Organic nanowire for pneumoconiosis detection electronic nose and detection method thereof

Abstract

The invention discloses an organic nanowire for an electronic nose for pneumoconiosis detection and a detection method thereof, and the detection method comprises the following steps: representing the organic nanowire by SEM and XRD to judge whether the morphological characteristics of the organic nanowire are qualified, applying a load to an organic nanowire sample, and calculating the hardness value of the organic nanowire according to the load, preparing an indirectly-heated gas-sensitive element from the organic nanowires to test the sensitive characteristics of the indirectly-heated gas-sensitive element to different gases, and judging whether the gas-sensitive property and the mechanical property are qualified or not according to the hardness value and the sensitive characteristics; the diameter of the nanowire is smaller, the surface area is larger, the oxygen adsorption amount is increased, so that the gas-sensitive performance is improved, precious metal doping plays a good catalytic role, the activation energy of chemical adsorption of detected gas can be effectively reduced, the sensitivity of gas detection is improved, and the application prospect is wide. The detection method provided by the invention can realize accurate, effective and low-cost detection of the mechanical properties and gas-sensitive properties of the nanowire product, and ensures the quality of the nanowire for the electronic nose.

Description

Technical Field

[0001] The present invention relates to the technical field of organic nanowires, and in particular to an organic nanowire for a pneumoconiosis detection electronic nose and a detection method and application thereof. Background Art

[0002] Pneumoconiosis generally refers to pneumoconiosis, which is a systemic disease characterized by diffuse fibrosis (scarring) of lung tissue caused by long-term inhalation of industrial dust (dust) during occupational activities and its retention in the lungs. Pneumoconiosis can be divided into inorganic pneumoconiosis and organic pneumoconiosis according to the type of inhaled dust. Pneumoconiosis caused by inhalation of inorganic dust during production labor is called inorganic pneumoconiosis. Most pneumoconiosis are inorganic pneumoconiosis. Pneumoconiosis caused by inhalation of organic dust is called organic pneumoconiosis, such as asbestosis and farmer's lung.

[0003] An electronic nose is an electronic system that uses the response pattern of a gas sensor array to identify odors. It can continuously and in real time monitor the odor conditions at a specific location over a period of hours, days, or even months. Based on this principle, researchers have proposed an integrated sensing system that can realize the functions of an electronic nose and have developed a set of renewable technologies for its production. This device is a flexible electronic platform that can analyze exhaled gases and identify lesions of the respiratory tract and organs. Since the composition of the exhaled gases of pneumoconiosis patients and normal people is different, the electronic nose can detect whether a person has pneumoconiosis by identifying the composition of the person's exhaled gases.

[0004] Existing electronic nose products are mainly composed of three functional devices: an odor sampling operator, a gas sensor array, and a signal processing system. Nanowires are usually used as sensitive materials in the gas sensor array. However, most of the existing nanowires for electronic noses have a single component, resulting in low mechanical properties and gas-sensitive properties, limited application range, and no good application prospects. After the production of the nanowires for electronic noses is completed, there is a lack of accurate, effective and low-cost detection methods for the mechanical properties and gas-sensitive properties of the nanowire products, resulting in an inability to accurately determine whether the produced nanowires for electronic noses meet the requirements for electronic nose use, which affects the pneumoconiosis detection efficiency of the electronic nose to a certain extent. Therefore, the present invention proposes an organic nanowire for pneumoconiosis detection electronic nose and a detection method and application thereof to solve the problems existing in the prior art. Summary of the invention

[0005] In view of the above problems, the purpose of the present invention is to propose an organic nanowire for electronic nose for pneumoconiosis detection and a detection method thereof, which solves the problem that most of the existing organic nanowires for electronic noses have a single component, resulting in low mechanical properties and gas-sensing properties, and the lack of accurate, effective and low-cost detection methods for the mechanical properties and gas-sensing properties of the nanowire products after the production of the nanowires for electronic noses is completed.

[0006] In order to achieve the purpose of the present invention, the present invention is implemented through the following technical scheme: an organic nanowire for an electronic nose for pneumoconiosis detection comprises the following raw materials in parts by weight: 50 to 60 parts of zinc oxide, 10 to 15 parts of nanosilver, 5 to 10 parts of nickel, 5 to 10 parts of rare earth elements and 15 to 20 parts of organic semiconductor materials.

[0007] A further improvement is that the nickel is prepared by electrolysis, specifically, first roasting the enriched sulfide ore into oxides, then reducing the oxides into crude nickel with carbon, and then electrolyzing the crude nickel to obtain pure metallic nickel.

[0008] A further improvement is that the organic nanowires are prepared by physical evaporation in a high-temperature vacuum atmosphere tube furnace, using helium as a carrier gas and oxygen as a reaction gas, and are purified by ultraviolet light excitation after preparation.

[0009] A method for detecting organic nanowires for an electronic nose for detecting pneumoconiosis comprises the following steps:

[0010] Step 1: first characterize the organic nanowires prepared by physical evaporation method and excited by violet light by SEM and XRD, and judge whether their morphological characteristics are qualified according to the characterization results, and then put the organic nanowires with qualified morphological characteristics into a sealed container as organic nanowire samples for storage;

[0011] Step 2: first place the organic nanowire sample in step 1 under a scanning probe microscope, then use the SPM probe to apply a load to the organic nanowire sample, and use the scanning probe microscope to accurately locate and in-situ observe the organic nanowire sample where the load is applied, and then calculate the hardness value of the organic nanowire sample based on the indentation projection area and indentation depth at the organic nanowire sample where the load is applied;

[0012] Step 3: First, the organic nanowire sample tested in step 2 is mixed with distilled water, and then the mixed solution is coated on the surface of the ceramic tube to form a gas-sensitive film, and then a resistance wire is installed on the dried ceramic tube and welded to the base to make a indirectly heated gas sensor, and then the indirectly heated gas sensor is placed in a container filled with different gases and the sensitive characteristics of the indirectly heated gas sensor to different gases are tested;

[0013] Step 4: Compare and analyze the hardness value of the organic nanowire sample calculated in step 2 with the standard hardness value, and judge whether its mechanical properties are qualified based on the comparative analysis results. Then, compare and analyze the sensitive characteristics of the indirectly heated gas sensor tested in step 3 with the standard sensitive characteristics, and judge whether its gas sensing performance is qualified based on the comparative analysis results.

[0014] A further improvement is that in step 1, the specific steps of characterizing by SEM and XRD are: firstly observing the surface morphology of the organic nanowires by a scanning electron microscope, and then characterizing the phase structure, phase composition and grain size of the organic nanowires by an X-ray diffractometer, and the scanning method is continuous scanning.

[0015] A further improvement is that in step 2, the indentation projection area A of the organic nanowire sample where the load is applied is c The calculation formula is:

[0016] A c =ε·h c2

[0017] Among them, h c is the indentation depth, ε is a constant and is related to the shape of the SPM probe. The hardness value H of the organic nanowire sample is calculated as follows:

[0018]

[0019] Among them, F max is the maximum load.

[0020] A further improvement is that in step three, after the ceramic tube is coated with the blended solution, it is dried in a dryer, and the drying temperature is set at 60-80°C and the drying time is 15-20 minutes. After drying, it is naturally cooled to room temperature and then taken out.

[0021] A further improvement is that in step three, when the indirectly heated gas sensor detects different gases, its gas-sensitive film interacts with the gas to be measured, causing the film quality and conductivity of the gas-sensitive film to change, thereby causing the surface acoustic wave frequency of the ceramic tube to drift, and then the sensitive characteristics of the indirectly heated gas sensor are characterized according to the drift change value of the surface acoustic wave frequency.

[0022] The beneficial effects of the present invention are as follows: the present invention uses zinc oxide as a main material, nano silver, nickel, rare earth elements and organic semiconductor materials as auxiliary materials to prepare organic nanowires and uses ultraviolet light for excitation, so that the prepared nanowires have a thinner diameter and a larger surface area, and the oxygen adsorption amount is increased, thereby improving the gas sensing performance; the noble metal doping plays a good catalytic role, can effectively reduce the activation energy of chemical adsorption of the detected gas, improve the sensitivity of gas detection, and shorten the response time; the ultraviolet light excitation introduces a large number of electrons and holes, so that the number of carriers increases sharply, the conductivity increases, the resistance decreases sharply, and the gas sensitivity is further improved; the addition of rare earth elements can improve the selectivity of organic nanowires for specific gas detection, thereby improving the sensitivity for specific gas detection;

[0023] In addition, the present invention first characterizes the organic nanowires by SEM and XRD to determine whether their morphological characteristics are qualified, then uses a scanning probe microscope to apply a load to the organic nanowire sample and calculates its hardness value based on this, and then the organic nanowires are made into a side-heated gas sensor to test its sensitive characteristics to different gases, thereby achieving accurate, effective and low-cost detection of the mechanical properties and gas-sensing properties of the nanowire products, thereby ensuring the quality of the nanowires used in the electronic nose. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0025] Figure 1 It is a schematic flow chart of the detection method of the present invention. DETAILED DESCRIPTION

[0026] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0027] Embodiment 1

[0028] The present embodiment provides an organic nanowire for an electronic nose for detecting pneumoconiosis, comprising the following raw materials in parts by weight: 50 parts of zinc oxide, 15 parts of nanosilver, 10 parts of nickel, 10 parts of rare earth elements and 15 parts of organic semiconductor materials, wherein the nickel is prepared by electrolysis, specifically: firstly roasting the enriched sulfide ore into oxides, then reducing the oxides into crude nickel with carbon, and then electrolyzing the crude nickel to obtain pure metallic nickel. The organic nanowires in the present embodiment are prepared by a high-temperature vacuum atmosphere tubular furnace through physical evaporation, using helium as a carrier gas and oxygen as a reaction gas, and are purified by ultraviolet light excitation after preparation.

[0029] Specifically, the pre-prepared zinc oxide, nanosilver, nickel, rare earth elements and organic semiconductor materials are first mixed and ground into a mixed powder, and then the mixed powder is poured into an alumina container and sent into a high-temperature vacuum atmosphere tube furnace for high-temperature heating. During the heating process, a certain amount of helium is first introduced, and then a certain amount of oxygen is introduced. The temperature is kept until the reaction of the mixed powder is completed, and the obtained reaction precipitate is the organic nanowire.

[0030] See also Figure 1 This embodiment also provides a method for detecting organic nanowires for an electronic nose for detecting pneumoconiosis, comprising the following steps:

[0031] Step 1: firstly characterize the organic nanowires prepared by physical evaporation method and excited by violet light by SEM and XRD, and judge whether their morphological characteristics are qualified according to the characterization results, and then put the organic nanowires with qualified morphological characteristics into a sealed container as organic nanowire samples for storage. The specific steps of characterization by SEM and XRD are: firstly observe the surface morphology of the organic nanowires by scanning electron microscope, and then characterize the phase structure, phase composition and grain size of the organic nanowires by X-ray diffractometer, and the scanning mode is continuous scanning;

[0032] Step 2: First, place the organic nanowire sample in step 1 under a scanning probe microscope, then use the SPM probe to apply a load to the organic nanowire sample, and use the scanning probe microscope to accurately locate and in-situ observe the organic nanowire sample where the load is applied, and then calculate the hardness value of the organic nanowire sample based on the indentation projection area and indentation depth where the load is applied to the organic nanowire sample. The indentation projection area A of the organic nanowire sample where the load is applied is c The calculation formula is:

[0033] A c =ε·h c2

[0034] Among them, h c is the indentation depth, ε is a constant and is related to the shape of the SPM probe. The hardness value H of the organic nanowire sample is calculated as follows:

[0035]

[0036] Among them, f max is the maximum load;

[0037] Step 3: First, the organic nanowire sample tested in step 2 is mixed with distilled water, and then the mixed solution is applied to the surface of the ceramic tube to form a gas-sensitive film. After the ceramic tube is coated with the mixed solution, it is dried in a dryer, and the drying temperature is set to 60°C and the drying time is 20 minutes. After drying, it is naturally cooled to room temperature and then taken out. Then, a resistance wire is added to the dried ceramic tube and welded to the base to make a indirectly heated gas sensor. Then, the indirectly heated gas sensor is placed in a container filled with different gases and the sensitive characteristics of the indirectly heated gas sensor to different gases are tested;

[0038] Step 4: Compare and analyze the hardness value of the organic nanowire sample calculated in step 2 with the standard hardness value, and judge whether its mechanical properties are qualified based on the comparative analysis results. Then, compare and analyze the sensitive characteristics of the indirectly heated gas sensor tested in step 3 with the standard sensitive characteristics, and judge whether its gas sensing performance is qualified based on the comparative analysis results. When the indirectly heated gas sensor detects different gases, its gas sensitive film interacts with the gas to be tested, causing the film quality and conductivity of the gas sensitive film to change, thereby causing the surface acoustic wave frequency of the ceramic tube to drift, and then the sensitive characteristics of the indirectly heated gas sensor are characterized based on the drift change value of the surface acoustic wave frequency.

[0039] Embodiment 2

[0040] The present embodiment provides an organic nanowire for an electronic nose for detecting pneumoconiosis, comprising the following raw materials in parts by weight: 60 parts of zinc oxide, 10 parts of nanosilver, 5 parts of nickel, 5 parts of rare earth elements and 20 parts of organic semiconductor materials, wherein the nickel is prepared by electrolysis, specifically: firstly roasting the enriched sulfide ore into oxides, then reducing the oxides into crude nickel with carbon, and then electrolyzing the crude nickel to obtain pure metallic nickel. The organic nanowires in the present embodiment are prepared by a high-temperature vacuum atmosphere tubular furnace through physical evaporation, using helium as a carrier gas and oxygen as a reaction gas, and are purified by ultraviolet light excitation after preparation.

[0041] Specifically, the pre-prepared zinc oxide, nano silver, nickel, rare earth elements and organic semiconductor materials are first mixed and ground into a mixed powder, and then the mixed powder is poured into an alumina container and sent into a high-temperature vacuum atmosphere tube furnace for high-temperature heating. During the heating process, a certain amount of helium is first introduced, and then a certain amount of oxygen is introduced, and the temperature is kept until the reaction of the mixed powder is completed. The reaction precipitate obtained is the organic nanowire.

[0042] See also Figure 1This embodiment also provides a method for detecting organic nanowires for an electronic nose for detecting pneumoconiosis, comprising the following steps:

[0043] Step 1: firstly characterize the organic nanowires prepared by physical evaporation method and excited by violet light by SEM and XRD, and judge whether their morphological characteristics are qualified according to the characterization results, and then put the organic nanowires with qualified morphological characteristics into a sealed container as organic nanowire samples for storage. The specific steps of characterization by SEM and XRD are: firstly observe the surface morphology of the organic nanowires by scanning electron microscope, and then characterize the phase structure, phase composition and grain size of the organic nanowires by X-ray diffractometer, and the scanning mode is continuous scanning;

[0044] Step 2: First, place the organic nanowire sample in step 1 under a scanning probe microscope, then use the SPM probe to apply a load to the organic nanowire sample, and use the scanning probe microscope to accurately locate and in-situ observe the organic nanowire sample where the load is applied, and then calculate the hardness value of the organic nanowire sample based on the indentation projection area and indentation depth where the load is applied to the organic nanowire sample. The indentation projection area A of the organic nanowire sample where the load is applied is c The calculation formula is:

[0045] A c =ε·h c2

[0046] Among them, h c is the indentation depth, ε is a constant and is related to the shape of the SPM probe. The hardness value H of the organic nanowire sample is calculated as follows:

[0047]

[0048] Among them, F max is the maximum load;

[0049] Step 3: First, the organic nanowire sample tested in step 2 is mixed with distilled water, and then the mixed solution is applied to the surface of the ceramic tube to form a gas-sensitive film. After the ceramic tube is coated with the mixed solution, it is dried in a dryer, and the drying temperature is set to 80°C and the drying time is 15 minutes. After drying, it is naturally cooled to room temperature and then taken out. Then, a resistance wire is added to the dried ceramic tube and welded to the base to make a indirectly heated gas sensor. Then, the indirectly heated gas sensor is placed in a container filled with different gases and the sensitive characteristics of the indirectly heated gas sensor to different gases are tested;

[0050] Step 4: Compare and analyze the hardness value of the organic nanowire sample calculated in step 2 with the standard hardness value, and judge whether its mechanical properties are qualified based on the comparative analysis results. Then, compare and analyze the sensitive characteristics of the indirectly heated gas sensor tested in step 3 with the standard sensitive characteristics, and judge whether its gas sensing performance is qualified based on the comparative analysis results. When the indirectly heated gas sensor detects different gases, its gas sensitive film interacts with the gas to be tested, causing the film quality and conductivity of the gas sensitive film to change, thereby causing the surface acoustic wave frequency of the ceramic tube to drift, and then the sensitive characteristics of the indirectly heated gas sensor are characterized based on the drift change value of the surface acoustic wave frequency.

[0051] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. An organic nanowire for electronic nose for pneumoconiosis detection, characterized by: The invention comprises the following raw materials in parts by weight: 50-60 parts of zinc oxide, 10-15 parts of nano silver, 5-10 parts of nickel, 5-10 parts of rare earth elements and 15-20 parts of organic semiconductor materials.

2. The organic nanowire for electronic nose for pneumoconiosis detection according to claim 1, characterized in that: The nickel is prepared by electrolysis, specifically, first roasting the enriched sulfide ore into oxides, then reducing the oxides into crude nickel with carbon, and then electrolyzing the crude nickel to obtain pure metallic nickel.

3. The organic nanowire for electronic nose for pneumoconiosis detection according to claim 1, characterized in that: The organic nanowires are prepared by a high-temperature vacuum atmosphere tube furnace through a physical evaporation method, using helium as a carrier gas and oxygen as a reaction gas, and are purified by ultraviolet light excitation after preparation.

4. A detection method for organic nanowires for electronic nose for pneumoconiosis detection as claimed in claim 1, characterized in that: The following steps are involved: Step 1: first characterize the organic nanowires prepared by physical evaporation method and excited by violet light by SEM and XRD, and judge whether their morphological characteristics are qualified according to the characterization results, and then put the organic nanowires with qualified morphological characteristics into a sealed container as organic nanowire samples for storage; Step 2: first place the organic nanowire sample in step 1 under a scanning probe microscope, then use the SPM probe to apply a load to the organic nanowire sample, and use the scanning probe microscope to accurately locate and in-situ observe the organic nanowire sample where the load is applied, and then calculate the hardness value of the organic nanowire sample based on the indentation projection area and indentation depth at the organic nanowire sample where the load is applied; Step 3: First, the organic nanowire sample tested in step 2 is mixed with distilled water, and then the mixed solution is coated on the surface of the ceramic tube to form a gas-sensitive film, and then a resistance wire is installed on the dried ceramic tube and welded to the base to make a indirectly heated gas sensor, and then the indirectly heated gas sensor is placed in a container filled with different gases and the sensitive characteristics of the indirectly heated gas sensor to different gases are tested; Step 4: Compare and analyze the hardness value of the organic nanowire sample calculated in step 2 with the standard hardness value, and judge whether its mechanical properties are qualified based on the comparative analysis results. Then, compare and analyze the sensitive characteristics of the indirectly heated gas sensor tested in step 3 with the standard sensitive characteristics, and judge whether its gas sensing performance is qualified based on the comparative analysis results.

5. The method for preparing an organic nanowire for an electronic nose for pneumoconiosis detection according to claim 4, characterized in that: In the step 1, the specific steps of characterizing by SEM and XRD are: firstly observe the surface morphology of the organic nanowires by scanning electron microscope, and then characterize the phase structure, phase composition and grain size of the organic nanowires by X-ray diffractometer, and the scanning mode is continuous scanning.

6. The method for preparing an organic nanowire for an electronic nose for pneumoconiosis detection according to claim 4, characterized in that: In the step 2, the indentation projection area A of the organic nanowire sample where the load is applied c The calculation formula is: A c =e·h c2 Among them, h c is the indentation depth, ε is a constant and is related to the shape of the SPM probe. The hardness value H of the organic nanowire sample is calculated as follows: Among them, F max is the maximum load.

7. The method for preparing an organic nanowire for an electronic nose for pneumoconiosis detection according to claim 4, characterized in that: In the step three, after the ceramic tube is coated with the blended solution, it is dried in a drying machine, and the drying temperature is set at 60-80° C. and the drying time is 15-20 minutes. After the drying is completed, it is naturally cooled to room temperature and then taken out.

8. The method for preparing organic nanowires for electronic nose for pneumoconiosis detection according to claim 4, characterized in that: In the step three, when the indirectly heated gas sensor detects different gases, its gas-sensitive film interacts with the gas to be measured, causing the film quality and conductivity of the gas-sensitive film to change, thereby causing the surface acoustic wave frequency of the ceramic tube to drift, and then the sensitive characteristics of the indirectly heated gas sensor are characterized according to the drift change value of the surface acoustic wave frequency.

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