CN112858426B - Soil pH value detection device for blueberry planting - Google Patents
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/302—Electrodes, e.g. test electrodes; Half-cells pH sensitive, e.g. quinhydron, antimony or hydrogen electrodes
Abstract
The invention provides a soil pH value detection device for blueberry planting, which comprises: the device comprises a substrate (1), a drain electrode (2), a source electrode (3), an insulating film (4), a cathode (5), an anode (6), a counter electrode (7), a coulomb titration device (8), an output signal (9), a channel (10) and a reference electrode (11). The device has high sensitivity and accuracy in a wide pH range, so that the harsh requirement of strawberry planting on the pH value of soil can be well met.
Description
Technical Field
The invention belongs to the technical field of detection in agricultural planting, and particularly relates to a soil pH value detection device for blueberry planting.
Background
The adaptability of various plants to the pH value of soil has a certain range, and the plants can fully acquire the nutrition required by growth from the soil only when the pH value of the soil is proper. Blueberry is particularly sensitive to soil pH, and slight fluctuations in soil pH may have a significant impact on blueberry growth and blueberry yield. The pH value of the soil is one of limiting factors affecting the productivity and the fertility of the soil, has close relation with available nutrients of the soil, and obviously affects the effective absorption of nutrient elements required by plants and microorganisms. Chai Xizhou et al consider that soil pH is a common combination of many chemical properties, related to soil microbial activity, organic matter conversion, the form of mineral nutrient presence and nutrient holding capacity, etc. The soil pH value can be effectively and even measured in the ground to obtain the soil pH value, the soil fertilization formula can be determined, and the method has important significance for the development of blueberry planting industry.
CN103353469a discloses a practical soil PH detecting circuit, comprising a first operational amplifier and a second operational amplifier; the non-inverting input end of the first operational amplifier is connected with one end of the first resistor and the first fixed end of the variable resistor, and the second fixed end of the variable resistor is connected with the movable end and is grounded together; the output end of the first operational amplifier is connected with the inverting input end and is connected with the non-inverting input end of the second operational amplifier and the first end of the sampling resistor; the second end of the sampling resistor is connected with one end of a third resistor, the other end of the third resistor is connected with the inverting input end of the second operational amplifier, and the second resistor is connected between the output end and the inverting input end of the second operational amplifier in a bridging way; the first end of sampling resistor connects first metal probe, and the second end of sampling resistor connects the second metal probe.
CN103969195a discloses a novel pH value detecting instrument based on optical method, the structural principle of which is shown in fig. 1, and the pH value detecting instrument comprises: the device comprises a microprocessor (1), an LCD (liquid crystal display) display (2), a keyboard (3), an LED driver (4), a dual-wavelength LED light source (5), a lens (6), a pH sensor (7), a sample cell (8), an optical filter (9), a lens (10) and a light intensity detector (11), wherein a Polyaniline (PANI) film synthesized on transparent conductive glass (ITO) by an electrochemical method is used as the pH sensor to realize the detection of the pH value of a solution.
CN104280443a discloses a method for manufacturing an OTFT pH sensor with high sensitivity and pH verification made by using the OTFT device, which comprises preparing a TFT device with a gate having a slot by using a commonly used manufacturing process of a semiconductor device, and packaging the device according to the existing packaging process. An OTFT pH sensor was fabricated by electrochemical deposition of an electronic polymer film in the gate grooved region.
CN107561143a discloses an intelligent pH sensor based on an ISFET, through integrating ISFET/REFET, thermistor, signal conditioning module, clock calendar module, LCD display, microcontroller and USB communication interface, the pH value signal of the water body is collected through ISFET/REFET ion sensitive probe, and then converted into voltage signal through differential current readout circuit, and sent to microcontroller for processing, and displayed in real time by LCD display, and also can upload measurement data through USB communication interface, thus meeting the detection requirement of automatic monitoring technology.
GB1714735.6 discloses a pH sensor for measuring pH in a measuring environment. The sensor includes: a reference electrode, a pH-sensitive electrode, and a controller for measuring a potential difference between the pH-sensitive electrode and the reference electrode, the measured potential difference being indicative of a pH value at the pH-sensitive electrode, the controller being operable to apply a voltage between the first and second electrodes to control the pH value at the pH-sensitive electrode, and to measure the potential difference between the pH-sensitive electrode and the reference electrode after applying the recalibration voltage.
JP2017-208553A discloses a measuring apparatus capable of measuring a state of a measurement object with high accuracy in various ways, comprising: a first electrode and a second electrode for forming an energizing path through a measurement object on a front side and measuring a conductivity of the measurement object; and a reference electrode and an ISFET for measuring a pH value of the measurement object, wherein a reference electrode of the reference electrode is disposed on a back side of the first electrode and the second electrode.
A novel pH-ISFET chip system research, wang Zumin, etc., electronic and informatics report, 200729 (10), research designs a novel ISFET/REFET/PRE sensor and signal detection circuit integrated chip system, adopts a commercial standard CMOS technology to realize basic integrated chips, explores and researches sensitive film preparation technology compatible with the integrated chips and related subsequent technology, and focuses on research on H prepared by an electric polymerization method + Sensitive PPy film, compared with an integrated chip developed by adopting a low-temperature Ta2O5 sensitive film technology, the integrated chipHas excellent performance with sensitivity of 54mV/pH, response time of 0.1s and linear correlation coefficient of 99.99% in the pH range of 1-12.
The conventional soil pH value detection method in the prior art is mainly characterized in that potential measurement is adopted in the core part, a series of test steps are adopted to obtain a relatively accurate soil pH value, the process is relatively complicated, the sensitivity is poor, the pH value detection method is influenced by environmental factors such as alkali metal ions, so that a relatively large measurement error is generated, and the requirements of blueberry planting are difficult to meet. The inventor finds that the requirement on the pH value of the soil in the blueberry planting is very high, and the pH value of the soil is required to be maintained in a narrow range in order to obtain the ideal yield and quality, so that the conventional device and method for detecting the pH value of the soil are difficult to meet the requirement. There is therefore a need in the art for a highly sensitive soil pH detection device and method suitable for use in blueberry planting.
Disclosure of Invention
In order to solve the problems, the inventor provides a soil pH value detection device for blueberry planting through intensive research and combined development. The detection can measure the pH value of the soil with high sensitivity and accuracy, thereby being suitable for the requirement of accurate and frequent detection of the pH value in the blueberry planting.
In one aspect of the present invention, there is provided a soil ph detecting device for blueberry planting, the device comprising: an ion-sensitive field effect transistor, an anode, a cathode, a reference electrode and a counter electrode.
Preferably, the ion sensitive field effect transistor comprises: substrate, drain electrode, source electrode, insulating film.
Preferably, the substrate is an N-doped silicon substrate.
Preferably, the drain and source are formed by doping two regions on the substrate with P.
Preferably, a channel is formed between the drain electrode and the source electrode, and an insulating film is positioned above the channel.
Preferably, the insulating film is an oxide film. More preferably, the insulating film is a rare earth oxide film.
Preferably, the soil pH value detection device is also integrated with a coulomb titration device.
Or in addition, the soil pH value detection device for blueberry planting comprises: substrate, drain, source, insulating film, cathode, anode, counter electrode, coulometric device, output signal (preferably current signal), channel, reference electrode.
In another aspect of the present invention, there is provided a method of using the soil ph detecting device for blueberry planting according to the foregoing, characterized in that the method comprises the steps of: (1) Standard soil samples with 20% of water content are prepared by using standard solutions with pH values of 4.00, 6.00, 8.00 and 10.00 and dried soil, and the soil pH value detection device is used for detection and calibration; (2) taking soil to be tested, and drying; (3) Distilled water is added into the soil to prepare a test sample with the water content of 20%, and the pH value of the test sample is detected and calculated.
Preferably, the temperature of both the standard soil sample and the test sample is 25 ℃.
Preferably, the calculation of the pH value is completed by an integrated circuit connected with a soil pH value detection device.
In a preferred embodiment of the present invention, the rare earth oxide film as the insulating film is Nd 2 O 3 And (3) a film. More preferably, the Nd 2 O 3 In crystalline form.
In a particularly preferred embodiment of the present invention, nd in the above-mentioned crystalline form 2 O 3 Having 400, 440 and 622 crystal planes.
Preferably, nd 2 O 3 The thickness of the film is 15-20nm. More preferably, nd 2 O 3 The film is formed by reactive sputter deposition on a substrate and rapid thermal annealing.
In a preferred embodiment, the rapid thermal annealing is performed by gradient thermal annealing. More preferably, the gradient thermal annealing procedure comprises: sequentially maintaining at 600deg.C for 30-60min, at 700deg.C for 90-120min, and at 800deg.C for 120-180min.
Preferably, the EIS (electrolyte-insulator-semiconductor) is fabricated on copper wires of a printed circuit board by forming conductive wires using silver gel, and the EIS structure and wires are encapsulated by epoxy encapsulation.
Nd for RTA by XRD for rapid thermal annealing 2 O 3 The crystal structure of the film was examined. X-ray diffraction patterns indicate that when the gradient rapid thermal annealing of the present invention is employed, the film contains Nd in a cubic phase structure 2 O 3 . When the gradient rapid thermal annealing of the present invention is employed, two larger (400) and (622) peak intensities, particularly (400) and (622) planes, are found in the XRD pattern, which is very pronounced, and this result shows diffusion of Nd from the film to the Si substrate, at Nd 2 O 3 A silicate layer is formed on the/Si interface. Nd with high k value due to the formation of thinner silicate layer and larger surface roughness 2 O 3 The film has good induction characteristics, including sensitivity in solution from pH1 to pH 13 as high as 59.44-60.76mV/pH, drift rate in buffer solution at pH 7 of 1.67-1.74mV/H, and shows high sensitivity to H + Is resistant to interference by other metal ions in the soil, such as sodium ions.
In a particularly preferred embodiment, the surface of the insulating film is applied with a polymer film. Preferably, the polymer film is a block polymer. More preferably, the polymer film is a copolymer film containing sodium sulfonate groups. The present inventors have made separate filed applications for this technical solution.
Particularly preferably, the polymer is a polymer of the following formula (1):
wherein the weight average molecular weight of the polymer is 3,000-50,000 and y=30-50.
The polymer can be prepared by copolymerizing sodium p-styrenesulfonate and N- (2-hydroxyethyl) acrylamide.
It was found that,when using the polymer membrane, micropores in the membrane allow for a smaller volume of H + Enter, especially sodium sulfonate group, is more beneficial to H in solution + Can prevent some of the larger volume metal ions such as transition metal ions and Ca 2+ Thereby improving detection sensitivity and anti-interference ability against other cations.
In a preferred embodiment, the insulating film is a composite film comprising Al from bottom to top 2 O 3 Film, pt film and Nd 2 O 3 And (3) a film. The present inventors also made separate applications for this technical solution.
When using a liner of Pt/Al 2 O 3 Nd of layer 2 O 3 When the film is used as an extended gate electrode, the film has the advantages of high sensitivity, short response time, high stability, high repeatability, high ion interference capability and the like. The Pt/Al 2 O 3 Layer improves Nd 2 O 3 The membrane pH sensor is resistant to sodium and potassium interfering ions.
Preferably, the Al 2 O 3 The film and the Pt film were subjected to sputter etching treatment to enhance the surface roughness, thereby improving Nd 2 O 3 For H + Is provided.
Drawings
Fig. 1 is a schematic diagram of the working principle of a soil ph detecting device for blueberry planting according to the present invention, wherein: 1 is a substrate, 2 is a drain electrode, 3 is a source electrode, 4 is an insulating film, 5 is a cathode, 6 is an anode, 7 is a counter electrode, 8 is a coulometric titration apparatus, 9 is an output signal (typically a current signal), 10 is a channel, and 11 is a reference electrode.
FIG. 2 is a gradient rapid annealing Nd according to the invention 2 O 3 XRD pattern of the film.
Detailed description of the preferred embodiments
The present invention will be described in further detail with reference to examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
As described with reference to fig. 1, a soil ph detecting device for blueberry planting includes: a substrate 1, a drain electrode 2, a source electrode 3, an insulating film 4, a cathode 5, an anode 6, a counter electrode 7, a coulometric titration apparatus 8, and an output signal 9, which is a current signal, a channel 10, a reference electrode 11, and an insulating film 4 of Nd 2 O 3 Film thickness of 16nm, nd 2 O 3 The film was deposited on the substrate by reactive sputtering (Nd target available from positive metallurgical technology company in shenzhen, sputtering done on a converging sputtering machine) and rapid thermal annealing by gradient thermal annealing, the gradient thermal annealing procedure comprising: the temperature was maintained at 600℃for 45min, at 700℃for 90min, and at 800℃for 120min in this order. The pH value detection device has an error of 0.39% within a pH value range of 1-13 through a comparison test with a standard substance.
Comparative example 1
Example 1 was repeated with the only difference that Nd 2 O 3 The film was not gradient annealed, but was maintained directly at 800 ℃ for 120min. The device was tested against the standard and had an error of 0.72% over a pH range of 1-13.
Comparative example 2
Example 1 was repeated except that the insulating film 4 was Ta 2 O 5 And (3) a film. The device was tested against the standard and had an error of 0.94% over a pH range of 1-13.
As is clear from the above examples and comparative examples, nd 2 O 3 The accuracy of the soil pH value detection device prepared by the film is obviously higher than that of Ta 2 O 5 A device for preparing the membrane. In addition, it was not previously thought that gradient annealed Nd 2 O 3 The accuracy of the soil pH value detection device prepared by the film is obviously higher than that prepared by single-temperature annealing 2 O 3 And a membrane device.
This written description uses examples to disclose the invention, including the best mode, and also to enable any person skilled in the art to make and use the invention. The patentable scope of the invention is defined by the claims, and may include other examples that occur to those skilled in the art. Such other examples are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal languages of the claims. All references referred to herein are incorporated by reference to the extent not inconsistent herewith.
Claims (8)
1. A soil pH valve detection device for blueberry planting, its characterized in that, the device includes: an ion sensitive field effect transistor, an anode, a cathode, a reference electrode, and a counter electrode, the ion sensitive field effect transistor comprising: a substrate, a drain electrode, a source electrode and an insulating film, wherein the insulating film is Nd 2 O 3 A film of Nd 2 O 3 In crystalline form, nd 2 O 3 Has 400 crystal face, 440 crystal face and 622 crystal face, nd 2 O 3 The thickness of the film is 15-20nm, nd 2 O 3 The film is deposited on the substrate by reactive sputtering and is rapidly thermally annealed;
a polymer film is applied to the surface of the insulating film, and the polymer film is a copolymer film containing sodium sulfonate groups:wherein the weight average molecular weight of the polymer is 3,000-50,000 and y=30-50.
2. The soil ph detection device for blueberry planting as defined in claim 1, wherein the substrate is an N-doped silicon substrate.
3. The soil ph detecting apparatus for blueberry planting according to claim 1 or 2, wherein the drain electrode and the source electrode are formed by doping P in two regions on a substrate.
4. The soil ph detecting device for blueberry planting as recited in claim 3, wherein a channel is formed between the drain electrode and the source electrode, and the insulating film is located above the channel.
5. The soil ph detecting device for blueberry planting according to claim 1 or 2, wherein the soil ph detecting device is further integrated with a coulomb titration device.
6. A method of using the soil ph detection device for blueberry planting as claimed in any one of the preceding claims, the method comprising the steps of: (1) Standard soil samples with 20% of water content are prepared by using standard solutions with pH values of 4.00, 6.00, 8.00 and 10.00 and dried soil, and the soil pH value detection device is used for detection and calibration; (2) taking soil to be tested, and drying; (3) Distilled water is added into the soil to prepare a test sample with the water content of 20%, and the pH value of the test sample is detected and calculated.
7. The method of claim 6, wherein the standard soil sample and the test sample are each at a temperature of 25 ℃.
8. The method of claim 6, wherein the pH calculation is performed by an integrated circuit coupled to a soil pH detection device.
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| CN202110062449.0A CN112858426B (en) | 2021-01-18 | 2021-01-18 | Soil pH value detection device for blueberry planting |
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| CN202110062449.0A CN112858426B (en) | 2021-01-18 | 2021-01-18 | Soil pH value detection device for blueberry planting |
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|---|---|---|---|---|
| TWI295729B (en) * | 2005-11-01 | 2008-04-11 | Univ Nat Yunlin Sci & Tech | Preparation of a ph sensor, the prepared ph sensor, systems comprising the same, and measurement using the systems |
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| CN104937402A (en) * | 2013-01-25 | 2015-09-23 | 威立雅水务解决方案与技术支持公司 | Ph value measuring device comprising in situ calibration means |
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| Structural Properties and Sensing Characteristics of Thin Nd2O3 Sensing Films for pH Detection;Tung-Ming Pan et al.;《Electrochemical and Solid-State Letters》;20090805;第12卷(第10期);第J96-J99页 * |
| Structural Properties and Sensing Characteristics of Thin Nd2O3 Sensing Films for pH Detection;Tung-Ming Pan et al.;Electrochemical and Solid-State Letters;第12卷(第10期);第J96-J99页 * |
| 新型pH-ISFET芯片系统研究;汪祖民 等;《电子与信息学报》;20071031;第29卷(第10期);第2525-2528页 * |
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