CN109607593A - A kind of preparation and its application of NiO-ZnO flower-like structure composite material - Google Patents
A kind of preparation and its application of NiO-ZnO flower-like structure composite material Download PDFInfo
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Abstract
A kind of preparation and its application of NiO-ZnO flower-like structure composite material, it is related to a kind of preparation of gas sensitive and its application, the present invention uses one one-step hydro-thermal synthesis method of low temperature, using zinc nitrate, nickel nitrate as raw material, urea is auxiliary addition agent, has synthesized NiO-ZnO flower-like structure composite material in a mild condition.Entire production process is simple and easy, efficient, energy saving, is suitable for large-scale production.The NiO-ZnO flower-like structure composite material that the present invention is prepared has unique space structure, not only increase the specific surface area of material, flourishing classification hole path can also be constructed simultaneously, make material that there is better permeability, higher sensitivity is shown to trimethylamine, good response-recovery characteristics and selectivity have broad application prospects in terms of manufacturing gas sensor.
Description
Technical field
The present invention relates to a kind of preparation of gas sensitive and its applications, multiple more particularly to a kind of NiO-ZnO flower-like structure
The preparation and its application of condensation material.
Background technique
With the continuous generation of marine product poisoning, the quality security problem of marine product has drawn the extensive pass of society
Note.Studies have shown that marine product addles, degree is related with the front three amine concentration that it is discharged, can be dense by the trimethylamine of detection volatilization
Spend the freshness to determine marine product.Therefore, high-performance trimethylamine gas sensor is developed, it is effectively and real to be carried out to its concentration
When monitoring, it can be achieved that marine products quality safety detection, have a very important significance.
ZnO is constantly subjected to the extensive concern of semiconductor gas sensor detection field as a kind of n-type semiconductor.
Result of study shows that the gas sensor made using ZnO as basis material has that detection range is wide, chemical stability is good, sensitive
The features such as high is spent, is the most wide semiconductor gas sensor of current most study, application range.However, current semiconductor sensing
The indexs such as the sensitivity of device are not still able to satisfy the requirement of site environment detection, have space to be hoisted there are huge.In recent years
That comes is some studies have shown that having the ZnO material of layering, porous structure, since it is with high-specific surface area, high Surface Permeability
The advantages that with light weight, is provided with special nature not available for conventional blocks material or general nano structural material, can improve
The air-sensitive performance of ZnO material.However, the self structure optimization of sensitive material can not bring the General Promotion of air-sensitive performance, open
Highly sensitive, highly selective, low-power consumption gas sensor is sent out, is still the challenge being concerned.Therefore, from sensitive material
The modification of material is started with, by the spirit for improving gas sensor in ZnO nano material surface modification the second component metals oxide
Sensitivity and selectivity are the effective way and thinking for improving semiconductor gas sensor performance.However, how to realize that ZnO is classified
The controllable preparation of composite material having porous structure accurately controls working condition, preparation cost is reduced, to synthesize specific structure and shape
The product of looks is the hot technology of current large-scale industrial production.
Summary of the invention
The purpose of the present invention is to provide the preparation and its application of a kind of NiO-ZnO flower-like structure composite material, the present invention
Using low-temperature hydro-thermal synthesis, it is prepared for NiO-ZnO flower-like structure composite material in a mild condition, and be applied to three
The detection of methylamine gas.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of preparation of NiO-ZnO flower-like structure composite material, it is described the preparation method is as follows:
(1) zinc nitrate, nickel nitrate are weighed in the balance, urea is dissolved in the mixing of 40 mL distilled water and the configuration of 40 mL ethylene glycol
In solution, magnetic agitation 30 minutes, are configured to hydrothermal synthesis presoma reaction solution at room temperature；
(2) hydrothermal synthesis presoma reaction solution is transferred in inner liner polytetrafluoroethylene stainless steel autoclave, filling degree is
80%, sealing；12 hours are kept the temperature at a temperature of 120 DEG C, room temperature is then cooled to the furnace, obtains reaction product；
(3) the solution centrifuge separation after reaction is obtained into reaction product, reuses distilled water, dehydrated alcohol washs repeatedly；
(4) reaction product after washing is put into the drying box of steady temperature, 60 DEG C, 24 hours, is dried, it is dry
It cools down after the completion；
(5) product after drying is put into clean crucible and is placed in Muffle furnace, 450 DEG C are calcined 4 hours, are finally produced
Object saves it in drier with pending analysis detection.
A kind of application of NiO-ZnO flower-like structure composite material, the material are applied and production gas as gas sensitive material
Body sensor.
The advantages and effects of the present invention are:
(1) present invention has synthesized the NiO- assembled by nanometer sheet using zinc nitrate, nickel nitrate as raw material under the conditions of low-temperature hydrothermal
ZnO flower-like structure composite material.With cost is relatively low, controllability is good, the material purity height of preparation, advantages of good crystallization, good dispersion
Advantage is suitable for large-scale industrial production.
(2) NiO-ZnO flower-like structure composite material produced by the present invention not only increases material because having unique space structure
The specific surface area of material, while flourishing classification hole path can also be constructed, make material that there is better permeability, as gas sensitive
The gas sensor of preparation shows higher sensitivity, repeatable response and the ability and selectivity restored to trimethylamine,
It has broad application prospects in terms of the toxic and harmful gas in detection environment.
(3) the NiO-ZnO flower-like structure trimethylamine gas sensor manufacture craft that the present invention makes is simple, low in cost,
Suitable for industrialized mass production.
Detailed description of the invention
Fig. 1 is the X-ray diffraction spectrogram of product；
Fig. 2 (a)-(b) is the electron scanning micrograph of product prepared by embodiment 1, the production that (c)-(d) prepared by embodiment 2
The electron scanning micrograph of object, (e)-(f) are the electron scanning micrograph of product prepared by embodiment 3, (g)-(h)
For the electron scanning micrograph of product prepared by embodiment 4, (i)-(j) is the scanning electron of product prepared by embodiment 5
Microscope photo；
Fig. 3 (a) is the structural schematic diagram of tma sensor, (b) is sensitivity of the gas sensor to 5 ppm front three amine gas
With temperature change curve graph；
Fig. 4 (a) be in embodiment 3 gas sensor at 250 DEG C to the dynamic response curve figure of various concentration front three amine gas,
(b) for gas sensor in embodiment 3 to trimethylamine gas concentration with change of sensitivity curve graph；
Fig. 5 is for gas sensor in embodiment 3 at 250 DEG C to the selective figure of 5 ppm difference reducibility gas.
Specific embodiment
The following describes the present invention in detail with reference to examples.
Starting material of the present invention is zinc nitrate and nickel nitrate cheap and easy to get, is reacted by low-temperature hydrothermal, by centrifugation, is washed
The processing such as wash, dry and calcine.Prepared NiO-ZnO flower-like structure composite material is by shape, the similar nanometer sheet of size
Composition, diameter is 2-6 μm.The thickness of nanometer sheet is about 20-40 nm, and each adjacent nano piece spacing is very big, favorably
In the adsorption and desorption of object gas.NiO-ZnO flower-like structure composite material is prepared into gas sensor, because of its unique sky
Between structure, higher sensitivity, good response-recovery characteristics and selectivity are shown to trimethylamine.
(1) NiO-ZnO flower-like nanostructure composite material and preparation method thereof, comprising the following steps:
Step 1: by a certain amount of zinc nitrate, nickel nitrate, urea are dissolved in the mixed of 40 mL distilled water and the configuration of 40 mL ethylene glycol
It closes in solution, magnetic agitation is configured to hydrothermal synthesis presoma reaction solution up to being completely dissolved.
Step 2: presoma reaction solution made from step 1 is transferred to inner liner polytetrafluoroethylene stainless steel autoclave
In, filling degree is 80%, sealing.12 hours are kept the temperature at a temperature of 120 DEG C, room temperature is then cooled to the furnace, obtains reaction product.
Step 3: reaction product made from centrifugation step two, and washed repeatedly with distilled water, dehydrated alcohol, 60 DEG C later,
It is dried within 24 hours.
Step 4: product of the step 3 after dry is placed in Muffle furnace, and 450 DEG C are calcined 4 hours to get NiO-ZnO is arrived
Flower-like structure composite material.
(2) the step of preparing gas sensor using NiO-ZnO flower-like structure composite material:
Step 1: being made slurry for NiO-ZnO flower-like structure composite material addition water, be coated onto band there are two gold electrode and
In the aluminium oxide ceramics pipe outer wall of four platinum conducting wires.
Step 2: nickel-chromium alloy heater strip being passed through and is stained with the alumina ceramic tube of sample, and by heater strip and ceramic tube
In parallel, ceramic tube is made it away from.
Step 3: the both ends of four conductor wires of ceramic tube and heater strip are respectively welded on six leg bases, and gas is made
Body sensor element.
Step 4: WS-30A air-sensitive tester is used, the gas sensitization characteristic of sensor is tested.Test temperature is 100-
350℃。
Embodiment 1
(1) ZnO flower-like structure material is prepared
Step 1: 2.38 g zinc nitrates, 2.40 g urea, be dissolved in 40 mL distilled water and 40 mL ethylene glycol configuration
In mixed solution, hydrothermal synthesis presoma reaction solution is configured to up to being completely dissolved within magnetic agitation 30 minutes.
Step 2: presoma reaction solution made from step 1 is transferred to inner liner polytetrafluoroethylene stainless steel autoclave
In, filling degree is 80%, sealing.
Step 3: the reaction kettle of step 2 is placed in baking oven, is kept the temperature 12 hours at a temperature of 120 DEG C, is then cooled down.
Step 4: reactant solution made from step 3 is centrifugated, and obtains sediment, reuses distilled water, anhydrous
Ethyl alcohol washs repeatedly.
Step 5: the product of step 4 is placed in the drying box of steady temperature, and 60 DEG C are dried 24 hours, has been dried
At rear cooling.
Step 6: product of the step 5 after dry is put into clean crucible and is placed in Muffle furnace, 400 DEG C of calcinings 4 are small
When, ZnO powder is obtained, is saved it in drier with pending analysis detection.
(2) structural characterization of ZnO flower-like structure material
Crystalline product structure is characterized using XRD powder diffractometer (XRD, PANalytical X ' Pert Pro).Fig. 1
For X x ray diffraction (XRD) map of sample.To find out that diffractive features peak is all very sharp from figure, no any miscellaneous peak occurs,
Show that the sample purity prepared and crystallinity are very high.Diffraction maximum is complied fully with NO.36-1451 in standard PDF card, explanation
The sample is monoclinic phase ZnO.
Product morphology is characterized using scanning electron microscope (FESEM, ZEISS Ultra Plus).Such as Fig. 2 (a)-(b)
Shown, it is about that 20-40 nm nanometer sheet self assembly forms by many thickness that product presentation is flower-shaped, and diameter is 2-6 μm, dispersion
Property is good, and powder surface has a large amount of hole.
Embodiment 2
(1) NiO-ZnO flower-like structure composite material is prepared
Step 1: 2.38 g zinc nitrates, 0.23 g nickel nitrate, 2.40 g urea are dissolved in 40 mL distilled water and 40
In the mixed solution of mL ethylene glycol configuration, hydrothermal synthesis forerunner's precursor reactant is configured to up to being completely dissolved within magnetic agitation 30 minutes
Solution.
Step 2: three, four, five, six the same as embodiment 1.
(2) structural characterization of NiO-ZnO flower-like structure composite material
Crystalline product structure is characterized using XRD powder diffractometer (XRD, PANalytical X ' Pert Pro).From figure
To find out in sample in addition to the peak of monoclinic phase ZnO in 1, the peak of NiO does not occur, may be lower due to NiO comparision contents,
Particle size is smaller.Diffractive features peak is all very sharp, and no any miscellaneous peak occurs, and shows the sample purity prepared and crystallinity very
It is high.Product morphology is characterized using scanning electron microscope.As shown in Fig. 2 (c)-(d), pattern presentation is flower-shaped, with pure appearance of ZnO
Unanimously, no significant change.
Embodiment 3
(1) NiO-ZnO flower-like structure composite material is prepared
Step 1: 2.38 g zinc nitrates, 0.69 g nickel nitrate, 2.40 g urea are dissolved in 40 mL distilled water and 40 mL
In the mixed solution of ethylene glycol configuration, it is molten to be configured to hydrothermal synthesis forerunner's precursor reactant up to being completely dissolved within magnetic agitation 30 minutes
Liquid.
Step 2: three, four, five, six the same as embodiment 1.
(2) structural characterization of NiO-ZnO flower-like structure composite material
Crystalline product structure is characterized using XRD powder diffractometer (XRD, PANalytical X ' Pert Pro).From figure
To find out in sample in addition to the peak of monoclinic phase ZnO in 1, the peak of NiO does not occur, may be lower due to NiO comparision contents,
Particle size is smaller.Diffractive features peak is all very sharp, and no any miscellaneous peak occurs, and shows the sample purity prepared and crystallinity very
It is high.Product morphology is characterized using scanning electron microscope.As shown in Fig. 2 (e)-(f), pattern presentation is flower-shaped, with pure appearance of ZnO
Unanimously, no significant change.
Embodiment 4
(1) NiO-ZnO flower-like structure composite material is prepared:
Step 1: 2.38 g zinc nitrates, 1.15 g nickel nitrates, 2.40 g urea are dissolved in 40 mL distilled water and 40
In the mixed solution of mL ethylene glycol configuration, hydrothermal synthesis forerunner's precursor reactant is configured to up to being completely dissolved within magnetic agitation 30 minutes
Solution.
Step 2: three, four, five, six the same as embodiment 1.
(2) structural characterization of NiO-ZnO flower-like structure composite material
Crystalline product structure is characterized using XRD powder diffractometer (XRD, PANalytical X ' Pert Pro).From figure
To find out the diffraction maximum in addition to the peak of monoclinic phase ZnO, occurring 1 NiO in sample in 1, corresponding standard card is (JPCDS card
Number 47-1049).And the characteristic peak of all products does not find other impurity diffraction maximums, show product be mainly by ZnO and
NiO composition, and purity and crystallinity are very high.Product morphology is characterized using scanning electron microscope.As shown in Fig. 2 (g)-(h),
Flower-shaped, no significant change consistent with pure appearance of ZnO is presented in its pattern.
Embodiment 5
(1) NiO-ZnO flower-like structure composite material is prepared
Step 1: 2.38 g zinc nitrates, 2.3 g nickel nitrates, 2.40 g urea are dissolved in 40 mL distilled water and 40
In the mixed solution of mL ethylene glycol configuration, hydrothermal synthesis forerunner's precursor reactant is configured to up to being completely dissolved within magnetic agitation 30 minutes
Solution.
Step 2: three, four, five, six the same as embodiment 1.
(2) structural characterization of NiO-ZnO flower-like structure composite material
Crystalline product structure is characterized using XRD powder diffractometer (XRD, PANalytical X ' Pert Pro).From figure
To find out the diffraction maximum in addition to the peak of monoclinic phase ZnO, occurring 2 apparent NiO in sample in 1, corresponding standard card is
(JPCDS card number 47-1049).And the characteristic peak of all products does not find other impurity diffraction maximums, shows that product is main
It is made of ZnO and NiO, and purity and crystallinity are very high.Product morphology is characterized using scanning electron microscope.Such as Fig. 2 (i)-
(j) shown in, pattern presentation is flower-shaped, and consistent with pure appearance of ZnO, no significant change, bouquet surface is with NiO nano-particle content
Increase and become coarse.
Gas sensor is made with NiO-ZnO flower-like nanostructure composite material obtained, correlation has been carried out to trimethylamine
Air-sensitive performance test:
It weighs a certain amount of NiO-ZnO flower-like nanostructure composite material addition water and slurry is made, be coated in alumina ceramic tube
On, there are two gold electrode and four platinum conducting wires, Guan Zhongwei nickel-chrome heater strips on alumina ceramic tube.Ceramic tube is welded on six
On leg base, gas sensor element is made, as shown in Fig. 3 (a).Using WS-30A air-sensitive tester, the gas of sensor is tested
Body sensitivity characteristic.
5 ppm trimethylamine gas sensitivities with shown in temperature change curve graph such as Fig. 3 (b), we can see that
In 100 DEG C to 350 DEG C temperature ranges, the sensitivity of all the sensors increases with the raising of operating temperature first, and reaches
Then maximum value gradually decreases.Embodiment 2, embodiment 3, embodiment 4, the optimum working temperature of 5 sensor of embodiment are 250 °
C, maximum response are 3.6,4,3.1 and 2.3 respectively.And the optimum working temperature of pure ZnO sensor is 300 °C, peak response
Value is 2.2.This shows that operating temperature can not only be reduced by suitably modifying NiO on ZnO sensitive material surface, can also improve front three
The sensitivity of amine.Here selecting 3 sensor of embodiment with maximum sensitivity is best sensor, is carried out to its sensitive property
Test.
Fig. 4 (a) show the response-recovery curve of 1-500 ppm front three amine gas.It is obvious that when sensor is exposed to
Resistance sharply declines when front three amine gas, and then resistance is restored to its initial value after discharging front three amine gas, shows it to not
There is good resolution capability with concentration trimethylamine.It can be easily from respective concentration sensitivity relation figure (Fig. 4 (b))
Out, the sensitivity of sensor increases sharply as front three amine concentration increases, until 100 ppm.It is sensitive when higher than 100 ppm
The ascendant trend of degree slows down gradually, and shows that sensor is gradually saturated.The spirit of the bright sensor in the low concentration range of interior list of illustrations
Sensitivity increases with the increase approximately linear of concentration, this illustrates that the sensor of production is more suitable for detecting the trimethylamine of low concentration.Fig. 5
It show the sensitivity when operating temperature is 250 DEG C to 5 ppm gas with various.It can be seen from the figure that other gases are compared,
Sensor in embodiment 3, in the 6 kinds of gases tested, to the high sensitivity of trimethylamine in methanol, acetone, toluene, benzene,
Alcohol gas, this illustrates that the sensor has fine selectivity to trimethylamine.
Claims (2)
1. a kind of preparation of NiO-ZnO flower-like structure composite material, which is characterized in that it is described the preparation method is as follows:
(1) zinc nitrate, nickel nitrate are weighed in the balance, urea is dissolved in the mixing of 40 mL distilled water and the configuration of 40 mL ethylene glycol
In solution, magnetic agitation 30 minutes, are configured to hydrothermal synthesis presoma reaction solution at room temperature；
(2) hydrothermal synthesis presoma reaction solution is transferred in inner liner polytetrafluoroethylene stainless steel autoclave, filling degree is
80%, sealing；12 hours are kept the temperature at a temperature of 120 DEG C, room temperature is then cooled to the furnace, obtains reaction product；
(3) the solution centrifuge separation after reaction is obtained into reaction product, reuses distilled water, dehydrated alcohol washs repeatedly；
(4) reaction product after washing is put into the drying box of steady temperature, 60 DEG C, 24 hours, is dried, it is dry
It cools down after the completion；
(5) product after drying is put into clean crucible and is placed in Muffle furnace, 450 DEG C are calcined 4 hours, are finally produced
Object saves it in drier with pending analysis detection.
2. a kind of application of NiO-ZnO flower-like structure composite material, which is characterized in that the material is as gas sensitive material application
With production gas sensor.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110530937A (en) * | 2019-09-25 | 2019-12-03 | 上海交通大学 | A kind of preparation method of the ethylene glycol sensor based on CuO-NiO nano tube hetero-junction structure |
| CN110596196A (en) * | 2019-09-16 | 2019-12-20 | 山东大学 | Semiconductor heterojunction gas sensitive material and preparation method and application thereof |
| CN111579600A (en) * | 2020-06-28 | 2020-08-25 | 郑州轻工业大学 | Camellia flower-shaped ZnO/SnO-SnO2Composite material and preparation method and application thereof |
| CN112255279A (en) * | 2020-09-29 | 2021-01-22 | 沈阳化工大学 | Flower-shaped V2O5Preparation of microsphere and application of microsphere in acetone gas sensor |
| CN112320859A (en) * | 2020-10-10 | 2021-02-05 | 沈阳化工大学 | NiO-SnO2Preparation method and application of flower-shaped structure composite material |
| CN113155912A (en) * | 2021-04-16 | 2021-07-23 | 沈阳化工大学 | Preparation method and application of CuO-ZnO flower-shaped structure composite sensitive material |
| CN113155907A (en) * | 2021-03-10 | 2021-07-23 | 东北电力大学 | Detection of SF6Decomposition gas H2ZnO-NiO gas sensor of S |
| CN113433171A (en) * | 2021-06-24 | 2021-09-24 | 兰州大学 | Gas-sensitive material, gas-sensitive sensor, and preparation method and application thereof |
| CN116179192A (en) * | 2022-12-30 | 2023-05-30 | 苏州为度生物技术有限公司 | Magneto-optical three-function composite microsphere and preparation method thereof |
| CN117069165A (en) * | 2023-08-15 | 2023-11-17 | 哈尔滨理工大学 | Preparation method of Pd modified two-dimensional porous NiO/ZnO gas-sensitive material and method for preparing CO gas sensor by using Pd modified two-dimensional porous NiO/ZnO gas-sensitive material |
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2019
- 2019-01-10 CN CN201910023463.2A patent/CN109607593A/en active Pending
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110596196A (en) * | 2019-09-16 | 2019-12-20 | 山东大学 | Semiconductor heterojunction gas sensitive material and preparation method and application thereof |
| CN110530937A (en) * | 2019-09-25 | 2019-12-03 | 上海交通大学 | A kind of preparation method of the ethylene glycol sensor based on CuO-NiO nano tube hetero-junction structure |
| CN111579600A (en) * | 2020-06-28 | 2020-08-25 | 郑州轻工业大学 | Camellia flower-shaped ZnO/SnO-SnO2Composite material and preparation method and application thereof |
| CN111579600B (en) * | 2020-06-28 | 2022-11-22 | 郑州轻工业大学 | Camellia flower-shaped ZnO/SnO-SnO 2 Composite material and preparation method and application thereof |
| CN112255279A (en) * | 2020-09-29 | 2021-01-22 | 沈阳化工大学 | Flower-shaped V2O5Preparation of microsphere and application of microsphere in acetone gas sensor |
| CN112320859A (en) * | 2020-10-10 | 2021-02-05 | 沈阳化工大学 | NiO-SnO2Preparation method and application of flower-shaped structure composite material |
| CN113155907A (en) * | 2021-03-10 | 2021-07-23 | 东北电力大学 | Detection of SF6Decomposition gas H2ZnO-NiO gas sensor of S |
| CN113155912A (en) * | 2021-04-16 | 2021-07-23 | 沈阳化工大学 | Preparation method and application of CuO-ZnO flower-shaped structure composite sensitive material |
| CN113433171A (en) * | 2021-06-24 | 2021-09-24 | 兰州大学 | Gas-sensitive material, gas-sensitive sensor, and preparation method and application thereof |
| CN116179192A (en) * | 2022-12-30 | 2023-05-30 | 苏州为度生物技术有限公司 | Magneto-optical three-function composite microsphere and preparation method thereof |
| CN116179192B (en) * | 2022-12-30 | 2023-12-15 | 苏州为度生物技术有限公司 | Magneto-optical three-function composite microsphere and preparation method thereof |
| CN117069165A (en) * | 2023-08-15 | 2023-11-17 | 哈尔滨理工大学 | Preparation method of Pd modified two-dimensional porous NiO/ZnO gas-sensitive material and method for preparing CO gas sensor by using Pd modified two-dimensional porous NiO/ZnO gas-sensitive material |
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