CN212008403U - Hydrogen sensor and detection system thereof - Google Patents
Hydrogen sensor and detection system thereof Download PDFInfo
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- CN212008403U CN212008403U CN202020455829.1U CN202020455829U CN212008403U CN 212008403 U CN212008403 U CN 212008403U CN 202020455829 U CN202020455829 U CN 202020455829U CN 212008403 U CN212008403 U CN 212008403U
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Abstract
The utility model discloses a hydrogen sensor and detecting system thereof, hydrogen sensor, it includes: the device comprises a substrate, wherein an isolation region is arranged in the middle of the substrate and divides the substrate into a first electrode region and a second electrode region; the surface of the first electrode area is sputtered with a platinum film layer, the surface of the second electrode area is sputtered with a tungsten film layer, the isolation area is provided with an electrolyte mixture layer, and the platinum film layer is connected with the tungsten film layer through the electrolyte mixture layer. Compared with the prior art, the device has the advantages of wide working temperature range, good humidity adaptation, fast response time, high detection precision, wide detection concentration range, safety, no toxicity and low power consumption.
Description
Technical Field
The utility model relates to a hydrogen detects technical field, especially relates to a hydrogen sensor and detecting system thereof.
Background
At present, hydrogen is increasingly applied to various industries as a natural, completely clean and green energy source, particularly hydrogen fuel electric vehicles, but the hydrogen has the inherent characteristics: the concentration of the leaked gas in the air reaches a certain degree, and the gas easily explodes when meeting a fire source under the standard air pressure. It is very necessary to rapidly detect whether hydrogen gas leaks.
As in the Chinese patent: CN200780018403 discloses a hydrogen sensor in which a thin layer (made of a silicon-containing compound, a fluorinated compound, or a fat) is formed on the surface of a substrate such as a resin, and a catalyst layer (platinum or palladium) is further formed on the surface of the thin layer. When the catalyst layer comes into contact with the leaked hydrogen gas, the catalyst layer rapidly hydrogenates the thin film layer and changes the light reflectance of the thin film layer.
The sensor is characterized in that: forming the protective film on the surface of the catalyst layer prevents the catalyst layer from absorbing moisture or oxygen in the environment, thereby preventing deterioration of the protective film and the catalyst layer from lowering the influence of water by the water-repellent layer.
In addition, Chinese patents are available: CN201110335970 discloses a three-electrode solid electrolyte hydrogen sensor and a hydrogen concentration measuring method using the same, the sensor is a solid electrolyte hydrogen sensor, and solves the problem of low hydrogen concentration detection accuracy of the existing solid electrolyte hydrogen sensor, the sensor comprises 3 electrodes, the distances of the three electrodes are equal, one of the three electrodes is a reference electrode, and the electromotive forces E1 and E2 of the other 2 electrodes relative to the reference electrode are compared to calculate the hydrogen concentration, so as to improve the detection accuracy.
However, the existing hydrogen sensors all have the following disadvantages: the working temperature range is narrow, the adaptability of the humidity range is poor, the hydrogen concentration can not be linearly and quantitatively detected, the falling resistance and the vibration resistance are poor, and the requirements of vehicle specifications can not be met.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to overcome prior art not enough, provide a hydrogen sensor and detecting system thereof, it has solved among the prior art internet education electronic product and has experienced poor technical problem.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
in a first aspect, an embodiment of the present invention provides a hydrogen sensor, which includes: the device comprises a substrate, wherein an isolation region is arranged in the middle of the substrate and divides the substrate into a first electrode region and a second electrode region; the surface of the first electrode area is sputtered with a platinum film layer, the surface of the second electrode area is sputtered with a tungsten film layer, the isolation area is provided with an electrolyte mixture layer, and the platinum film layer is connected with the tungsten film layer through the electrolyte mixture layer.
Wherein, the thickness of the platinum film layer is 100-500 mm.
Wherein the thickness of the tungsten film layer is 100-500 mm.
Wherein, the substrate is an alumina or ceramic substrate.
Wherein the thickness of the electrolyte mixture layer is 0.5-1 mm.
The first electrode area and the second electrode area are both provided with a pad, a contact pin is arranged on the pad, and nickel is plated on the surface of the contact pin.
In a second aspect, an embodiment of the present invention provides a hydrogen detection system, which includes: the hydrogen sensor comprises a control and algorithm processing unit, an operational amplification processing unit electrically connected with the control and algorithm processing unit, a hydrogen sensor connected with the operational amplification processing unit, and a power conversion unit, wherein the power conversion unit converts external voltage into 5V voltage and supplies the voltage to the control and algorithm processing unit, the operational amplification processing unit and the hydrogen sensor; the operation amplification processing unit amplifies the electric signal of the hydrogen concentration detected by the hydrogen sensor, and the control and algorithm processing unit performs operation processing on the transmitted amplified signal to obtain the detected hydrogen concentration value.
The control and algorithm processing unit is electrically connected with a temperature sensor and a humidity sensor, the temperature sensor is used for detecting the temperature of the hydrogen concentration environment to be detected, the humidity sensor is used for detecting the humidity of the hydrogen concentration environment to be detected, and the control and algorithm processing unit compensates data detected by the hydrogen sensor according to the humidity and the temperature of the detection environment.
In a third aspect, an embodiment of the present invention provides a method for manufacturing a hydrogen sensor, including the following steps:
dividing the aluminum oxide or ceramic substrate into an isolation region, a first electrode region and a second electrode region, wherein the isolation region divides the aluminum oxide or ceramic substrate into the first electrode region and the second electrode region;
sputtering a platinum film layer on the first electrode area and a tungsten film layer on the second electrode area by adopting a sputtering method;
coating the electrolyte mixture on the isolation area to form an electrolyte mixture layer, and tightly pressing the electrolyte mixture layer by using a Teflon rod so that the electrolyte mixture is tightly attached to the surface of the substrate, wherein two sides of the electrolyte mixture layer are respectively connected to the platinum film layer of the first electrode area and the tungsten film layer of the second electrode area;
and drying the alumina or ceramic substrate coated with the electrolyte mixture layer at high temperature to form the ceramic substrate.
The method comprises the following steps of coating an electrolyte mixture on an isolation region to form an electrolyte mixture layer, and tightly pressing the electrolyte mixture layer by using a Teflon rod so that the electrolyte mixture is tightly attached to the surface of a substrate, wherein the electrolyte mixture is a uniform electrolyte mixture prepared by uniformly mixing Kafft AB glue and Nafion according to the mass components of 1:3 in the step that two sides of the electrolyte mixture layer are respectively connected to a platinum film layer of a first electrode region and a tungsten film layer of a second electrode region; or a mixture of phosphotungstic acid or cesium phosphotungstate and KE-1024 which are uniformly mixed according to the mass component ratio of 3:1 is adopted.
Compared with the prior art, the utility model discloses a hydrogen sensor and detecting system thereof, operating temperature range is wide, and humidity adaptation is good, and response time is fast, detects the precision height, and detection concentration range is wide, and is safe, nontoxic, and the consumption is little.
The foregoing is a summary of the present invention, and other objects, features and advantages of the present invention will be apparent from the following detailed description of the preferred embodiments, which is provided for the purpose of illustration and understanding of the present invention.
Drawings
Fig. 1 is a schematic structural diagram of the hydrogen sensor of the present invention.
Fig. 2 is a functional block diagram of the hydrogen gas detection system of the present invention.
Fig. 3 is a flow chart of a manufacturing method of the hydrogen sensor of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention will be described in further detail with reference to the accompanying drawings and the following detailed description.
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 some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by those skilled in the art without creative efforts belong to the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and to simplify the description, but do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the present invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "secured" are to be construed broadly and can, for example, be connected or detachably connected or integrated; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.
In the present disclosure, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may comprise direct contact between the first and second features, or may comprise contact between the first and second features not directly. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above should not be understood to necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples described in this specification can be combined and combined by one skilled in the art.
Referring to fig. 1, in the present embodiment, an embodiment of the present invention provides a hydrogen sensor, which includes: the substrate comprises a substrate 10, wherein an isolation region 12 is arranged in the middle of the substrate 10, and the isolation region 12 divides the substrate 10 into a first electrode region 11 and a second electrode region 13; the first electrode region 11 has a platinum film layer sputtered on the surface, the second electrode region 13 has a tungsten film layer sputtered on the surface, the isolation region 12 is provided with an electrolyte mixture layer 14, and the electrolyte mixture layer 14 connects the platinum film layer of the first electrode region 11 with the tungsten film layer of the second electrode region 13. Specifically, the first electrode region 11 sputtered with the platinum film layer is an anode, and the second electrode region 13 sputtered with the tungsten film layer is a cathode. Wherein, the platinum film sputtered on the first electrode region 11 can be replaced by a palladium film.
Wherein, the substrate 10 is an alumina or ceramic substrate.
Specifically, the thickness of the platinum film layer is 100-500 mm. The purity of the sputtered platinum is more than 99.98%, and the thickness of the tungsten film layer is 100-500 mm. The thickness of the platinum film layer and the tungsten film layer sputtered on the same hydrogen sensor is the same.
Wherein the thickness of the electrolyte mixture layer 14 is 0.5 to 1mm, a thickness uniformity error of +/-0.1mm, preferably 1mm, is required, and the electrolyte mixture is tightly adhered to the surface of the electrode by compressing with a teflon rod. The preparation process of the electrolyte mixture comprises the following steps:
firstly, wetting Nafion (perfluorosulfonic acid resin) thoroughly with 70% alcohol, and uniformly stirring;
then, the Carftt AB glue as a curing agent and Nafion were mixed and stirred uniformly in a ratio of 1:3 to form an electrolyte mixture.
Of course, the Nafion can also be replaced with h3o40pw12.xh2o (phosphotungstic acid) or CS2.5H0.5PW12P40 (cesium phosphotungstate). The curative Kafter AB glue may be replaced with KE-1024 (A/B).
The first electrode area and the second electrode area are both provided with a pad, a contact pin is arranged on the pad, and nickel is plated on the surface of the contact pin.
In a second aspect, referring to fig. 2, an embodiment of the present invention provides a hydrogen detection system, which includes: a control and algorithm processing unit 1, an operational amplification processing unit 5 electrically connected to the control and algorithm processing unit 1, a hydrogen sensor 6 connected to the operational amplification processing unit 5, and a power conversion unit 2, wherein the power conversion unit 2 converts an external voltage into a 5V voltage and supplies the 5V voltage to the control and algorithm processing unit 1, the operational amplification processing unit 5 and the hydrogen sensor 6; the operation amplification processing unit 5 amplifies the electrical signal of the hydrogen concentration detected by the hydrogen sensor 6, and the control and algorithm processing unit 1 performs operation processing on the transmitted amplified signal to obtain the detected hydrogen concentration value.
Further, the control and algorithm processing unit 1 is also electrically connected with a temperature sensor 3 and a humidity sensor 4, the temperature sensor 3 is used for detecting the temperature of the environment to be detected with the hydrogen concentration, the humidity sensor 4 is used for detecting the humidity of the environment to be detected with the hydrogen concentration, and the control and algorithm processing unit 1 compensates data detected by the hydrogen sensor according to the humidity and the temperature of the detection environment. In order to transmit the detected hydrogen concentration signal to an external system, the control and algorithm processing unit 1 is also electrically connected with a LIN/CAN bus unit 7, as shown in the figure: the external interface is a 4PIN connector, PWR + is a positive power supply, SIG + and SIG-are CANH and CANL of a CAN communication bus or SIG + are LIN buses, and PWR-is a power ground.
The hydrogen sensor 6 is the most critical module of the system, and is used for sensing the concentration of hydrogen, and the concentration is in direct proportion to the electromotive force variation of the hydrogen; when the hydrogen concentration is high, the output electromotive force variation is fast, the output electromotive force variation is small when the hydrogen concentration is low, and the response is slow. The operational amplification processing unit 5 receives the potential signal of the hydrogen sensor 6 for processing and sends the potential signal to the control and algorithm processing unit 1 for algorithm processing, so that the concentration and the voltage are in a linear ratio relationship. The LIN/CAN bus unit 7 sends the signals processed by the control and algorithm processing unit 1 to an external system through a bus to give an alarm or prompt. The temperature sensor 3 and the humidity sensor 4 collect temperature and humidity information and send the information to the control and algorithm processing unit 1, and the control and algorithm processing unit carries out temperature and humidity compensation on the hydrogen sensor 6 through related algorithms. The functions of the temperature sensor 3 and the humidity sensor 4 can also be realized by other similar temperature and humidity sensor modules outside the system. The temperature sensor 3 and the humidity sensor 4 are also powered by the power conversion unit 2.
Because the probe of the system generates electric potential, external power supply is not needed, the power consumption of the system is very small, only the single chip microcomputer and the temperature and humidity sensor are used for supplying power, and when the system is in a dormant state, the power consumption is 0.05 milliampere; when the system needs to work, the system is awakened through the external bus. The control and algorithm processing unit 1 adopts multi-model single-chip microcomputers such as MCU.
The temperature and humidity compensation correction method for the hydrogen sensor 6 is as follows:
reference voltage: calibration of the reference potential was performed with nitrogen mixing in a 0% hydrogen environment; since the potential of hydrogen fluctuates by about 1V, the circuit needs to give a bias voltage, which is greater than 1V, to avoid negative voltage.
The initial electromotive force of hydrogen in air (humidity 45%, temperature 25 ℃) was recorded as the sub-reference Ei.
Placing the sensor in a high-temperature and low-temperature box, adjusting the temperature to be in the range of-40 ℃ to 85 ℃, adjusting once every 10 ℃, and recording the corresponding potential value of each time, wherein the potential value corresponding to the group of temperatures is Xn; the effect of temperature on the potential is: Ei-Xn.
Similarly, the sensor is placed in a humidity box, the humidity is adjusted to be 0% to 100%, the corresponding potential value is recorded every 5%, and the potential value corresponding to one group of humidity is Yn; the effect of humidity on the potential is Ei-Yn;
all the values are made into EEPROM of single chip, and when the actual environment temperature and humidity can be compensated by table lookup according to these values.
In a third aspect, referring to fig. 3, an embodiment of the present invention provides a method for manufacturing a hydrogen sensor, including the following steps:
step S100, dividing the aluminum oxide or ceramic substrate into an isolation region, a first electrode region and a second electrode region, wherein the isolation region divides the aluminum oxide or ceramic substrate into the first electrode region and the second electrode region; in the present embodiment, as shown: the isolation region 12 is a rectangular region with a size of 1 × 6.2mm, and the first electrode region 11 and the second electrode region 13 divided by the isolation region 12 are both rectangular regions with a size of 2.6 × 6.2 mm. The circular area is the area of the electrolyte mixture layer 14.
Step S200, sputtering a platinum film layer on the first electrode area and a tungsten film layer on the second electrode area by adopting a sputtering method; the thickness of the platinum film layer is 100-500 mm. The purity of the sputtered platinum is more than 99.98%, and the thickness of the tungsten film layer is 100-500 mm. The thickness of the platinum film layer and the tungsten film layer sputtered on the same hydrogen sensor is the same.
Step S300, coating the electrolyte mixture on an isolation area to form an electrolyte mixture layer, and tightly pressing the electrolyte mixture layer by using a Teflon rod so that the electrolyte mixture is tightly attached to the surface of the substrate, wherein two sides of the electrolyte mixture layer are respectively connected to the platinum film layer of the first electrode area and the tungsten film layer of the second electrode area; the electrolyte mixture layer 14 has a thickness of 0.5 to 1mm, requires a thickness uniformity error of +/-0.1mm, preferably 1mm, and is compressed with a teflon rod so that the electrolyte mixture is closely attached to the electrode surface.
And S400, drying the alumina or ceramic substrate coated with the electrolyte mixture layer at high temperature to form the aluminum or ceramic substrate. In this embodiment, drying is performed at a high temperature of 100 ℃ for one hour, and then the product is cooled in a normal temperature environment for 30 minutes, and then the product can be molded for use.
The method comprises the following steps of coating an electrolyte mixture on an isolation region to form an electrolyte mixture layer, and tightly pressing the electrolyte mixture layer by using a Teflon rod so that the electrolyte mixture is tightly attached to the surface of a substrate, wherein the electrolyte mixture is a uniform electrolyte mixture prepared by uniformly mixing Kafft AB glue and Nafion according to the mass components of 1:3 in the step that two sides of the electrolyte mixture layer are respectively connected to a platinum film layer of a first electrode region and a tungsten film layer of a second electrode region; or a mixture of phosphotungstic acid or cesium phosphotungstate and KE-1024 which are uniformly mixed according to the mass component ratio of 3:1 is adopted.
The preparation method of the electrolyte mixed solution comprises the following steps:
firstly, wetting Nafion thoroughly with 70% alcohol, and stirring uniformly;
and secondly, mixing and stirring the Kaftet AB glue and Nafion uniformly according to the ratio of 1:3 to form an electrolyte mixture.
As a sensor for detecting hydrogen leakage, the probe of the hydrogen sensor aims at a hydrogen leakage port, and the closer the probe is, the better the probe is, so that the hydrogen concentration can be quickly detected in response to alarm in time;
if test hydrogen concentration in the closed container, for example, the concentration in the hydrogen tank, then need make this product aim at the gas outlet for the H2 probe and the complete seamless connection of gas outlet of this product, thereby avoid outside air's interference, and then guarantee to detect the precision.
Compared with the prior art, the hydrogen sensor and the detection system thereof have the advantages of wide working temperature range, good humidity adaptation, fast response time, high detection precision, wide detection concentration range, safety, no toxicity and low power consumption.
The technical content of the present invention is further described by the embodiments only, so that the reader can understand it more easily, but the embodiments of the present invention are not limited thereto, and any technical extension or re-creation according to the present invention is protected by the present invention. The protection scope of the present invention is subject to the claims.
Claims (8)
1. A hydrogen gas sensor, comprising: the device comprises a substrate, wherein an isolation region is arranged in the middle of the substrate and divides the substrate into a first electrode region and a second electrode region; the surface of the first electrode area is sputtered with a platinum film layer, the surface of the second electrode area is sputtered with a tungsten film layer, the isolation area is provided with an electrolyte mixture layer, and the platinum film layer is connected with the tungsten film layer through the electrolyte mixture layer.
2. The hydrogen sensor according to claim 1, wherein the thickness of the platinum film layer is 100-500 mm.
3. The hydrogen sensor according to claim 1, wherein the thickness of the tungsten film layer is 100-500 mm.
4. A hydrogen sensor according to claim 1, characterized in that the substrate is an alumina or ceramic substrate.
5. The hydrogen sensor according to claim 1, wherein the thickness of the electrolyte mixture layer is 0.5 to 1 mm.
6. The hydrogen sensor according to claim 1, wherein the first electrode region and the second electrode region are provided with a pad, the pad is provided with a pin, and the surface of the pin is plated with nickel.
7. A hydrogen gas detection system, comprising: a control and algorithm processing unit, an operational amplification processing unit electrically connected to the control and algorithm processing unit, the hydrogen sensor according to any one of claims 1 to 6 connected to the operational amplification processing unit, and a power conversion unit converting an external voltage into a voltage of 5V to be supplied to the control and algorithm processing unit, the operational amplification processing unit, and the hydrogen sensor; the operation amplification processing unit amplifies the electric signal of the hydrogen concentration detected by the hydrogen sensor, and the control and algorithm processing unit performs operation processing on the transmitted amplified signal to obtain the detected hydrogen concentration value.
8. The hydrogen detection system according to claim 7, wherein the control and algorithm processing unit is further electrically connected with a temperature sensor and a humidity sensor, the temperature sensor is used for detecting the temperature of the environment in which the hydrogen concentration is to be detected, the humidity sensor is used for detecting the humidity of the environment in which the hydrogen concentration is to be detected, and the control and algorithm processing unit compensates data detected by the hydrogen sensor according to the humidity and the temperature of the detection environment.
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