CN111115717A - Preparation method of flower-shaped nickel oxide composed of porous sheets - Google Patents
Preparation method of flower-shaped nickel oxide composed of porous sheets Download PDFInfo
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- CN111115717A CN111115717A CN202010056488.5A CN202010056488A CN111115717A CN 111115717 A CN111115717 A CN 111115717A CN 202010056488 A CN202010056488 A CN 202010056488A CN 111115717 A CN111115717 A CN 111115717A
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Abstract
A method for preparing flower-shaped nickel oxide composed of porous sheets is characterized in that: dissolving nickel acetate tetrahydrate in distilled water to form a nickel acetate solution, dissolving PVA and urea in distilled water to form a mixed solution, slowly dropwise adding the mixed solution into the nickel acetate solution, mixing, then adding polyethylene glycol 2000, dropwise adding ammonia water with the mass concentration of 25% -28% while stirring, transferring the mixture into a reaction kettle after dropwise adding, heating, centrifugally washing, drying, and annealing to obtain black nickel oxide. The flower-shaped nickel oxide prepared by the method has rich pore-size structures and large specific surface area, and is beneficial to full contact with gas to be detected; the product has uniform appearance, uniform and controllable size, good dispersibility and no agglomeration; the yield of the product is high, when the product is used for manufacturing a gas sensor, the working temperature is low, the selectivity to formaldehyde is high, the sensitivity to formaldehyde gas under 100ppm at normal temperature can reach 19, the response time is fast, the recovery time is short, and the stability is good.
Description
Technical Field
The invention relates to the technical field of micro-nano structure metal oxide preparation, in particular to a preparation method of a flower-shaped nickel oxide material consisting of porous sheets.
Background
At present, SnO is used as a gas-sensitive material for a metal oxide semiconductor gas-sensitive sensor for ethanol and most gases2、ZnO、Fe2O3、WO3、TiO2As main matrix materials, the binary oxides belong to broad-spectrum gas-sensitive materials, and have gas-sensitive response to various gases (such as ethanol, formaldehyde, acetone, hydrogen and the like) and lack selectivity.
The nickel oxide has unique optical and electrical characteristics, and thus has wide application in the fields of solar cells, gas sensitive elements and the like. So far, nickel oxides with various morphologies such as nanowires, nanorods, nanobelts, nanotubes, nanosheets, and the like have been reported in the literature. In recent years, micro-nano materials with a hierarchical self-assembly structure have attracted attention in the fields of gas sensors and photocatalysis due to large specific surface area. Nickel oxide, which is a P-type semiconductor, is commonly used for detecting hydrogen sulfide gas, ammonia gas, nitrogen dioxide gas, formaldehyde gas, and the like, and has the problems of low sensitivity and poor selectivity. In recent years, in order to improve the sensitivity and selectivity, people have made continuous efforts, including noble metal doping of Au, Ag, Pt, Pd, Cd, etc., morphology control, nanoparticles, core-shell nanospheres, porous nanorods, nanotubes, nanobelts, porous networks, etc. The improvements make progress in improving the sensitivity of the metal oxide gas-sensitive material, but the selectivity and response effect on formaldehyde are still not ideal.
Based on the problems of irregular shape, large size distribution span, poor dispersibility, low yield, poor gas selectivity, low sensitivity and the like of the nickel oxide prepared in the prior art when the nickel oxide is used in the field of gas sensors, the nickel oxide prepared by the method has high selectivity, high sensitivity and good stability to formaldehyde, and has important significance.
Disclosure of Invention
The invention aims to provide a preparation method of porous flaky flower-shaped nickel oxide, which can prepare the flower-shaped nickel oxide with regular appearance, uniform particle size, good dispersibility, high yield and excellent stability.
The purpose of the invention is realized by the following technical scheme:
a method for preparing flower-shaped nickel oxide composed of porous sheets is characterized in that: dissolving nickel acetate tetrahydrate in distilled water to form a nickel acetate solution, dissolving PVA and urea in distilled water to form a mixed solution, slowly dropwise adding the mixed solution into the nickel acetate solution, mixing, then adding polyethylene glycol 2000, dropwise adding ammonia water with the mass concentration of 25% -28% while stirring, transferring the mixture into a hydrothermal reaction kettle after dropwise adding, heating, centrifugally washing, drying, and annealing to obtain black nickel oxide.
Furthermore, the mass-volume ratio of the nickel acetate tetrahydrate to the distilled water is 0.374-0.648 g:5 mL.
Further, the proportion relation of the PVA, the urea and the distilled water is 0.25 g: 0.24-0.54 g:5 mL.
Further, the volume ratio of the polyethylene glycol 2000 to the ammonia water to the mixed solution is 10:1: 16-18.
Wherein, polyethylene glycol 2000 is both the solvent, and is surfactant active again, and the aqueous ammonia both plays the complexation, adjusts the pH value of system again, and the complexation of aqueous ammonia: ni2++NH3+H2O⇋ [Ni(H2O)6x(NH3)x]2+。
Further, the heating is carried out at 100-200 ℃ for 2-10 h.
Further, the annealing treatment is specifically annealing at 450-600 ℃ for 1-3 h.
Preferably, the annealing treatment is specifically annealing at 500 ℃ for 2 h.
Specifically, the preparation method of the flower-shaped nickel oxide with porous flaky composition is characterized by comprising the following steps of:
(1) dissolving nickel acetate tetrahydrate in distilled water to form a nickel acetate solution, dissolving PVA and urea in distilled water to form a mixed solution, wherein the mass-to-volume ratio of the nickel acetate tetrahydrate to the distilled water is 0.374-0.648 g:5mL, and the mass-to-volume ratio of the PVA, the urea to the distilled water is 0.25 g: 0.24-0.5 g:5 mL;
(2) slowly adding the mixed solution into a nickel acetate solution, adding polyethylene glycol 2000, stirring while dropwise adding ammonia water with the mass concentration of 25-28%, continuously stirring at the speed of 300rpm for 10min after dropwise adding is completed to obtain a precursor solution, wherein the volume ratio of the polyethylene glycol 2000 to the ammonia water to the mixed solution is 10:1: 16-18;
(3) transferring the precursor solution obtained in the step (2) to a hydrothermal reaction kettle, and heating for 6-10 hours at 100-200 ℃;
(4) filtering and centrifuging the solution obtained in the step (3), washing the solution for a plurality of times by using ethanol and deionized water, and then drying the solution for 8 hours at 70 ℃;
(5) and (3) annealing the precursor obtained by drying in the step (4) at the temperature of 450-600 ℃ for 1-3h to obtain the black nickel oxide powder.
The urea is used as a precipitator, the hydrolysis degree is low at normal temperature, nickel acetate tetrahydrate is used as a raw material, acetate in a mixed system is hydrolyzed to be alkalescent, the urea is promoted to be further hydrolyzed, and more nickel hydroxide precipitates are formed; combining with ammonia water complexation and pH adjustment of the system to make nickel ion completely form nickel hydroxide precipitate and complex [ Ni (H2O)6x(NH3)x](OH)2And then the nickel oxide is prepared by combining annealing treatment, so that the purity and the yield of the product are improved.
According to the method, a mixed solution containing PVA and urea is added into a nickel acetate aqueous solution, the solubility and the solution saturation of reactants are changed through the solvent action of polyethylene glycol 2000 and the complexing action of ammonia water, the reaction rate is controlled, the surfactant synergistic effect of polyethylene glycol 2000 and PVA has a tendency of forming sheet-shaped bundle glue in a system, nickel hydroxide and a complex compound generated by reaction are guided to be attached to the surface of the bundle glue and are converted to a specific shape to form a nano sheet, and specific annealing treatment is combined, so that the flower-shaped nickel oxide which is formed by porous sheets and has the advantages of regular shape, uniform particle size, good dispersibility, high yield and excellent stability is formed.
The invention has the following technical effects:
the flower-like nickel oxide prepared by the invention is flower-like micron particles consisting of porous sheets, and has excellent comprehensive properties:
(1) the product has rich pore diameter structure and large specific surface area, and is beneficial to full contact with the gas to be detected;
(2) the product has uniform appearance, irregular flower-shaped structure formed by porous sheets, uniform and controllable size of about 5 mu m, good dispersibility and no agglomeration.
(3) The yield of the product is high and reaches more than 85 percent.
(4) When the product is used for manufacturing a gas sensor, the working temperature is low, the optimal working temperature is 160 ℃, the selectivity to formaldehyde is high, the sensitivity to formaldehyde gas under 100ppm at normal temperature can reach 19, the minimum detection limit value to formaldehyde gas can be as low as 1ppm, the response-recovery time is short, the response time is 2s, the recovery time is 3s, the resistance level before detection can be completely recovered during desorption, and the stability is good.
Drawings
FIG. 1: the XRD pattern of the flower-shaped nickel oxide prepared by the invention.
FIG. 2: scanning electron microscope images of the flower-like nickel oxide prepared by the invention.
FIG. 3: scanning electron microscope images of the flower-like nickel oxide prepared by the invention.
FIG. 4: scanning electron microscope images of the flower-like nickel oxide prepared by the invention.
FIG. 5: the flower-shaped nickel oxide prepared by the invention has a repeated response-recovery curve under the condition of 100ppm formaldehyde gas concentration.
FIG. 6: the gas selectivity of the nickel oxide prepared by the method is detected under different concentrations.
Detailed Description
The present invention is described in detail below by way of examples, it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and those skilled in the art can make some insubstantial modifications and adaptations of the present invention based on the above-mentioned disclosure.
Example 1
A preparation method of flower-shaped nickel oxide with porous flaky composition is characterized by comprising the following steps:
(1) dissolving nickel acetate tetrahydrate in distilled water to form a nickel acetate solution, dissolving PVA and urea in distilled water to form a mixed solution, wherein the mass-volume ratio of the nickel acetate tetrahydrate to the distilled water is 0.374g:5mL, and the mass-volume ratio of the PVA, the urea to the distilled water is 0.25 g: 0.24 g:5 mL;
(2) slowly adding the mixed solution into a nickel acetate solution, adding polyethylene glycol 2000, stirring while dropwise adding ammonia water with the mass concentration of 28%, continuously stirring at the speed of 300rpm for 10min after dropwise adding is completed to obtain a precursor solution, wherein the volume ratio of the polyethylene glycol 2000 to the ammonia water to the mixed solution is 10:1: 16;
(3) transferring the precursor solution in the step (2) to a hydrothermal reaction kettle, and heating at 200 ℃ for 6 hours;
(4) filtering and centrifuging the solution obtained in the step (3), washing the solution for a plurality of times by using ethanol and deionized water, and then drying the solution for 8 hours at 70 ℃;
(5) and (4) annealing the precursor obtained by drying in the step (4) at 600 ℃ for 1h to obtain the black nickel oxide powder.
Example 2
A preparation method of flower-shaped nickel oxide with porous flaky composition is characterized by comprising the following steps:
(1) dissolving nickel acetate tetrahydrate in distilled water to form a nickel acetate solution, dissolving PVA and urea in distilled water to form a mixed solution, wherein the mass-volume ratio of the nickel acetate tetrahydrate to the distilled water is 0.648g:5mL, and the mass-volume ratio of the PVA, the urea and the distilled water is 0.25 g: 0.54 g:5 mL;
(2) slowly adding the mixed solution into a nickel acetate solution, adding polyethylene glycol 2000, stirring while dropwise adding ammonia water with the mass concentration of 25%, continuously stirring at the speed of 300rpm for 10min after dropwise adding is completed to obtain a precursor solution, wherein the volume ratio of the polyethylene glycol 2000 to the ammonia water to the mixed solution is 10:1: 18;
(3) transferring the precursor solution in the step (2) to a hydrothermal reaction kettle, and heating at 100 ℃ for 8 hours;
(4) filtering and centrifuging the solution obtained in the step (3), washing the solution for a plurality of times by using ethanol and deionized water, and then drying the solution for 8 hours at 70 ℃;
(5) and (4) annealing the precursor obtained by drying in the step (4) at 450 ℃ for 3h to obtain the black nickel oxide powder.
Example 3
A preparation method of flower-shaped nickel oxide with porous flaky composition is characterized by comprising the following steps:
(1) dissolving nickel acetate tetrahydrate in distilled water to form a nickel acetate solution, dissolving PVA and urea in distilled water to form a mixed solution, wherein the mass volume ratio of the nickel acetate tetrahydrate to the distilled water is 0.623g:5mL, and the mass volume ratio of the PVA, the urea and the distilled water is 0.25 g: 0.48 g:5 mL;
(2) slowly adding the mixed solution into a nickel acetate solution, adding polyethylene glycol 2000, stirring while dropwise adding ammonia water with the mass concentration of 28%, continuously stirring at the speed of 300rpm for 10min after dropwise adding is completed to obtain a precursor solution, wherein the volume ratio of the polyethylene glycol 2000 to the ammonia water to the mixed solution is 10:1: 17;
(3) transferring the precursor solution in the step (2) to a hydrothermal reaction kettle, and heating at 180 ℃ for 10 hours;
(4) filtering and centrifuging the solution obtained in the step (3), washing the solution for a plurality of times by using ethanol and deionized water, and then drying the solution for 8 hours at 70 ℃;
(5) and (4) annealing the precursor obtained by drying in the step (4) at 500 ℃ for 2h to obtain the black nickel oxide powder.
The pH of the solution was 9.12 when the nickel ions were completely precipitated, as calculated from the Ksp of nickel hydroxide, and the yield was low when the pH was too high or too low.
XRD detection of nickel oxide:
the radiation source is Cu Bak, the wavelength is 1.54060 m, the scanning angle is 30-90 degrees, the voltage is 30 kV, the current is 20 mA, the scanning speed is 4.2 degrees/min, the X-ray diffraction pattern of the obtained micron particles is shown in figure 1, the XRD pattern diffraction peak of a sample is consistent with that of a standard card JCPDS number 04-0835, other miscellaneous peaks are not observed, and the synthesis of pure-phase nickel oxide is proved without other impurities.
As can be seen from FIGS. 2 to 4, the nickel oxide prepared by the invention is flower-like micron particles composed of porous sheets, has uniform and controllable size, particle size of about 5 μm, uniform appearance and good dispersibility.
And (3) testing gas-sensitive performance:
the gas sensitivity of a P-type semiconductor is defined as Rg/Ra, where Ra and Rg are the resistance values of the sensor when exposed to air and a target gas, respectively. The response time is specified as the time for the sensor resistance to rise to a stable value of 90% after injection of the target gas, and the recovery time is defined as the time for the sensor resistance to fall to a final resistance value of 10% after removal of the target gas.
The test is carried out at the ambient temperature of 25-30 ℃ and the ambient humidity of 30-40%, and the test is carried out by using a CGS (gas sensitive system) intelligent gas analysis system of Beijing Airit technology Limited. The indirectly heated gas sensor is formed by adopting an indirectly heated device structure, wherein the base of the indirectly heated gas sensor is a hard plastic substrate, a conductive metal rod is arranged on the indirectly heated gas sensor, the conductive metal rod is connected with a ceramic device in the middle of the indirectly heated gas sensor, the surface of the indirectly heated gas sensor is coated with corresponding gas-sensitive material nickel oxide, and the center of a ceramic tube penetrates through a heating resistance wire and is fixed on the base. And connecting the gas-sensitive element on a gas-sensitive test system, and recording the measured data in real time.
The resistance values of the gas sensor under different currents are obtained through testing, and the current and the temperature are converted according to a formula of y =2x-60, wherein x refers to the current (mA) and y refers to the temperature (DEG C).
The gas sensitive element has an optimal working temperature within a certain temperature range, the working temperature of the element is too low, the surface activity of the element is low, the action with gas molecules is weak, and the generated electronic exchange and the like are few, so that the sensitivity is low, the flower-shaped nickel oxide prepared by the method has huge specific surface area and porous structure, so that the prepared gas sensitive element has high activity in a low-temperature environment, the gas sensitive element with excellent performance requires low working temperature, the temperature difference with the environment (such as room temperature) is small, the practicability of the element is enhanced, and the optimal working temperature of the gas sensitive element under 100ppm formaldehyde gas is about 160 ℃.
As shown in fig. 5, when the gas sensor is made of the flower-like nickel oxide prepared by the present invention, the gas sensor has a fast response at a low concentration of 1ppm of the target gas, and the sensitivity achieved at a concentration of 100ppm is as high as 19, the response time is 2s, and the recovery time is 3s, and the gas sensor can still recover to the resistance value of the initial state under repeated responses, and has excellent stability.
And (3) selective detection:
the response of the flower-shaped nickel oxide prepared by the method to formaldehyde gas and other gases under 100ppm at a certain time point is shown in figure 6, and tests show that the sample has high selectivity to formaldehyde, can reach 19 sensitivity under 100ppm, and has low response to gases such as ethanol, acetone, ammonia gas and the like.
Claims (7)
1. A method for preparing flower-shaped nickel oxide composed of porous sheets is characterized in that: dissolving nickel acetate tetrahydrate in distilled water to form a nickel acetate solution, dissolving PVA and urea in distilled water to form a mixed solution, slowly dropwise adding the mixed solution into the nickel acetate solution, mixing, then adding polyethylene glycol 2000, dropwise adding ammonia water with the mass concentration of 25% -28% while stirring, transferring the mixture into a hydrothermal reaction kettle after dropwise adding, heating, centrifugally washing, drying, and annealing to obtain black nickel oxide.
2. The method for preparing a flower-like nickel oxide composed of porous flakes according to claim 1, wherein: the mass-volume ratio of the nickel acetate tetrahydrate to the distilled water is 0.374-0.648 g:5 mL.
3. The method for producing a flower-like nickel oxide composed of porous flakes according to claim 1 or 2, wherein: the proportion relation of the PVA, the urea and the distilled water is 0.25 g: 0.24-0.54 g:5 mL.
4. A method for preparing a flower-like nickel oxide composed of porous flakes according to any one of claims 1 to 3, characterized in that: the volume ratio of the polyethylene glycol 2000 to the ammonia water to the mixed solution is 10:1: 16-18.
5. The method for producing a flower-like nickel oxide composed of porous flakes according to any one of claims 1 to 4, wherein: the heating is carried out for 2-10h at 100-200 ℃.
6. The method for preparing a flower-like nickel oxide composed of porous flakes according to claim 5, wherein: the annealing treatment is specifically annealing at 450-600 ℃ for 1-3 h.
7. A preparation method of flower-shaped nickel oxide with porous flaky composition is characterized by comprising the following steps:
(1) dissolving nickel acetate tetrahydrate in distilled water to form a nickel acetate solution, dissolving PVA and urea in distilled water to form a mixed solution, wherein the mass-to-volume ratio of the nickel acetate tetrahydrate to the distilled water is 0.374-0.648 g:5mL, and the mass-to-volume ratio of the PVA, the urea to the distilled water is 0.25 g: 0.24-0.5 g:5 mL;
(2) slowly adding the mixed solution into a nickel acetate solution, adding polyethylene glycol 2000, stirring while dropwise adding ammonia water with the mass concentration of 25-28%, continuously stirring at the speed of 300rpm for 10min after dropwise adding is completed to obtain a precursor solution, wherein the volume ratio of the polyethylene glycol 2000 to the ammonia water to the mixed solution is 10:1: 16-18;
(3) transferring the precursor solution obtained in the step (2) to a hydrothermal reaction kettle, and heating for 6-10 hours at 100-200 ℃;
(4) filtering and centrifuging the solution obtained in the step (3), washing the solution for a plurality of times by using ethanol and deionized water, and then drying the solution for 8 hours at 70 ℃;
(5) and (3) annealing the precursor obtained by drying in the step (4) at the temperature of 450-600 ℃ for 1-3h to obtain the black nickel oxide powder.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112266027A (en) * | 2020-10-22 | 2021-01-26 | 重庆文理学院 | Preparation method of honeycomb-shaped nickel oxide |
| CN113030194A (en) * | 2021-02-03 | 2021-06-25 | 中国科学院合肥物质科学研究院 | Gas sensor array, three alcohol types and identification method of concentration of three alcohol types |
| CN113388858A (en) * | 2021-05-18 | 2021-09-14 | 武汉工程大学 | Mesoporous nickel oxide nanoflower electrode for synthesizing ammonia by electrochemical reduction of nitrogen and preparation method thereof |
| CN113670991A (en) * | 2021-09-08 | 2021-11-19 | 大连理工大学 | Hematite-based single crystal room temperature gas-sensitive material exposing high-energy crystal face, and preparation method and application thereof |
| CN114527168A (en) * | 2022-02-24 | 2022-05-24 | 重庆文理学院 | Preparation method of respiration sensor for monitoring chronic kidney diseases |
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2020
- 2020-01-18 CN CN202010056488.5A patent/CN111115717A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112266027A (en) * | 2020-10-22 | 2021-01-26 | 重庆文理学院 | Preparation method of honeycomb-shaped nickel oxide |
| CN112266027B (en) * | 2020-10-22 | 2022-09-13 | 重庆文理学院 | Preparation method of honeycomb-shaped nickel oxide |
| CN113030194A (en) * | 2021-02-03 | 2021-06-25 | 中国科学院合肥物质科学研究院 | Gas sensor array, three alcohol types and identification method of concentration of three alcohol types |
| CN113388858A (en) * | 2021-05-18 | 2021-09-14 | 武汉工程大学 | Mesoporous nickel oxide nanoflower electrode for synthesizing ammonia by electrochemical reduction of nitrogen and preparation method thereof |
| CN113670991A (en) * | 2021-09-08 | 2021-11-19 | 大连理工大学 | Hematite-based single crystal room temperature gas-sensitive material exposing high-energy crystal face, and preparation method and application thereof |
| CN113670991B (en) * | 2021-09-08 | 2024-01-30 | 大连理工大学 | Hematite-based monocrystal room temperature gas-sensitive material exposing high-energy crystal face, and preparation method and application thereof |
| CN114527168A (en) * | 2022-02-24 | 2022-05-24 | 重庆文理学院 | Preparation method of respiration sensor for monitoring chronic kidney diseases |
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