CN110849939A - Doped ZnO material and preparation method thereof and acetone sensor - Google Patents
Doped ZnO material and preparation method thereof and acetone sensor Download PDFInfo
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Abstract
The invention discloses a doped ZnO material, a preparation method thereof and an acetone sensor, wherein the method comprises the following steps: mixing a zinc source with water, stirring until the zinc source is dissolved, then adding an alkali source and absolute ethyl alcohol, and stirring until a clear solution is obtained; adding a soluble gold source or a soluble palladium source into the clarified solution, and transferring the obtained solution into a microwave reactor for reaction; and after the reaction is finished, sequentially cooling, washing, drying and annealing to obtain the Au or Pd doped ZnO material. The invention adopts a one-step microwave hydrothermal method to directly dope Au or Pd into the ZnO material, and has the advantages of easy preparation operation and simple process. Compared with common physical doping, the method of the invention has the advantages that the dopant is dispersed more uniformly, and the components in the synthesized composite material can be contacted on the molecular level. The acetone sensor based on the Au or Pd doped ZnO material shows better gas-sensitive property to low-concentration acetone.
Description
Technical Field
The invention relates to the field of gas sensors, in particular to a doped ZnO material, a preparation method thereof and an acetone sensor.
Background
The current primary method of blood glucose detection and monitoring is invasive, i.e., drawing blood by needle-pricking a fingertip or a vein. Some patients need to prick their fingers to obtain blood data even seven times a day, which causes pain and inconvenience to the patients. Meanwhile, the test paper is used throughout the year, so that the family of the patient is subjected to great economic pressure. Recent studies have shown that acetone in breath can be an important marker for monitoring diabetes. However, most of the existing detection means of acetone in breath are large-scale instruments such as chromatography, mass spectrometry, spectrometers and the like, and the detection means needs to be operated by professional personnel and is expensive, so that much inconvenience is brought to detection.
At present, ZnO sensors for detecting acetone have been researched and reported, but the sensors have the defects of high working temperature, poor selectivity, high detection concentration, poor moisture resistance, slow response-recovery speed and the like, and are not suitable for being used as breath marker sensors. Some researchers have proved that doping of noble metals Au and Pd can effectively improve the gas-sensitive property of ZnO acetone, but the research of realizing ultralow concentration (several-dozens of ppb) acetone, low temperature, high selection, moisture resistance and rapid detection is still challenging.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a doped ZnO material, a method for preparing the same, and an acetone sensor, which are used to solve the problems of high operating temperature, poor selectivity, high detection concentration, poor moisture resistance, slow response-recovery rate, etc. of the existing sensors.
The technical scheme of the invention is as follows:
a preparation method of a doped ZnO material comprises the following steps:
mixing a zinc source with water, stirring until the zinc source is dissolved, then adding an alkali source and absolute ethyl alcohol, and stirring until a clear solution is obtained;
adding a soluble gold source or a soluble palladium source into the clarified solution, and transferring the obtained solution into a microwave reactor for reaction;
and after the reaction is finished, sequentially cooling, washing, drying and annealing to obtain the Au or Pd doped ZnO material.
Further, the reaction temperature is 140-180 ℃; and/or the reaction time is 30-60 min.
Further, the annealing temperature is 400-550 ℃; and/or the annealing time is 2-5 h.
Further, the molar ratio of the zinc source to the alkali source to the soluble gold source is 1: 22-44: 0-0.077; or
The molar ratio of the zinc source, the alkali source and the soluble palladium source is 1: 22-44: 0-0.088.
Further, the zinc source is selected from one or more of zinc acetate, zinc chloride and zinc nitrate; and/or
The alkali source is selected from one of potassium hydroxide and sodium hydroxide.
Further, the soluble gold source is one or more of chloroauric acid, gold nitrate, gold chloride and gold acetate.
Further, the soluble palladium source is one or more of palladium nitrate, palladium chloride and palladium sulfate.
The doped ZnO material is prepared by the preparation method of the doped ZnO material.
Further, based on the doped ZnO material, the Au accounts for 0-6% of the doped ZnO material by mass; or
The Pd accounts for 0-7% of the mass percent of the doped ZnO material.
An acetone sensor comprises a ceramic tube, wherein the surface of the ceramic tube is coated with a doped ZnO material prepared by the method; and/or
The surface of the ceramic tube is coated with the doped ZnO material.
Has the advantages that: the invention adopts a one-step microwave hydrothermal method to directly dope Au or Pd into the ZnO material, and has the advantages of easy preparation operation and simple process. Compared with common physical doping, the method of the invention has the advantages that the dopant is dispersed more uniformly, and the components in the synthesized composite material can be contacted on the molecular level. The acetone sensor based on the Au or Pd doped ZnO material shows better gas-sensitive property to low-concentration acetone, and has the advantages of low working temperature, high sensitivity, wide detection range (5ppb-100ppm), excellent selectivity and quick response speed.
Drawings
FIG. 1: a) the X-ray diffraction patterns of Au/ZnO, Pd/ZnO and undoped ZnO materials provided by the embodiment are shown in (b-e) a scanning electron microscope image, a transmission electron microscope image, a high-resolution transmission electron microscope image and a selected area electron diffraction image of undoped ZnO respectively, f) a Pd/ZnO transmission electron microscope image, (g-i) a transmission electron microscope image, a high-resolution transmission electron microscope image and a selected area electron diffraction image of Au/ZnO respectively, and (j-k) X-ray photoelectron spectra of Au/ZnO and Pd/ZnO respectively.
FIG. 2: a) the sensitivity curves of the Au/ZnO and Pd/ZnO and undoped ZnO materials provided for the examples at different operating temperatures for 100ppm acetone gas, b) the selectivities of Au/ZnO and Pd/ZnO and undoped ZnO for different gases, c) the sensitivities of Au/ZnO and Pd/ZnO and undoped ZnO for different concentrations of acetone gas (low concentration), d) the sensitivities of Au/ZnO and Pd/ZnO and undoped ZnO for different concentrations of acetone gas (high concentration).
Detailed Description
The invention provides a doped ZnO material, a preparation method thereof and an acetone sensor, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and more clear and definite. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of a doped ZnO material, which comprises the following steps:
s10, mixing a zinc source with water, stirring until the zinc source is dissolved, then adding an alkali source and absolute ethyl alcohol, and stirring until a clear solution is obtained;
s20, adding a soluble gold source or a soluble palladium source into the clear solution, and transferring the obtained solution into a microwave reactor for reaction;
and S30, after the reaction is finished, cooling, washing, drying and annealing are sequentially carried out, so that the Au or Pd doped ZnO material is obtained.
In the prior art, metal oxides are generally synthesized and then dopants are added to the oxides by physical methods of impregnation. In the embodiment, Au or Pd is directly doped into the ZnO material by adopting a one-step microwave hydrothermal method, the preparation operation is easy, and the process is simple. Compared with common physical doping, the method has the advantages that the dopant is dispersed more uniformly, and the components in the synthesized composite material can be contacted on a molecular layer. The acetone sensor based on the Au or Pd doped ZnO material in the embodiment has good gas-sensitive property for low-concentration acetone, and has the advantages of low working temperature, high sensitivity, wide detection range (5ppb-100ppm), excellent selectivity and fast response speed.
Noble metal (Au and Pd)) doping can not only change the energy band structure of the material and increase the number of active sites, but also catalyze and activate gas reaction. In addition, the doped ZnO material synthesized by the one-step microwave hydrothermal method has small particle size (nanometer level) and a porous structure, and improves the gas permeation efficiency and the contact area with the material. The sensitivity of the sensor to acetone can therefore be enhanced by the addition of different noble metals, which provides a new approach to the fabrication of ultra low concentration (ppb) acetone sensors.
In one embodiment, the molar ratio of the zinc source, the alkali source and the soluble gold source is 1: 22-44: 0-0.077; or
The molar ratio of the zinc source, the alkali source and the soluble palladium source is 1: 22-44: 0-0.088. The doping of a very small amount of noble metal can avoid the noble metal covering ZnO active sites, which is not favorable for gas-sensitive characteristics.
In one embodiment, step S10 includes: pouring the zinc source into a beaker, adding distilled water, stirring until the zinc source particles are completely dissolved, then adding the alkali source, then adding absolute ethyl alcohol, and stirring until a clear solution is obtained.
In one embodiment, the zinc source is selected from one or more of the group consisting of zinc salts readily soluble in water, such as zinc acetate, zinc chloride, and zinc nitrate.
In one embodiment, the alkali source is selected from one of potassium hydroxide, sodium hydroxide, and the like.
In one embodiment, step S20 includes: adding a soluble gold source or a soluble palladium source into the clarified solution, transferring the obtained solution into a microwave reactor, setting the temperature of the microwave reactor, and reacting for a period of time at the high temperature.
In one embodiment, the soluble gold source is chloroauric acid, gold nitrate, gold chloride, gold acetate, and the like, without limitation.
In one embodiment, the soluble palladium source is palladium nitrate, palladium chloride, palladium sulfate, and the like, without limitation.
In one embodiment, the temperature of the reaction is 140 to 180 ℃. The temperature required by ZnO crystallization is ensured in the temperature range.
In one embodiment, the reaction time is 30 to 60 min. The ZnO is ensured to be completely crystallized in the time range.
In one embodiment, step S30 includes: and after the reaction is finished, cooling, taking out, washing, drying, and then putting into a muffle furnace for annealing to obtain the Au or Pd doped ZnO material.
In one embodiment, the annealing temperature is 400 to 550 ℃. The aim is to burn off the organic constituents of the material and to avoid secondary crystallization at too high temperatures.
In one embodiment, the annealing time is 2 to 5 hours.
The embodiment of the invention provides a doped ZnO material, wherein the doped ZnO material is prepared by the preparation method of the doped ZnO material.
In one embodiment, based on the doped ZnO material, the Au accounts for 0-6% of the doped ZnO material by mass; or
The Pd accounts for 0-7% of the mass percent of the doped ZnO material. The doping of a small amount of noble metal can avoid the noble metal covering ZnO active sites, which is not favorable for gas-sensitive characteristics.
The embodiment of the invention provides an acetone sensor, which comprises a ceramic tube, wherein the surface of the ceramic tube is coated with a doped ZnO material prepared by the method in the embodiment of the invention; and/or the surface of the ceramic tube is coated with the doped ZnO material according to the embodiment of the invention.
In this embodiment, the ceramic tube may be indirectly heated Al2O3A tube. The doped ZnO material of the embodiment is made into paste and coated on a ceramic tube, a pair of Au electrodes are arranged at two ends of the ceramic tube, a nickel-chromium alloy coil is inserted in the middle of the tube to provide the working temperature of a testing element, a device and a heating wire are welded on a six-pin base, and the device and the heating wire are aged after being dried under an infrared lamp. The gas-sensitive characteristic test of the material is carried out in a CGS-8 type gas-sensitive element characteristic tester produced by Beijing Elite technology Limited under the test condition of 25% +/-5% relative humidity. The sensitivity of the gas sensor is defined as S ═ Rg/Ra (oxidizing gas), and S ═ Ra/Rg (reducing gas). Rg and Ra are the resistance values of the gas sensitive element in the gas to be measured and the air respectively. The time required for the gas sensor to reach 90% of the total resistance change during adsorption and desorption is defined as the response time and recovery time, respectively.
The embodiment has the following advantages:
1. compared with the traditional diabetes diagnosis method, the detection of acetone in breath as a non-invasive inspection technology has the advantages of no wound, short period, continuous monitoring and the like. And most of the existing detection means of the exhalation marker are large-scale instruments, need professional operation, are expensive and bring much inconvenience to detection. The portable breath detector based on the semiconductor sensor has the advantages of small volume, low price, portability and the like, can be applied to clinical assay and diagnosis of medical institutions, can also be used for health state tracking and disease pre-check in families, and has greater development potential.
2. In the prior art, metal oxides are generally synthesized and then dopants are added to the oxides by physical methods of impregnation. In the embodiment, Au or Pd is directly doped into the ZnO material by adopting a one-step microwave hydrothermal method. The preparation operation is easy and the process is simple. Compared with common physical doping, the method has the advantages that the dopant is dispersed more uniformly, and the components in the synthesized composite material can be contacted on a molecular layer.
3. Although conventional oxide semiconductor materials have a certain response to acetone gas, they tend to have low sensitivity to low concentrations of acetone, poor selectivity, high operating temperature, and poor moisture resistance. The Au or Pd doped ZnO material in the embodiment has low working temperature, high sensitivity, wide detection range (5ppb-100ppm), excellent selectivity and quick response speed to low-concentration acetone. Compared with the existing acetone sensor, the acetone sensor of the embodiment has better gas-sensitive property, and the performance of the acetone sensor meets the requirement of a sensor for detecting the exhalation marker.
The invention is further illustrated by the following specific examples.
Example 1
Au/ZnO (Au-doped ZnO) material synthesis:
first, 1.0g of zinc acetate was poured into a beaker, 15ml of distilled water was added, and the mixture was stirred until the particles were completely dissolved. 8.5g potassium hydroxide is weighed out again and added to the above solution, then 100ml absolute ethyl alcohol is poured in, stirred and sonicated until the solution is clear, then 0.18mM 10 is added to the solution-2And (3) a chloroauric acid solution in mol/L. And finally transferring the clarified solution into a microwave reactor, setting the microwave reactor to 160 ℃ for reaction for 60min, cooling the sample, taking out, washing, drying, and then putting into a muffle furnace for annealing at 450 ℃ for 3h to obtain a product, namely Au/ZnO. Sample characterization included: x-ray diffraction, scanning electron microscopy, transmission electron microscopy, elemental spectroscopy.
Device fabrication and gas sensitivity testing:
indirectly heated Al is used for gas sensor2O3A tubular device. A small amount of the prepared sample was taken, a small amount of distilled water was added, and the mixture was ground into a paste and then coated on a ceramic tube. Two ends of the tube are provided with a pair of Au electrodes connected with a Pt lead, a nickel-chromium alloy coil is inserted in the middle of the tube to provide the working temperature of the testing element, the device and a heating wire are welded on a six-pin base, the device and the heating wire are dried for 10min under an infrared lamp, and the device is aged for 12h at 100 ℃. The device characteristic test is carried out in a CGS-8 type gas-sensitive element characteristic tester produced by Beijing Elite technology Limited, and the experimental condition is that the relative humidity is 65% +/-5%. Sensitivity of the gas sensor is defined as S ═ Rg/Ra (oxidability)Gas), S ═ Ra/Rg (reducing gas). Rg and Ra are resistance values of the element in the gas to be measured and in the air, respectively. The time required for the gas sensor to reach 90% of the total resistance change during adsorption and desorption is defined as the response time and recovery time, respectively.
Example 2
The difference from example 1 is that 0.25mM of 10 is added-2And (3) obtaining a product named Pd/ZnO (Pd doped ZnO) by using a mol/L palladium nitrate solution.
FIG. 1a is the X-ray diffraction pattern of Au/ZnO and Pd/ZnO and undoped ZnO materials. As can be seen from the figure, the diffraction peak positions of the undoped ZnO are consistent with that of the XRD standard card (JCPDS 36-1451) of wurtzite ZnO. The three diffraction peaks of Au/ZnO at 38.17 deg., 44.39 deg. and 64.68 deg. were consistent with Au Standard card JCPDS 04-0784, indicating that Au has been successfully incorporated into ZnO. The diffraction peak of Pd in Pd/ZnO is matched with JCPDS 46-1043 card. However, the diffraction peak of Pd is significantly weaker than that of Au, probably because the metallic Au particles are mainly dispersed on the surface of ZnO, and most of Pd is doped into the framework of ZnO. FIGS. 1b-i show the SEM, TEM and SEM of Au/ZnO and Pd/ZnO and undoped ZnO material, and the selected area electron diffraction pattern. It can be seen that the ZnO nanorods have a diameter of about 50nm, a length of about 200nm, a high crystallinity, and a single crystal structure. After doping with Au and Pd, a porous structure appears in the nanorods. Some Au particles grew on the surface of the Au/ZnO material, while almost no Pd particles were found in Pd/ZnO, which is consistent with the results of XRD analysis. In addition, FIG. 1j-k shows the X-ray photoelectron spectra of Au/ZnO and Pd/ZnO. It can be analyzed from the figure that Au and Pd are well doped into ZnO, Au in Au/ZnO is metal particles, and Pd in Pd/ZnO is Pd2+Entering a ZnO framework.
FIG. 2a is a graph showing the sensitivity of Au/ZnO and Pd/ZnO and undoped ZnO materials to 100ppm acetone gas at different operating temperatures according to the embodiment of the present invention. As can be seen from the figure, the optimum operating temperature for the acetone sensor with these three materials is 150 deg.C, at which the sensitivity of Au/ZnO and Pd/ZnO and undoped ZnO to 100ppm acetone gas is 97, 63 and 24, respectively.
Fig. 2b is a graph of the selectivity of three sensors for different gases. It can be seen from the figure that the addition of Au and Pd can significantly improve the selectivity of ZnO to acetone gas.
FIGS. 2c-d show the sensitivity of Au/ZnO and Pd/ZnO and undoped ZnO to different concentrations of acetone gas. The detection limit of the Au/ZnO and Pd/Zn sensors for acetone is 5ppb, and the detection saturation phenomenon still does not occur for 100ppm of acetone. In addition, the signal response time of Au/ZnO and Pd/ZnO is less than 10s and 15s respectively. According to literature reports, the concentration of acetone in human breath is between 50ppb and 5 ppm. Therefore, the Au/ZnO and Pd/ZnO sensors can be completely used for quickly detecting the diabetes expiration marker acetone.
In summary, the doped ZnO material, the preparation method thereof and the acetone sensor provided by the invention have the advantages that the Au or Pd doped ZnO material synthesized by the one-step microwave hydrothermal method has a small (nanometer) particle size and a porous structure, and the gas permeation efficiency and the contact area with the material are improved. In addition, the addition of the noble metals Au and Pd obviously increases the gas-sensitive characteristics of ZnO to acetone, including low working temperature, high sensitivity, wide detection range (5ppb-100ppm), excellent selectivity and fast response speed, thereby providing a new way for manufacturing the acetone sensor for the diabetes expiration detection.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of a doped ZnO material is characterized by comprising the following steps:
mixing a zinc source with water, stirring until the zinc source is dissolved, then adding an alkali source and absolute ethyl alcohol, and stirring until a clear solution is obtained;
adding a soluble gold source or a soluble palladium source into the clarified solution, and transferring the obtained solution into a microwave reactor for reaction;
and after the reaction is finished, sequentially cooling, washing, drying and annealing to obtain the Au or Pd doped ZnO material.
2. The method for preparing the doped ZnO material according to claim 1, wherein the reaction temperature is 140-180 ℃; and/or the reaction time is 30-60 min.
3. The preparation method of the doped ZnO material according to claim 1, wherein the annealing temperature is 400-550 ℃; and/or the annealing time is 2-5 h.
4. The method for preparing the doped ZnO material according to claim 1, wherein the molar ratio of the zinc source, the alkali source and the soluble gold source is 1: 22-44: 0-0.077; or
The molar ratio of the zinc source, the alkali source and the soluble palladium source is 1: 22-44: 0-0.088.
5. The method for preparing doped ZnO material of claim 1, wherein the zinc source is selected from one or more of zinc acetate, zinc chloride and zinc nitrate; and/or
The alkali source is selected from one of potassium hydroxide and sodium hydroxide.
6. The method of claim 1, wherein the soluble gold source is one or more of chloroauric acid, gold nitrate, gold chloride, and gold acetate.
7. The method of claim 1, wherein the soluble palladium source is one or more of palladium nitrate, palladium chloride, and palladium sulfate.
8. A doped ZnO material, characterised in that it has been produced by a process according to any one of claims 1 to 7.
9. The doped ZnO material of claim 8, wherein the Au accounts for 0-6% of the doped ZnO material by mass; or
The Pd accounts for 0-7% of the mass percent of the doped ZnO material.
10. An acetone sensor, comprising a ceramic tube, wherein the surface of the ceramic tube is coated with a doped ZnO material prepared by the method of any one of claims 1 to 7; and/or
The surface of the ceramic tube is coated with the doped ZnO material of any of claims 8-9.
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