CN120421053A - Microfluidic panel, mercury ion detection device based on gallium nitride and preparation method of mercury ion detection device - Google Patents
Microfluidic panel, mercury ion detection device based on gallium nitride and preparation method of mercury ion detection deviceInfo
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- CN120421053A CN120421053A CN202510313361.XA CN202510313361A CN120421053A CN 120421053 A CN120421053 A CN 120421053A CN 202510313361 A CN202510313361 A CN 202510313361A CN 120421053 A CN120421053 A CN 120421053A
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Abstract
本发明公开了一种微流控面板、基于氮化镓的汞离子浓度检测装置及其制备方法，涉及离子浓度检测技术领域，微流控面板包括蛇形通道，其首端与反应池相连，尾端分别与第一通道和第二通道相连；所述第一通道流经半导体结构的栅极区；在所述蛇形通道、所述第一通道和所述第二通道的连接处设置有磁性件，用于分流溶液中的正离子和负离子。本发明采用电化学的方法利用适配体表面的胸腺嘧啶碱基与汞离子结合，在传感器表面形成稳定的T‑Hg‑T复合物，从而改变GaN器件栅极表面的电荷分布，导致二维电子气浓度变化和源漏电流变化，该传感器件没有参比电极，结构简单，检测的漏极电流对器件表面电荷变化敏感。提高检测的灵敏度。
The present invention discloses a microfluidic panel, a gallium nitride-based mercury ion concentration detection device and a preparation method thereof, relating to the field of ion concentration detection technology. The microfluidic panel includes a serpentine channel, the head end of which is connected to a reaction pool, and the tail end is respectively connected to a first channel and a second channel; the first channel flows through the gate region of a semiconductor structure; a magnetic member is provided at the connection between the serpentine channel, the first channel and the second channel for diverting positive ions and negative ions in a solution. The present invention adopts an electrochemical method to utilize the thymine bases on the surface of the aptamer to combine with mercury ions to form a stable T-Hg-T complex on the sensor surface, thereby changing the charge distribution on the gate surface of the GaN device, resulting in changes in the two-dimensional electron gas concentration and the source-drain current. The sensor device has no reference electrode, has a simple structure, and the detected drain current is sensitive to changes in the device surface charge. The sensitivity of the detection is improved.
Description
Technical Field
The invention relates to the technical field of ion concentration detection, in particular to a microfluidic panel, a mercury ion concentration detection device based on gallium nitride and a preparation method thereof.
Background
The use of heavy metals in industrial production is increasing, and is thereafter becoming a key element for promoting social progress. Such as lead, cadmium, mercury, etc., play an important role in the fields of battery manufacturing, alloy production, etc. Later, heavy metals were recognized as being a serious hazard to the environment and physical health. These heavy metal elements often permeate into the water body through industrial wastewater, causing pollution. Mercury ions are also extremely toxic heavy metal ions, and a small excess of mercury ions can interfere the functions of enzymes and proteins in a human body to influence the normal activities of cells, so that the cells are damaged and necrotized. Long-term exposure to mercury ion environments may lead to damage to the nervous system, the initiation of kidney disease, and the like. Therefore, there is a need to tightly control the emission of mercury ions to reduce their harm to the environment and human body. The existing technology for detecting the heavy metal content in the water body can be mainly divided into three categories, namely a spectroscopic analysis method, an electrochemical analysis method and a biochemical analysis method. The spectroscopy requires large equipment, is accurate in detection, and lacks flexibility. The detection devices used in the electrochemical methods are all moving toward miniaturization and integration. In the electrochemical sensor method, by fixing a specific recognition element on the surface of an electrode, a sensor with high sensitivity to specific heavy metal ions can be designed and manufactured, so that rapid and effective detection of the heavy metal ions in the environment is realized.
Microfluidic technology focuses on precisely manipulating fluids on the micrometer scale. The micro-fluidic chip is integrated with micro-structures such as a micro-channel, a micro-reaction tank, a micro-valve, a micro-pump and the like, and is used for accurately controlling micro-fluid. Microfluidic chip technology is widely applied in the field of water quality detection by virtue of the advantages of low consumption of samples and reagents, high-speed analysis, multi-parameter integrated detection, automation, integration, portability and the like. By optimizing the design of the micro-flow channel, the technology can rapidly capture and separate trace heavy metal ions, and the detection threshold is obviously reduced. By combining electrochemical, optical or fluorescent sensing technology, the method can also realize high-specificity and high-precision heavy metal ion detection. In addition, the microminiaturization and portability of the microfluidic chip also enable on-site real-time monitoring to be realized, and the microfluidic chip is suitable for multiple scenes such as environmental monitoring, food safety and industrial wastewater treatment.
Disclosure of Invention
The present invention has been made in view of the above-mentioned problems occurring in the prior art.
In order to solve the technical problems, the first aspect of the invention provides a microfluidic panel which comprises a serpentine channel, wherein the head end of the serpentine channel is connected with a reaction tank, the tail end of the serpentine channel is respectively connected with a first channel and a second channel, the first channel flows through a grid region of a semiconductor structure, and a magnetic part is arranged at the joint of the serpentine channel, the first channel and the second channel and is used for shunting positive ions and negative ions in a solution.
As a preferable scheme of the microfluidic panel, at least one filter unit is connected in series on the serpentine channel.
As a preferable scheme of the microfluidic panel, the reaction tank is respectively connected with a first liquid inlet and a second liquid inlet, and the middle part of the serpentine channel is also connected with a third liquid inlet.
The invention further provides a mercury ion concentration detection device which comprises the microfluidic panel, a buffer layer and a two-dimensional electron gas layer which are sequentially stacked, wherein the two-dimensional electron gas layer comprises an intrinsic layer, an isolation layer and a barrier layer which are sequentially stacked, a groove is formed in the surface of the barrier layer, a specific identification layer is coated on the surface of the groove, and when liquid to be detected flows through the specific identification layer, the surface charge of the liquid to be detected is changed.
As a preferable scheme of the gallium nitride-based mercury ion concentration detection device, the specific recognition layer comprises a graphene/metal platinum nanoparticle composite and an aptamer coated on the surface of the groove.
The gallium nitride-based mercury ion concentration detection device is characterized in that the thickness of the buffer layer is 1-10000 nm, the material of the intrinsic layer is GaN, the thickness of the intrinsic layer is 10-6000 nm, the material of the barrier layer is AIGaN, the thickness of the barrier layer is 10-25 nm, and the material of the isolation layer is AIN, and the thickness of the isolation layer is 1nm.
The gallium nitride-based mercury ion concentration detection device also comprises a source electrode, a drain electrode and a gate region, wherein the source electrode and the drain electrode are arranged on the top of the intrinsic layer, the gate region is arranged on the top of the groove, and the gate region is partially arranged in the groove.
As a preferable scheme of the gallium nitride-based mercury ion concentration detection device, the device further comprises a bottom plate and a top plate, wherein the buffer layer and the two-dimensional electron gas layer are embedded into the bottom plate, and the microfluidic panel is positioned between the bottom plate and the top plate.
In a third aspect, the present invention also provides a method for preparing a gallium nitride-based mercury ion concentration detection apparatus, the method being suitable for preparing the gallium nitride-based mercury ion concentration detection apparatus, the method comprising forming a buffer layer on a surface of a substrate; forming an intrinsic layer on the surface of the buffer layer, forming an isolation layer on the surface of the intrinsic layer, forming a barrier layer on the surface of the isolation layer, forming a groove on the surface of the barrier layer, coating a specific identification layer on the surface of the barrier layer, and covering a microfluidic panel on the specific identification layer.
The preparation method of the gallium nitride-based mercury ion concentration detection device is characterized in that the specific recognition layer is made of graphene/metal platinum nanoparticle composite materials.
The invention has the beneficial effects that the electrochemical method is adopted, thymine base on the surface of the aptamer is combined with mercury ions, and a stable T-Hg-T compound is formed on the surface of the sensor, so that the charge distribution on the surface of the grid electrode of the GaN device is changed, the two-dimensional electron gas concentration change and the source leakage current change are caused, the sensing device is not provided with a reference electrode, the structure is simple, and the detected drain current is sensitive to the change of the charge on the surface of the device. Meanwhile, the graphene/metal nanocomposite material provides more surface active points, is easy for fixing an aptamer, adsorbs more complexes, and improves the detection sensitivity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a cross-sectional view of a gallium nitride-based mercury ion concentration detection apparatus.
Fig. 2 is a top view of a microfluidic panel.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Referring to fig. 1 and 2, a microfluidic panel M according to a first embodiment of the present invention is provided, where the microfluidic panel M includes a serpentine channel 1, and a first end of the serpentine channel 1 is connected to a reaction cell 2, and a second end of the serpentine channel 1 is respectively branched into two branches with respect to a first channel 1-1 and a second channel 1-2, that is, the serpentine channel 1. The first channel 1-1 flows through the gate region 14 of the semiconductor structure.
The magnetic piece 3 is placed at the joint of the serpentine channel 1, the first channel 1-1 and the second channel 1-2, the magnetic piece 3 can be a small magnet and is used for shunting positive and negative ions of the solution in the serpentine channel 1, positive ions enter the first channel 1-1, and negative ions enter the second channel 1-2.
The tail ends of the first channel 1-1 and the second channel 1-2 are respectively connected with a first liquid outlet 1-1-1 and a second liquid outlet 1-2-1. The reaction tank 2 is also connected with a first liquid inlet 5 and a second liquid inlet 6 respectively. A third liquid inlet 7 is also connected to the middle of the serpentine channel 1.
When the microfluidic panel M is used for testing the concentration of mercury ions, the first liquid inlet 5 and the second liquid inlet 6 are respectively filled with ethylenediamine tetraacetic acid buffer solution and water to be tested, and mixed and precipitated in the reaction tank 2. When the mixed solution is about to pass through the third liquid inlet, acetic acid-sodium acetate buffer solution is introduced into the third liquid inlet 7. The acetic acid-sodium acetate buffer can resist the addition of a small amount of acid or alkali in an unknown solution and the pH value change caused by chemical reaction possibly occurring in the serpentine channel 1 through the buffer effect, so that the environmental pH in the serpentine channel 1 is kept relatively stable. It can interact with the surface of the serpentine channel 1, reducing the non-specific adsorption of biomolecules on the walls of the serpentine channel 1. In addition, the buffer solution provides proper ionic strength, optimizes the interaction between the sensor surface and mercury ions, simultaneously inhibits the interference of other metal ions or impurities on the detection result, and improves the specificity of detection. The serpentine channel 1 has a roundabout structure so that the ethylenediamine tetraacetic acid buffer solution and the water body to be tested can be fully mixed.
Three filter units 4 are also connected in series in the serpentine channel 1, and the filter units 4 can filter the solution. When the solution flows into the serpentine channel 1, the first channel 1-1 and the second channel 1-2, the magnetic piece 3 can split positive and negative ions in the solution, hg 2+ can enter the first channel 1-1, when the solution flows through the gate region 14, the graphene/metal platinum nano-composite layer modified by the aptamer near the gate region 14 can specifically identify mercury ions, when Hg+ ions are combined with thymine bases on the surface of the aptamer, the surface charge of the electrode can be changed, and the current value and Hg 2+ concentration are in a linear relation. Specifically, the nitrogen atom in the thymine molecule forms a coordinate bond with the mercury ion, and this coordination enables thymine to effectively bind to the mercury ion, thereby forming a stable T-Hg-T complex on the sensor surface. An aptamer such as a thymine-containing DNA oligonucleotide is usually immobilized on the electrode surface. When Hg 2+ is present, it coordinates with thymine in the DNA, causing the DNA to transition from a flexible single strand to a relatively rigid double-stranded analog complex, thereby altering the charge distribution at the electrode surface. And measuring an I-V characteristic curve of the semiconductor device, and establishing a standard curve of the detection device according to current values output by Hg 2+ solutions with different concentrations.
As an alternative embodiment, the invention also provides a mercury ion concentration detection device based on gallium nitride, which comprises the microfluidic panel M and a semiconductor structure device, wherein the device comprises a buffer layer 9 and a two-dimensional electron gas layer 10 which are sequentially stacked on a substrate 17, the two-dimensional electron gas layer 10 comprises an intrinsic layer 10-1, an isolation layer 10-2 and a barrier layer 10-3 which are sequentially stacked on the surface of the substrate 17, the surface of the barrier layer 10-3 is provided with a groove, and the surface of the groove is coated with a specific identification layer 11.
Preferably, the specific recognition layer 11 comprises a graphene/metal platinum nanoparticle complex coated on the surface of the groove and an aptamer having thymine bases on the surface. The nitrogen atoms in the thymine molecules form coordination bonds with mercury ions, and the coordination effect enables thymine to be effectively combined with mercury ions, so that stable T-Hg-T complex is formed on the surface of the sensor. An aptamer such as a thymine-containing DNA oligonucleotide is usually immobilized on the electrode surface. When Hg < 2+ > is present, it will coordinate with thymine in the DNA, causing the DNA to transition from a flexible single strand to a relatively rigid double-stranded analog complex, thereby altering the charge distribution at the electrode surface.
Preferably, the thickness of the buffer layer is 1-10000 nm, the material of the intrinsic layer 10-1 is GaN, the thickness of the intrinsic layer is 10-6000 nm, the material of the barrier layer 10-3 is AIGaN, the thickness of the barrier layer is 10-25 nm, and the material of the isolation layer 10-2 is AIN, and the thickness of the barrier layer is 1nm.
Specifically, a source electrode 12 and a drain electrode 13 are further arranged on the top of the intrinsic layer 10-1, and a gate region 14 is arranged on the top of the groove, wherein the gate region 14 is partially arranged in the groove.
The semiconductor device structure is embedded in the bottom plate 15, and the microfluidic panel M is disposed between the bottom plate 15 and the top plate 16.
As an alternative embodiment, the present invention further provides a method for preparing a device for detecting a concentration of mercury ions based on gallium nitride, the method comprising:
Step one, a buffer layer 9 is grown on the surface of a substrate 17 through a metal organic chemical vapor phase epitaxy process, the buffer layer 9 comprises a GaN buffer layer or an AlGaN buffer layer, and a heterostructure layer is grown on the buffer layer.
And step two, coating a layer of AZ4210 photoresist with the thickness of 1-2 mu m on the temporary device obtained in the step one by adopting a spin speed of 3000rpm, and then placing the temporary device on a hot plate with the temperature of 100 ℃ for 2 minutes for pre-baking. The AlGaN barrier layer 10-3 is etched by ICP etching technique. After the mesa etching is completed, an ohmic contact area is defined on the active area through a photoetching technology, and then the active area is put into a photoetching machine to be exposed for 4 seconds, and then is put into a hot plate to be post-baked;
Then the substrate is put into a developing solution to develop an ohmic electrode area of a source electrode and a drain electrode, ti/Al/Ni/Au is sequentially grown on the defined ohmic contact area from bottom to top by adopting an electron beam evaporation or sputtering method, and a source electrode 12 and a drain electrode 13 are formed. And (3) placing the device in a nitrogen environment for rapid thermal annealing treatment, and removing the residual photoresist at the bottom. And growing a layer of passivation material by adopting a PECVD method.
And thirdly, coating a layer of AZ4210 photoresist with the thickness of 1-2 mu m on the temporary device obtained in the second step by adopting a spin speed of 3000rpm, exposing by using a photomask, developing the exposed photoresist by using a developing solution TMAH, and leaking out the gate region 14 to be etched.
The recess structure is then etched in the gate region 14 by an inductively coupled plasma etching system using a mixture of Cl 2 and BCl 3. And then a layer of Ni/Au metal combination is deposited on the two sides and the bottom of the groove by adopting a PECVD method. The Ni/Au gate electrode forms a good schottky contact with the AlGaN barrier layer 10-3.
And fourthly, coating a graphene/metal platinum nanoparticle composite material on the gate region 14 etched in the third step, and fixing an aptamer on the surface of the composite material through covalent bonds or electrostatic adsorption to obtain a third temporary device.
And step five, covering the temporary device obtained in the step four with a micro-channel layer with matched size. The layer adopts photoetching technology to form a channel pattern, ICP etching is used to form a channel, and the microfluidic panel M is obtained through reverse molding, solidification and stripping. Cutting the filter membrane to a proper size, and placing the filter membrane in a slot reserved for placing the filter membrane when designing the microfluidic channel to form the filter unit 4. The photoresist covers part of the source electrode 12 and part of the drain electrode 13, the main channel passes through the groove gate region 14, and a small magnet is embedded in the surface of the channel shunt, and meanwhile, holes are drilled at the liquid inlet and outlet ends.
And step six, carrying out plasma treatment on the surface of the micro-channel layer, and packaging the micro-fluidic channel by an adhesion or hot pressing method. After packaging, the preset fluid up-down channels are connected with the electrode leads, thereby manufacturing the final device.
It should be appreciated that the principle of specific recognition of mercury ions by the aptamer-modified graphene/metal platinum nanocomposite layer is that when Hg 2+ ions bind to thymine bases on the surface of the aptamer, the change of electrode surface charge is caused, and the current value is in a linear relationship with Hg 2+ concentration. Specifically, the nitrogen atom in the thymine molecule forms a coordinate bond with the mercury ion, and this coordination enables thymine to effectively bind to the mercury ion, thereby forming a stable T-Hg-T complex on the sensor surface. An aptamer such as a thymine-containing DNA oligonucleotide is usually immobilized on the electrode surface. When Hg 2+ is present, it coordinates with thymine in the DNA, causing the DNA to transition from a flexible single strand to a relatively rigid double-stranded analog complex, thereby altering the charge distribution at the electrode surface.
Further, the preparation step of the graphene/metal platinum nanoparticle composite in the fourth step comprises the following steps:
Dissolving a proper amount of ultrasonic-treated graphite oxide and a precursor of metal platinum in 30ml of deionized water, stirring and mixing, adding 2ml of sodium citrate solution, 5ml of absolute ethyl alcohol and a proper amount of sodium borohydride, heating the stirred solution at 180 ℃ for 5 hours, centrifugally separating, washing with distilled water and ethanol for multiple times, and drying in a 60 ℃ vacuum oven for 12 hours to obtain the graphene/metal platinum nanoparticle compound.
Further, the step of modifying the recessed gate includes:
And (3) putting a proper amount of synthesized graphene/platinum nanoparticle compound into deionized water, ultrasonically mixing until the uniform suspension is free of particles, dripping a small amount of solution on the surface of the groove, covering a glass cover on the surface of the groove, airing in a drying area, and fixing an aptamer on the surface of the composite material through covalent bond or electrostatic adsorption.
As an alternative embodiment, the present invention further provides a method for detecting Hg 2+ by using a gallium nitride-based mercury ion concentration detection apparatus, including the following steps:
Sequentially introducing Hg2 + standard buffer solutions with different concentrations into the serpentine channel 1, introducing the solutions into the first channel 1-1, applying different drain biases to the source electrode 12 and the drain electrode 13 of the device, and measuring the I-V characteristic curve of the GaN device. And establishing a standard curve of the detection device according to the current values output by Hg2 + solutions with different concentrations.
And secondly, irradiating the water body to be measured for 30s by an ultraviolet lamp in advance. And (3) respectively introducing a proper amount of ethylenediamine tetraacetic acid buffer solution and a water body to be measured into the two liquid inlets, and mixing and precipitating in the reaction tank. And when the mixed solution is about to pass through the third liquid inlet, introducing acetic acid-sodium acetate buffer solution into the third liquid inlet.
And step three, measuring the output current value of the mixed solution under the same condition when the mixed solution passes through the groove structure. And comparing the output current with a standard curve, and determining the concentration of Hg2 + in the solution to be detected according to the matched current value.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (10)
1. A microfluidic panel (M) is characterized by comprising,
The serpentine channel (1) is connected with the reaction tank (2) at the head end and connected with the first channel (1-1) and the second channel (1-2) at the tail end respectively, wherein the first channel (1-1) flows through the grid region (14) of the semiconductor structure;
And a magnetic piece (3) is arranged at the joint of the serpentine channel (1), the first channel (1-1) and the second channel (1-2) and is used for shunting positive ions and negative ions in the solution.
2. The microfluidic panel (M) according to claim 1, wherein at least one filter unit (4) is connected in series to the serpentine channel (1).
3. The microfluidic panel (M) according to claim 1 or 2, wherein the reaction tank (2) is respectively connected with the first liquid inlet (5) and the second liquid inlet (6), and the middle part of the serpentine channel (1) is also connected with a third liquid inlet (7).
4. The mercury ion concentration detection device based on gallium nitride is characterized by comprising the microfluidic panel (M) according to any one of claims 1-3, a buffer layer (9) and a two-dimensional electron gas layer (10) which are stacked in sequence;
The two-dimensional electron gas layer (10) comprises an intrinsic layer (10-1), an isolation layer (10-2) and a barrier layer (10-3) which are sequentially stacked, wherein a groove is formed in the surface of the barrier layer (10-3), and a specific identification layer (11) is coated on the surface of the groove;
when the liquid to be measured flows through the specific recognition layer (11), the surface charge thereof is changed.
5. The gallium nitride-based mercury ion concentration detection apparatus according to claim 4, wherein the specific recognition layer (11) comprises a graphene/metal platinum nanoparticle complex coated on the surface of the groove and an aptamer having thymine bases on the surface thereof.
6. The gallium nitride-based mercury ion concentration detection apparatus according to claim 5, wherein the buffer layer has a thickness of 1 to 10000nm, the intrinsic layer (10-1) is made of GaN and has a thickness of 10 to 6000nm, the barrier layer (10-3) is made of AIGaN and has a thickness of 10 to 25nm, and the isolation layer (10-2) is made of AIN and has a thickness of 1nm.
7. The gallium nitride-based mercury ion concentration detection apparatus according to claim 6, further comprising a source electrode (12) and a drain electrode (13) disposed on top of the intrinsic layer (10-1), a gate region (14) disposed on top of the recess, the gate region (14) being partially disposed within the recess.
8. The gallium nitride-based mercury ion concentration detection apparatus according to claim 7, further comprising a bottom plate (15) and a top plate (16), wherein the buffer layer (9) and the two-dimensional electron gas layer (10) are embedded in the bottom plate (15), and wherein the microfluidic panel (M) is located between the bottom plate (15) and the top plate (16).
9. A preparation method of a mercury ion concentration detection device based on gallium nitride is characterized by being suitable for preparing the mercury ion concentration detection device according to any one of claims 4-8, and comprises the following steps:
forming a buffer layer (9) on the surface of a substrate (17);
Forming an intrinsic layer (10-1) on the surface of the buffer layer (9);
Forming an isolation layer (10-2) on the surface of the intrinsic layer (10-1);
Forming a barrier layer (10-3) on the surface of the isolating layer (10-2);
A groove is formed in the surface of the barrier layer (10-3), and a specific recognition layer (11) is coated on the surface of the barrier layer;
-overlaying a microfluidic panel (M) on said coating-specific recognition layer (11).
10. The method for preparing a gallium nitride-based mercury ion concentration detection apparatus according to claim 9, wherein the material of the specific recognition layer (11) is a graphene/metal platinum nanoparticle composite material.
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