer to obtain the heating power and the heating temperature of the heating resistance layer and the temperature sensing electrode layer; the working temperature is constant by controlling the heating power of the resistance heating layer; environmental factors are calibrated according to heating power at constant low temperature, and the catalytic combustion effect is evaluated according to the heating power at constant medium temperature, so that the concentration of combustible gas is obtained, and the combustible gas is rapidly ignited at constant high temperature. The defects in the prior art are overcome, the working temperature of the gas sensor can be accurately controlled, the concentration of combustible gas in the environment can be reliably evaluated, the sensor is quick in response time, low in power consumption and low in cost, and the method is suitable for batch production.
Drawings
FIG. 1 is a schematic diagram of a combustible gas detection sensor according to the prior art;
FIG. 2 is a schematic structural diagram of a catalytic combustion type MEMS gas sensor provided by an embodiment of the invention;
fig. 3 is a sectional view a-a of fig. 2.
In the drawings, the components represented by the respective reference numerals are listed below:
the sensor comprises a substrate 1, a substrate 2, a first insulating support layer 3, a resistance heating layer 4, a second insulating support layer 5, a temperature sensing electrode layer 5, a catalytic material layer 6, a microcontroller 7, an active sensing element 10, an inert compensation element 20, a resistance heating layer 30, a second insulating support layer 40 and a temperature sensing electrode layer 50.
Detailed Description
The invention provides a catalytic MEMS gas sensor and a working method thereof, aiming at the technical problems of poor temperature isolation effect and poor safety of a combustible gas detection sensor in the prior art.
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Referring to fig. 2 and 3, an embodiment of the present invention provides a catalytic combustion type MEMS gas sensor, which includes a substrate 1, a first insulating support layer 2, a resistance heating layer 3, a second insulating support layer 4, a temperature sensing electrode layer 5, a catalytic material layer 6, and a micro controller 7. A first insulating support layer 2 is arranged on the substrate 1, a resistance heating layer 3 is arranged on the first insulating support layer 2, and a second insulating support layer 4 covers the resistance heating layer 3; a temperature sensing electrode layer 5 is provided on the second insulating support layer 4 and a catalytic material layer 6 is attached to the temperature sensing electrode layer 5 and the upper part of the second insulating support layer 4 heating the working area. The micro-controller 7 is disposed on the substrate 1, and the micro-controller 7 is electrically connected to the heating resistor layer 3 and the temperature sensing electrode layer 5.
In the catalytic combustion type MEMS gas sensor provided in the embodiment of the present invention, the substrate 1 is made of monocrystalline silicon, polycrystalline silicon, quartz, sapphire, yttria, porous anodic aluminum oxide, or porous silicon.
The cost of the polycrystalline silicon is lower than that of monocrystalline silicon, and the process scheme and equipment of the polycrystalline silicon are similar to those of monocrystalline silicon, so that the cost of the MEMS substrate can be reduced. The thermal conductivity of the quartz is about 7.6W/mK, which is about 1/20 of the thermal conductivity of the Si substrate (about 150W/mK); the sapphire has a thermal conductivity of about 45W/mK, which is about 1/3 of that of the Si substrate; the thermal conductivity of yttrium oxide is about 5W/mK, which is about 1/30 of that of the Si substrate. Better temperature isolation can be achieved with quartz, sapphire, or yttria substrates. In addition to the above materials, porous materials can also be selected as substrates, such as anodized aluminum and porous silicon substrates, the thermal conductivity of air is only 0.01-0.04W/mK, and lower thermal conductivity can be achieved by selecting porous materials as substrates.
In the catalytic combustion type MEMS gas sensor provided in the embodiment of the present invention, the first insulating support layer 2 and the second insulating support layer 4 are made of silicon nitride, silicon oxide, or silicon oxynitride.
The silicon nitride insulating film supporting layer formed by the chemical vapor deposition process has high mechanical strength and can bear thermal stress caused by high-temperature work of the MEMS. The silicon oxide film formed by the chemical vapor deposition process has a low thermal conductivity coefficient, and can realize better temperature isolation. The silicon oxynitride film formed by the chemical vapor deposition process can be used for adjusting the mechanical property, the thermal conductivity coefficient and the film stress of the film, and a highly reliable MEMS micro hot plate structure is realized.
In the catalytic combustion type MEMS gas sensor provided by the embodiment of the invention, the resistance heating layer 3 is made of base metal, base metal alloy, doped monocrystalline silicon, doped polycrystalline silicon, conductive metal carbide, conductive metal nitride or conductive metal oxide. The material of the substrate 1 is doped monocrystalline silicon.
The material of the resistance heating layer adopts base metals such as Ti, W and the like and base metal alloys, so that the cost of the electrode material can be reduced, and the traditional CMOS process is better compatible. The resistance heating layer is made of doped monocrystalline silicon and doped polycrystalline silicon, so that the mismatch of thermal expansion coefficients between the resistance heating layer and the film supporting layer can be reduced, the material cost is reduced, and the traditional CMOS process is better compatible. The resistance heating layer is made of proper conductive metal carbide, conductive metal nitride or conductive metal oxide, so that the mismatch of thermal expansion coefficients between the resistance heating layer and the film supporting layer can be reduced, the high-temperature resistance of the MEMS micro-heating plate is improved, and the material cost is reduced.
According to the catalytic combustion type MEMS gas sensor provided by the embodiment of the invention, the temperature sensing electrode layer 5 is made of Pt or a Pt alloy material. The catalytic material layer 6 adopts Si doped with one or more of noble metals Pd, Pt and Au3N4、SiO2Or Al2O3A material.
The Pt or Pt alloy material has a larger positive temperature coefficient, and can realize high-precision micro-heating plate working temperature measurement. One or more doped catalytic combustion materials in noble metals Pd, Pt and Au are adopted, so that the ignition point of combustible gas can be effectively reduced, and the working temperature of the gas sensor is reduced. The catalytic combustion carrier material adopts Si3N4、SiO2Or Al2O3The material is better compatible with the film supporting layer, and a more reliable device structure is realized.
Example two
Referring to fig. 2 and fig. 3, an embodiment of the present invention provides a method for operating a catalytic combustion type MEMS gas sensor, wherein the operating temperature of the MEMS gas sensor is 100-. The method comprises the following steps:
step S10, the control microcontroller 7 measures the resistance values of the heating resistor layer 3 and the temperature sensing electrode layer 5, and obtains the heating powers and heating temperatures of the heating resistor layer 3 and the temperature sensing electrode layer 5.
Wherein, resistance value of resistance zone of heating 3 is Rh, and mains voltage is VCC, adopts PWM mode control heating power, and PWM Duty cycle is D, and then heating power P is:
P＝D*VCC/Rh2；
the resistance of the temperature sensing electrode layer is Rs, the temperature coefficient of the temperature sensing electrode material is K, the resistance of the temperature sensing electrode layer at 25 ℃ is Rs0, and the working temperature T of the micro hot plate is as follows:
T＝25+(Rs-R0)/K。
step S20, controlling the heating power of the resistance heating layer 3 to realize constant working temperature; controlling the catalytic combustion type MEMS gas sensor to periodically work at a constant low temperature, a constant medium temperature and a constant high temperature; calibrating the environmental factors according to the heating power at a constant low temperature; evaluating the catalytic combustion effect according to the heating power at a constant intermediate temperature, and further obtaining the concentration of the combustible gas; the combustible gas can be quickly ignited at constant high temperature.
Wherein the target working temperature is TtargetThe current detected temperature sensing electrode temperature is T, such as T<TtargetIncreasing the PWM Duty ratio Duty, and periodically detecting the temperature T of the temperature sensing electrode again until T is equal to TtargetOr less than a target deviation; such as T>TtargetThen, the PWM Duty ratio Duty is reduced, and the temperature sensing electrode temperature T is periodically detected again until T is equal to TtargetOr less than the target deviation. By periodically detecting the temperature T of the temperature sensing electrode, the PWM Duty ratio Duty is adjusted in real time to make up for the working temperature deviation caused by the environmental temperature factor, the background gas thermal conductivity reason and the catalytic combustion effect, and the working temperature is constant.
Wherein, low temperature, medium temperature and high temperature refer to: the gas-sensitive resistor of the catalytic material has no obvious catalytic combustion effect on combustible gas at low temperature; the catalytic material has catalytic combustion effect on combustible gas at medium temperature, but the temperature is lower than the ignition temperature, and the ignition speed is slow; the catalytic material has obvious catalytic combustion effect on combustible gas at high temperature, the temperature is close to the ignition point, and the ignition speed is high.
The catalytic combustion type MEMS gas sensor periodically works at constant low temperature, constant medium temperature and constant high temperature; wherein, in a constant low temperature period, there are two or more constant medium temperature and constant high temperature periods.
For example, the catalytic combustion type MEMS gas sensor operates at a constant low temperature of 100 ℃, a constant medium temperature of 350 ℃, and a constant high temperature of 500 ℃. For example, cycling at three temperatures is as follows:
(1) the heating power was measured at a constant temperature of 100 c for 2 seconds and at 1.8 seconds, and the effect of environmental factors on the heating power was calibrated. (2) The heating power is tested at the constant 350 ℃ for 0.9 second and 0.5 second, and the influence of the catalytic combustion effect on the heating power is calculated. (3) Working for 0.1 second at constant 500 ℃ to accelerate the ignition of combustible gas; (4) repeating the steps (2) and (3) for 7 times; (5) and (4) circulating the steps (1) to (4).
The catalytic combustion type MEMS gas sensor and the working method thereof provided by the embodiment of the invention at least have the following beneficial effects or advantages:
according to the catalytic combustion type MEMS gas sensor and the working method thereof provided by the embodiment of the invention, the resistance values of the heating resistance layer and the temperature sensing electrode layer are measured by controlling the micro controller, so that the heating power and the heating temperature of the heating resistance layer and the temperature sensing electrode layer are obtained; the working temperature is constant by controlling the heating power of the resistance heating layer; environmental factors are calibrated according to heating power at constant low temperature, and the catalytic combustion effect is evaluated according to the heating power at constant medium temperature, so that the concentration of combustible gas is obtained, and the combustible gas is rapidly ignited at constant high temperature. The defects in the prior art are overcome, the working temperature of the gas sensor can be accurately controlled, the concentration of combustible gas in the environment can be reliably evaluated, the sensor is quick in response time, low in power consumption and low in cost, and the method is suitable for batch production.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A catalytic combustion type MEMS gas sensor is characterized by comprising a substrate (1), a first insulating support layer (2), a resistance heating layer (3), a second insulating support layer (4), a temperature sensing electrode layer (5), a catalytic material layer (6) and a microcontroller (7); the first insulating support layer (2) is arranged on the substrate (1), the resistance heating layer is arranged (3) on the first insulating support layer (2), and the second insulating support layer (4) covers the resistance heating layer (3); the temperature sensing electrode layer (5) is arranged on the second insulating support layer (4), and the catalytic material layer (6) is attached to the temperature sensing electrode layer (5) and the upper part of the heating working area of the second insulating support layer (4); the micro controller (7) is arranged on the substrate (1), and the micro controller (7) is electrically connected with the heating resistance layer (3) and the temperature sensing electrode layer (5).
2. The catalytic combustion MEMS gas sensor according to claim 1, characterized in that the material of the substrate (1) is monocrystalline silicon, polycrystalline silicon, quartz, sapphire, yttria, porous anodic alumina or porous silicon.
3. The catalytic combustion MEMS gas sensor according to claim 1, wherein the material of the first and second insulating support layers (2, 4) is silicon nitride, silicon oxide or silicon oxynitride.
4. The catalytic combustion MEMS gas sensor according to claim 1, characterized in that the material of the resistive heating layer (3) is a base metal, a base metal alloy, doped monocrystalline silicon, doped polycrystalline silicon, a conductive metal carbide, a conductive metal nitride or a conductive metal oxide.
5. The catalytic combustion MEMS gas sensor according to claim 1, characterized in that the material of the substrate (1) is doped monocrystalline silicon.
6. The catalytic combustion MEMS gas sensor according to claim 1, characterized in that the temperature sensing electrode layer (5) is of Pt or Pt alloy material.
7. Catalytic combustion MEMS gas sensor according to claim 1, characterized in that the catalytic material layer (6) is Si doped with one or more of the noble metals Pd, Pt, Au3N4、SiO2Or Al2O3A material.
8. A working method of a catalytic combustion type MEMS gas sensor is characterized by comprising the following steps:
controlling the micro controller (7) to measure the resistance values of the heating resistance layer (3) and the temperature sensing electrode layer (5), and obtaining the heating power and the heating temperature of the heating resistance layer (3) and the temperature sensing electrode layer (5);
the heating power of the resistance heating layer (3) is controlled to realize constant working temperature; controlling the catalytic combustion type MEMS gas sensor to periodically work at constant low temperature, constant medium temperature and constant high temperature; calibrating the environmental factors according to the heating power at a constant low temperature; evaluating the catalytic combustion effect according to the heating power at a constant intermediate temperature, and further obtaining the concentration of the combustible gas; the combustible gas can be quickly ignited at constant high temperature.
9. The operating method of the catalytic combustion type MEMS gas sensor as claimed in claim 8, wherein the operating temperature of the MEMS gas sensor is 100-600 ℃.
10. The operating method of the catalytic combustion MEMS gas sensor as claimed in claim 8, wherein the catalytic combustion MEMS gas sensor periodically operates at a constant low temperature, a constant medium temperature, a constant high temperature; wherein, in a constant low temperature period, there are two or more constant medium temperature and constant high temperature periods.
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Cited By (2)
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| CN111610233A (en) * | 2020-06-16 | 2020-09-01 | 黑龙江省网络空间研究中心 | Preparation method of MEMS catalytic combustion type gas sensor |
| CN114018990A (en) * | 2022-01-06 | 2022-02-08 | 武汉微纳传感技术有限公司 | Multi-mode working MEMS gas sensor and working method thereof |
Citations (12)
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