CN115165813A - Monolithic integrated optical excitation gas sensor and preparation method thereof - Google Patents
Monolithic integrated optical excitation gas sensor and preparation method thereof Download PDFInfo
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- CN115165813A CN115165813A CN202210674644.3A CN202210674644A CN115165813A CN 115165813 A CN115165813 A CN 115165813A CN 202210674644 A CN202210674644 A CN 202210674644A CN 115165813 A CN115165813 A CN 115165813A
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
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Abstract
The invention relates to a monolithically integrated, optically excited gas sensor, comprising: the device comprises a growth substrate, a PN semiconductor, a gas-sensitive test electrode and a light-excited gas-sensitive material, wherein the PN semiconductor is packaged on one surface of the growth substrate, the sensitive test electrode is arranged on the other surface of the growth substrate, and the light-excited gas-sensitive material is arranged on the gas-sensitive test electrode and the other surface of the growth substrate; the invention also provides a preparation method of the monolithic integrated photo-excitation gas sensor. According to the invention, the sensing material is monolithically integrated on the growth substrate of the wafer LED, so that an internal light source is realized, the volume of the light-excited gas sensor is effectively reduced, the detection system is simplified due to the absence of the external light source, and the power consumption is lower than that of the external light source; the method has the advantages of low cost, low power consumption, high performance, repeatability and industrialization, and can be widely applied to the detection of combustible gas, explosive gas, biological field and other special environments.
Description
Technical Field
The invention relates to the technical field of LEDs (light emitting diodes), in particular to a monolithic integrated photo-excitation gas sensor and a preparation method thereof.
Background
The gas sensor has the advantages of low cost, convenient and quick detection and the like in the aspect of detecting harmful gases, and is widely applied to various fields closely related to the life of people. With the development of the internet of things, a micro-electro-mechanical system (MEMS) sensor gradually replaces a traditional large-size gas sensor, so that the sensor is more miniaturized and integrated, and a micro-heater or a micro-hotplate is still adopted. The detection of the sensor system in special environments such as inflammable, explosive and biological environments is limited due to the excessively high working temperature, and meanwhile, the stability, repeatability, service life, energy consumption, cost and the like of the sensor system are influenced to a certain extent. The light-excited gas sensor does not need to be heated, and the working condition is room temperature, so that the gas sensor has many advantages compared with the traditional gas sensor, for example, the energy consumption is lower, the integration is convenient because of no heating circuit, and the gas sensor is suitable for detecting combustible gas and explosive gas and is suitable for being applied to special environments in the biological field and the like.
However, compared to the MEMS sensor, the conventional photo-excited gas sensor requires an external light source, which makes it difficult to integrate and miniaturize the sensor, and lacks high selectivity and stability in terms of performance, and cannot detect various odors/gases qualitatively and quantitatively, and the detection concentration limit of trace gases always stays at ppm level or sub-ppm level, and cannot detect harmful gases at ppb level.
Disclosure of Invention
In view of this, the present invention provides a monolithically integrated photo-excited gas sensor and a method for manufacturing the same, which can embed a light source.
In order to achieve the above object, the present invention provides a monolithically integrated photoexcited gas sensor, including:
the PN semiconductor is packaged on one surface of the growth substrate, the gas-sensitive test electrode is arranged on the other surface of the growth substrate, and the light-excited gas-sensitive material is arranged on the gas-sensitive test electrode and the other surface of the growth substrate.
Further, the PN semiconductor comprises a first semiconductor conducting layer, a light emitting layer, a second semiconductor conducting layer, a current spreading layer, a first electrode and a second electrode, wherein the first semiconductor conducting layer is located on the upper surface of the growth substrate, the light emitting layer is located on the first semiconductor conducting layer, the second semiconductor conducting layer is located on the light emitting layer, the current spreading layer is located on the second semiconductor conducting layer, the first electrode is located on the current spreading layer, and the second electrode is located on the first semiconductor conducting layer.
Further, the semiconductor device further comprises a passivation layer, wherein the passivation layer covers the first semiconductor conducting layer and the current spreading layer and exposes the first electrode and the second electrode relative to the passivation layer.
Further, a first bonding pad is formed on one end of the first electrode extending out of the passivation layer.
Further, a second bonding pad is formed on one end of the second electrode extending to the outside of the passivation layer.
Further, the growth substrate is a sapphire substrate.
Further, the light emitted by the PN semiconductor is ultraviolet light.
The invention also provides a preparation method of the monolithic integrated photo-excitation gas sensor, which comprises the following steps:
preparing and obtaining a growth substrate;
preparing a PN semiconductor on one surface of the growth substrate to obtain an LED wafer;
preparing a gas-sensitive test electrode on the other surface of the growth substrate;
preparing a light-excited gas-sensitive material on the other surface of the growth substrate, and electrically connecting the light-excited gas-sensitive material with the gas-sensitive test electrode;
and cutting and sorting the wafer of the monolithic integrated LED gas-sensitive sensor to obtain a plurality of light-excited gas-sensitive sensors.
Further, the method also comprises the following steps:
growing and forming a first semiconductor conducting layer, a light emitting layer and a second semiconductor conducting layer on the growth substrate;
photoetching and etching the above structure to expose the first semiconductor conductive layer,
evaporating an ITO film on the structure, and forming the current expansion layer on the second semiconductor conducting layer through photoetching and corrosion treatment;
depositing a silicon oxide protective layer on the structure, and forming a passivation layer on the first semiconductor conducting layer and the current spreading layer through photoetching and corrosion treatment, and exposing a part of the first semiconductor conducting layer and a part of the current spreading layer;
and depositing metal electrodes at the positions where the first semiconductor conducting layer and the current spreading layer are exposed to form a first electrode and a second electrode respectively.
Further, the method also comprises the following steps:
cleaning an LED wafer;
thinning a growth substrate;
and manufacturing a gas-sensitive test electrode by adopting a photoetching mask and electron beam evaporation method, and enabling the gas-sensitive test electrode to correspond to each core particle on the LED wafer.
Compared with the prior art, the invention has the following beneficial effects:
the invention designs a monolithic integrated light-activated gas sensor, wherein a PN semiconductor, a gas-sensitive test electrode and a light-activated gas-sensitive material are directly packaged on a growth substrate, and the sensing material is monolithically integrated on the growth substrate of a wafer LED, so that an internal light source is realized, the volume of the light-activated gas-sensitive sensor is effectively reduced, an external light source is omitted, a detection system is simplified, and the power consumption is lower than that of an external light source; the method has the advantages of low cost, low power consumption, high performance, repeatability and industrialization, and can be widely applied to the detection of combustible gas, explosive gas, biological field and other special environments.
Drawings
FIG. 1 is a schematic cross-sectional view of a monolithically integrated photoexcited gas sensor provided in accordance with the present invention;
FIG. 2 is a schematic flow chart of a method for manufacturing a monolithically integrated photoexcited gas sensor according to the present invention;
in the figure: 1-growth substrate, 2-PN semiconductor, 21-first semiconductor conducting layer, 22-luminous layer, 23-second semiconductor conducting layer, 24-current spreading layer, 25-first electrode, 26-second electrode, 27-passivation layer, 28-first pad, 29-second pad, 3-gas sensitive test electrode, 4-light excitation gas sensitive material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, a monolithically integrated optical excitation gas sensor according to a first embodiment of the present invention includes: growth substrate 1, PN semiconductor 2, gas sensitive test electrode 3 and light arouse gas sensitive material 4, PN semiconductor 2 encapsulate in growth substrate 1 one side, gas sensitive test electrode 3 sets up on the growth substrate 1 another side, light arouses gas sensitive material 4 to set up gas sensitive test electrode 3 and on the growth substrate 1 another side.
In the invention, the PN semiconductor 2, the gas-sensitive test electrode 3 and the light-excited gas-sensitive material 4 are directly packaged on the growth substrate 1, and the sensing material is monolithically integrated on the growth substrate of the wafer LED, so that an internal light source is realized, the volume of the light-excited gas-sensitive sensor is effectively reduced, the detection system is simplified without an external light source, and the power consumption is lower than that of an external light source; the method has the advantages of low cost, low power consumption, high performance, repeatability and industrialization, and can be widely applied to the detection of combustible gas, explosive gas, biological field and other special environments.
Specifically, the growth substrate 1 serves as a base to support, and the growth substrate 1 may include, but is not limited to, a silicon substrate, a gallium nitride substrate, a sapphire substrate, or the like. In the present embodiment, the growth substrate 1 is a sapphire substrate.
Specifically, the PN semiconductor 2 includes a first semiconductor conductive layer 21, a light emitting layer 22, a second semiconductor conductive layer 23, a current spreading layer 24, a first electrode 25, and a second electrode 26, the first semiconductor conductive layer 21 is located on the upper surface of the growth substrate 1, the light emitting layer 22 is located on the first semiconductor conductive layer 21, the second semiconductor conductive layer 23 is located on the light emitting layer 22, the current spreading layer 24 is located on the second semiconductor conductive layer 23, the first electrode 25 is located on the current spreading layer 24, and the second electrode 26 is located on the first semiconductor conductive layer 21.
A PN junction is formed between the first electrode 25 and the second electrode 26, and when the PN junction is energized, a specific light is emitted.
It should be noted that the light emitted by the PN semiconductor 2 may be ultraviolet light, blue light, green light, yellow light, red light, etc., and as an alternative embodiment, the light emitted by the PN semiconductor 2 is ultraviolet light. The deep ultraviolet has short wavelength and higher energy to excite the gas sensitive material, so that the detection performance of the light-excited gas sensitive material 4 is excellent. In addition, since deep ultraviolet has high excitation energy, its power consumption is low.
In some embodiments, the light emitting layer 22 is a MQW (multiple quantum well) structure, for example, including alternately stacked InGaN (indium gallium nitride) layers and GaN (gallium nitride) layers.
In some embodiments, the current spreading layer 24 may be a transparent Indium Tin Oxide (ITO) layer.
In this embodiment, a passivation layer 27 is further included, and the passivation layer 27 covers the first semiconductor conductive layer 21 and the current spreading layer 24 and exposes the first electrode 25 and the second electrode 26 relative to the passivation layer 27.
The passivation layer 27 protects the first semiconductor conductive layer 21 and the current spreading layer 24. In some embodiments, the material of the passivation layer 27 includes an oxide of silicon and/or a nitride of silicon, which may be, for example, siO 2 Layer or SiN layer or SiO 2 And SiN.
In some embodiments, a first pad 28 is formed on an end of the first electrode 25 extending beyond the passivation layer 27.
In some embodiments, a second pad 29 is formed on an end of the second electrode 26 extending beyond the passivation layer 27.
In order to reduce the absorption of the gas-sensitive test electrode 3 to deep ultraviolet light and increase the light transmittance, as an optional implementation manner, the gas-sensitive test electrode 3 is of an interdigital electrode structure. And (3) evaporating and plating the gas-sensitive test electrode 3 by using photoresist as a mask material through electron beam evaporation.
The composite, mixed or other structure of the photo-excitation gas-sensitive material 4 is selected, and the material can be modified through treatments such as doping, surface modification, high-temperature annealing and the like, so that the gas-sensitive material with better photo-excitation sensing performance is obtained. Because the gas-sensitive material is prepared on the back surface of the growth substrate 1, chemical reagents which are harmful to the growth substrate 1 by strong acid and strong base in the synthesis process are avoided when the gas-sensitive material is selected. Alternatively, capillary, electrospray, spin coating, etc. methods are contemplated for gas-sensitive material preparation on the back side of the growth substrate 1. As an alternative embodiment, the photoexcited gas-sensitive material 4 is prepared from ZnO nanorods. Preferably, znO nano-rods are used as gas-sensitive materials, and a hydrothermal synthesis method is adopted. The method can avoid the occurrence of strong acid and strong base chemical reagents in the synthesis process, and ensure the uniformity of the sensing material sheets.
The invention further comprises a power supply gold wire which is electrically connected with the PN semiconductor 2 and used for supplying power to the PN semiconductor 2.
The invention also comprises a gas-sensitive test gold wire which is electrically connected with the light-excited gas-sensitive material 4 and is used for testing the light-excited gas-sensitive material 4.
The invention designs a monolithic integrated light-activated gas sensor, wherein a PN semiconductor 2, a gas-sensitive test electrode 3 and a light-activated gas-sensitive material 4 are directly packaged on a growth substrate 1, and the sensing material is monolithically integrated on the growth substrate of a wafer LED, so that an internal light source is realized, the volume of the light-activated gas sensor is effectively reduced, a detection system is simplified without an external light source, and the power consumption is lower than that of an external light source; the method has the advantages of low cost, low power consumption, high performance, repeatability and industrialization, and can be widely applied to the detection of combustible gas, explosive gas, biological field and other special environments.
The invention also provides a preparation method of the monolithic integrated photo-excited gas-sensitive sensor, which is used for preparing the photo-excited gas-sensitive sensing structure described in the first embodiment, and referring to fig. 2, the preparation method comprises the following steps:
s1, preparing a growth substrate 1;
s2, preparing a PN semiconductor 2 on one surface of the growth substrate 1 to obtain an LED wafer;
s3, preparing a gas-sensitive test electrode 3 on the other surface of the growth substrate 1;
s4, preparing a light-excited gas-sensitive material 4 on the other surface of the growth substrate 1, and electrically connecting the light-excited gas-sensitive material 4 with the gas-sensitive test electrode 3;
and S5, cutting and sorting the wafer of the monolithic integrated LED gas-sensitive sensor to obtain a plurality of light-excited gas-sensitive sensing structures.
It should be noted that the preparation method in this embodiment is used to prepare the gas sensor structure in the first embodiment. Therefore, the features not explained in detail in the present embodiment can be fully explained with reference to the first embodiment.
In a specific implementation, the light emitted by the PN semiconductor 2 may be ultraviolet light, blue light, green light, yellow light, red light, and the like, and as an alternative implementation, the light emitted by the PN semiconductor 2 is ultraviolet light. The deep ultraviolet has short wavelength and higher energy to excite the gas sensitive material, so that the detection performance of the light-excited gas sensitive material 4 is excellent. In addition, since deep ultraviolet has high excitation energy, power consumption thereof is low. The ultraviolet light excited gas-sensitive sensor does not need to be heated, the working condition is room temperature, and the gas-sensitive sensor has better gas-sensitive sensing performance at room temperature, including selectivity, response recovery speed, sensitivity, stability and the like. In particular, the detection of harmful gas of ppb level can be realized.
As an alternative embodiment, the gas-sensitive test electrode 3 is an interdigital electrode structure.
As an optional implementation manner, preparing a PN semiconductor 2 on one side of the growth substrate 1 to obtain an LED wafer specifically includes:
s21, growing and forming a first semiconductor conducting layer 21, a light emitting layer 22 and a second semiconductor conducting layer 23 on the growth substrate 1;
s22, photoetching and etching the structure to expose the first semiconductor conducting layer 21,
s23, evaporating an ITO film on the structure, and forming the current expansion layer 24 on the second semiconductor conducting layer 23 through photoetching, corrosion and other treatment;
s24, depositing a silicon oxide protective layer on the structure, and performing photoetching, corrosion and other treatment to form a passivation layer 27 on the first semiconductor conducting layer 21 and the current spreading layer 24 and expose part of the first semiconductor conducting layer 21 and part of the current spreading layer 24;
and S25, depositing metal electrodes at positions where the first semiconductor conductive layer 21 and the first current spreading layer are exposed to form a first electrode 25 and a second electrode 26 respectively.
As an alternative embodiment, a gas-sensitive test electrode 3 is prepared on the other side of the growth substrate 1, and specifically includes:
s31, cleaning the LED wafer;
s32, thinning the growth substrate;
s33, manufacturing the gas-sensitive test electrode 3 by adopting a photoetching mask and electron beam evaporation method, and enabling the gas-sensitive test electrode 3 to correspond to each core particle on the LED wafer.
Specifically, when the LED wafer is cleaned, ultrasonic cleaning is respectively carried out on a single LED wafer for 5min by using acetone and isopropanol, organic matters on the surface of the wafer are removed, then deionized water is used for washing for 5min, and a nitrogen gun is used for drying; organic matters on the surface of the LED wafer can be effectively removed.
The thinning of the growth substrate can improve the heat dissipation and the manufacturing yield of the LED, and the gas-sensitive test electrode 3 and the light-excited gas-sensitive material 4 can be conveniently manufactured on the growth substrate.
As an optional implementation manner, preparing a photo-excitation gas-sensitive material 4 on the other surface of the growth substrate 1, and electrically connecting the photo-excitation gas-sensitive material 4 with the gas-sensitive test electrode 3 specifically includes:
and depositing the modified gas-sensitive material on the other surface of the growth substrate 1 to obtain the light-excited gas-sensitive material 4, wherein the light-excited gas-sensitive material 4 is electrically connected with the gas-sensitive test electrode 3.
Specifically, a composite type and a mixed type gas-sensitive sensing material, such as a ZnO nanorod, is selected, and the material is modified through treatments such as doping, surface modification, high-temperature annealing and the like, so that the gas-sensitive material with good photoexcitation sensing performance is obtained.
The preparation method of the light-excited gas-sensitive material 4 includes, but is not limited to, hydrothermal synthesis, magnetron sputtering, a gel-sol method, and the like. The method preferentially adopts a hydrothermal synthesis method to prepare the sensing material on the back surface of the sapphire substrate of the deep ultraviolet LED wafer, and the method can avoid the occurrence of strong acid and strong base chemical reagents in the synthesis process and ensure the uniformity in the sensing material sheet.
According to the preparation process in the embodiment, the gas sensor structure prepared by the preparation method in the embodiment has the advantages of low cost, low power consumption, high performance, repeatability and industrialization, is suitable for detecting combustible gas and explosive gas, and is suitable for being applied to special environments such as the biological field.
The above-described embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A monolithically integrated photoexcitable gas sensor, comprising:
the PN semiconductor is packaged on one surface of the growth substrate, the gas-sensitive test electrode is arranged on the other surface of the growth substrate, and the light-excited gas-sensitive material is arranged on the gas-sensitive test electrode and the other surface of the growth substrate.
2. A monolithically integrated photoexcited gas sensor of claim 1, wherein:
the PN semiconductor comprises a first semiconductor conducting layer, a light emitting layer, a second semiconductor conducting layer, a current spreading layer, a first electrode and a second electrode, wherein the first semiconductor conducting layer is located on the upper surface of the growth substrate, the light emitting layer is located on the first semiconductor conducting layer, the second semiconductor conducting layer is located on the light emitting layer, the current spreading layer is located on the second semiconductor conducting layer, the first electrode is located on the current spreading layer, and the second electrode is located on the first semiconductor conducting layer.
3. A monolithically integrated photoexcited gas sensor of claim 2, wherein:
the passivation layer covers the first semiconductor conducting layer and the current spreading layer and enables the first electrode and the second electrode to be exposed relative to the passivation layer.
4. A monolithically integrated photoexcited gas sensor of claim 3, wherein:
and a first bonding pad is formed on one end of the first electrode, which extends out of the passivation layer.
5. A monolithically integrated photoexcited gas sensor of claim 3, wherein:
and a second bonding pad is formed on one end of the second electrode extending to the outside of the passivation layer.
6. A monolithically integrated photoexcited gas sensor of claim 1, wherein:
the growth substrate is a sapphire substrate.
7. A monolithically integrated photoexcited gas sensor of claim 1, wherein:
the light emitted by the PN semiconductor is ultraviolet light.
8. A method of making a monolithically integrated photoexcited gas sensor, for use in making a monolithically integrated photoexcited gas sensor of any of claims 1-7, comprising the steps of:
preparing and obtaining a growth substrate;
preparing a PN semiconductor on one surface of the growth substrate to obtain an LED wafer;
preparing a gas-sensitive test electrode on the other surface of the growth substrate;
preparing a photo-excitation gas-sensitive material on the other surface of the growth substrate, and electrically connecting the photo-excitation gas-sensitive material with the gas-sensitive test electrode;
and cutting and sorting the wafer of the monolithic integrated LED gas-sensitive sensor to obtain a plurality of light-excited gas-sensitive sensors.
9. The method for preparing a monolithically integrated photoexcited gas sensor of claim 8, wherein the step of preparing a PN semiconductor on one side of the growth substrate to obtain an LED wafer specifically comprises:
growing and forming a first semiconductor conducting layer, a light emitting layer and a second semiconductor conducting layer on the growth substrate;
photoetching and etching the above-mentioned structure to expose first semiconductor conducting layer,
evaporating an ITO film on the structure, and forming the current expansion layer on the second semiconductor conducting layer through photoetching and corrosion treatment;
depositing a silicon oxide protective layer on the structure, and forming a passivation layer on the first semiconductor conducting layer and the current spreading layer through photoetching and corrosion treatment, and exposing a part of the first semiconductor conducting layer and a part of the current spreading layer;
and depositing metal electrodes at the positions where the first semiconductor conducting layer and the current spreading layer are exposed to form a first electrode and a second electrode respectively.
10. The method for preparing a monolithically integrated photoexcitation gas sensor of claim 8, wherein the step of preparing a gas-sensitive test electrode on the other side of the growth substrate specifically comprises:
cleaning an LED wafer;
thinning a growth substrate;
and manufacturing a gas-sensitive test electrode by adopting a photoetching mask and electron beam evaporation method, and enabling the gas-sensitive test electrode to correspond to each core particle on the LED wafer.
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