CN111392764A - Preparation method of ZnO nanoparticles - Google Patents
Preparation method of ZnO nanoparticles Download PDFInfo
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- CN111392764A CN111392764A CN202010362607.XA CN202010362607A CN111392764A CN 111392764 A CN111392764 A CN 111392764A CN 202010362607 A CN202010362607 A CN 202010362607A CN 111392764 A CN111392764 A CN 111392764A
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- 239000002105 nanoparticle Substances 0.000 title claims description 55
- 238000002360 preparation method Methods 0.000 title description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- 239000002245 particle Substances 0.000 claims abstract description 33
- 230000006911 nucleation Effects 0.000 claims abstract description 26
- 238000010899 nucleation Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000007789 sealing Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000000126 substance Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 14
- 229910007541 Zn O Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000006228 supernatant Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 239000010408 film Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A process for preparing nano ZnO particles includes such steps as taking 5 ml of 0.8 mol/L ZnO sol by micropipette, taking 0.2 ml of 0.5 mol/L, dropping NaOH into said sol, transferring the mixed solution to reactor, sealing, heating in 80 deg.C water bath for 24 hr, and forming nano ZnO particles in the solution containing OH by two steps, one is the first step of fast nucleation and growth of ZnO particles under excess Zn2+ condition and the other is the first, the third and the fourth steps of nucleation and growth under excess OH condition.
Description
The technical field is as follows:
the invention relates to a preparation method of ZnO nanoparticles.
Background art:
the ZnO nano particles can be prepared according to the method, the ZnO nano particles required by the membrane switch can be met, and the membrane switch of the ZnO nano particles has the characteristics of simple structure, attractive and flat appearance, light and thin finished product, good sealing effect, light touch connection type, long service life and the like, overcomes the problems that the traditional membrane switch cannot be waterproof and dustproof, an internal circuit is easy to oxidize and the like, and is widely applied to computers, aerospace, communication, industrial equipment, office equipment and the like.
The invention content is as follows:
the invention aims to provide a ZnO nanoparticle preparation method which can meet ZnO nanoparticles required by a thin-film switch and has a good using effect.
The above purpose is realized by the following technical scheme:
a process for preparing nano ZnO particles includes such steps as taking 3-7 ml of 0.6-1.0 mol/L ZnO sol by micropipette, taking 0.1-0.3 ml 0.2-0.8 mol/L, dropping NaOH to ZnO sol to generate milky flocculent deposit, transferring the mixed solution to reactor, sealing, heating in 60-100 deg.C water bath for 20-28 hr, adding OH solution to solution, and preparing nano ZnO particles by one step2A first step and a second step of rapid nucleation and growth of ZnO particles under an excess condition; the other is a first step, a third step and a fourth step of slow nucleation and growth process under the condition of excessive OH, after the reaction is finished, taking out the reaction kettle, naturally cooling the reaction kettle to room temperature, and pouring out the supernatant to obtain a mixed substance of white Zn O nano particles and some organic residues; drying at 40-60 deg.C for 20-40min to volatilize organic substances to obtain white powder; and centrifuging, washing with water and alcohol, and ultrasonically oscillating the obtained particle product for multiple times to obtain pure white ZnO nanoparticles, and ultrasonically dispersing into absolute ethyl alcohol for later use.
The preparation method of the ZnO nano-particles comprises the steps of firstly taking 5 ml of 0.8 mol/L ZnO sol by using a micropipette, then taking 0.2 ml of 0.5 mol/L prepared according to a reaction metering ratio, secondly dropping NaOH into the ZnO sol, enabling milky flocculent precipitates to appear during dropping, transferring the mixed solution into a reaction kettle, covering and sealing the reaction kettle, placing the reaction kettle into a 80-DEG C constant-temperature water bath kettle for heating for 24 hours, thirdly, forming the ZnO nano-particles in an OH-containing solution in a fourth step by two ways, wherein one way is that the ZnO nano-particles are formed in Zn2A first step and a second step of rapid nucleation and growth of ZnO particles under an excess condition; the other is a first step, a third step and a fourth step of slow nucleation and growth process under the condition of excessive OH, after the reaction is finished, taking out the reaction kettle, naturally cooling the reaction kettle to room temperature, and pouring out the supernatant to obtain a mixed substance of white Zn O nano particles and some organic residues; drying at 50 deg.CDrying for 30 min to volatilize organic matter to obtain white powder; and centrifuging, washing with water and alcohol, and ultrasonically oscillating the obtained particle product for multiple times to obtain pure white ZnO nanoparticles, and ultrasonically dispersing into absolute ethyl alcohol for later use.
The preparation method of the ZnO nano-particles comprises the steps of firstly taking 3 ml of 0.6 mol/L ZnO sol by using a micropipette, then taking 0.1 ml of 0.2 mol/L prepared according to a reaction metering ratio, secondly dropping NaOH into the ZnO sol, enabling milky flocculent precipitates to appear during dropping, transferring the mixed solution into a reaction kettle, covering and sealing the reaction kettle, placing the reaction kettle into a 60-DEG C constant-temperature water bath kettle for heating for 20 hours, thirdly, forming the ZnO nano-particles in an OH-containing solution in a fourth step by two ways, wherein one way is that the ZnO nano-particles are formed in Zn2A first step and a second step of rapid nucleation and growth of ZnO particles under an excess condition; the other is a first step, a third step and a fourth step of slow nucleation and growth process under the condition of excessive OH, after the reaction is finished, taking out the reaction kettle, naturally cooling the reaction kettle to room temperature, and pouring out the supernatant to obtain a mixed substance of white Zn O nano particles and some organic residues; drying at 40 deg.C for 20 min to volatilize organic substances to obtain white powder; and centrifuging, washing with water and alcohol, and ultrasonically oscillating the obtained particle product for multiple times to obtain pure white ZnO nanoparticles, and ultrasonically dispersing into absolute ethyl alcohol for later use.
The preparation method of the ZnO nano-particles comprises the steps of firstly taking 7 ml of 1.0 mol/L ZnO sol by using a micropipette, then taking 0.3 ml of 0.8 mol/L prepared according to a reaction metering ratio, secondly dropping NaOH into the ZnO sol, enabling milky flocculent precipitates to appear during dropping, transferring the mixed solution into a reaction kettle, covering and sealing the reaction kettle, placing the reaction kettle into a 100 ℃ constant-temperature water bath kettle for heating for 28 hours, thirdly, forming the ZnO nano-particles in a solution containing OH, and fourthly, wherein one step is that the ZnO nano-particles are formed in a Zn solution2A first step and a second step of rapid nucleation and growth of ZnO particles under an excess condition; the other is the first step, the third step and the fourth step of slow nucleation and growth process under the condition of excessive OH, after the reaction is finished, the reaction kettle is taken out, and the reaction kettle is naturally cooled to the temperature ofAt room temperature, pouring out the supernatant to obtain a mixed substance of white Zn O nano particles and some organic residues; drying at 60 deg.C for 40min to volatilize organic substances to obtain white powder; and centrifuging, washing with water and alcohol, and ultrasonically oscillating the obtained particle product for multiple times to obtain pure white ZnO nanoparticles, and ultrasonically dispersing into absolute ethyl alcohol for later use.
Has the advantages that:
1. the preparation method disclosed by the invention has the advantages that each link is accurately controlled, the prepared ZnO nanoparticles can completely meet the requirements of preparing the thin film switch, and the prepared thin film switch has good quality.
The film switch mainly comprises a ZnO nano particle film, a conductive silver paste circuit layer, an insulating ink layer and the like, wherein the circuit of the film switch is formed by printing the conductive silver paste circuit, the circuit has the function of serving as a transmission medium of an electric signal, the distribution uniformity of the conductive silver paste layer directly influences the resistance characteristic of the conductive silver paste layer, the rapid production can be realized, and the production efficiency is improved: the light-cured insulating ink is tried to be used, so that the color difference of a finished product caused by hot air interference during the heat curing of an oven is avoided: proper process parameters are selected, so that the uniform thickness, the resistance matching and the small sawtooth edge effect of the conductive silver paste circuit are ensured.
Description of the drawings:
FIG. 1 is a diagram of a process for forming ZnO nanoparticles according to the present invention.
The specific implementation mode is as follows:
the technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the present invention.
Example 1:
a process for preparing nano ZnO particles includes such steps as taking 3-7 ml of ZnO sol (0.6-1.0 mol/L mol), taking 0.1-0.3 ml of 0.2-0.8 mol/L mol, dripping NaOH to said sol to generate milky flocculent deposit, transferring the mixture to reactor, sealing, heating in 60-100 deg.C water bath for 20-28 hr, and adding OH solutionIn the fourth step, the formation of the ZnO nanoparticles has two ways: one is in Zn2A first step and a second step of rapid nucleation and growth of ZnO particles under an excess condition; the other is a first step, a third step and a fourth step of slow nucleation and growth process under the condition of excessive OH, after the reaction is finished, taking out the reaction kettle, naturally cooling the reaction kettle to room temperature, and pouring out the supernatant to obtain a mixed substance of white Zn O nano particles and some organic residues; drying at 40-60 deg.C for 20-40min to volatilize organic substances to obtain white powder; and centrifuging, washing with water and alcohol, and ultrasonically oscillating the obtained particle product for multiple times to obtain pure white ZnO nanoparticles, and ultrasonically dispersing into absolute ethyl alcohol for later use.
Example 2:
a process for preparing ZnO nanoparticles as described in example 1 includes such steps as taking 5 ml of 0.8 mol/L ZnO sol by micropipette, taking 0.2 ml of 0.5 mol/L, dropping NaOH to ZnO sol to generate milky flocculent deposit, transferring the mixture to reactor, sealing, heating in 80 deg.C water bath for 24 hr, and adding OH solution to the solution to form ZnO nanoparticles2A first step and a second step of rapid nucleation and growth of ZnO particles under an excess condition; the other is a first step, a third step and a fourth step of slow nucleation and growth process under the condition of excessive OH, after the reaction is finished, taking out the reaction kettle, naturally cooling the reaction kettle to room temperature, and pouring out the supernatant to obtain a mixed substance of white Zn O nano particles and some organic residues; drying at 50 deg.C for 30 min to volatilize organic substances to obtain white powder; and centrifuging, washing with water and alcohol, and ultrasonically oscillating the obtained particle product for multiple times to obtain pure white ZnO nanoparticles, and ultrasonically dispersing into absolute ethyl alcohol for later use.
Example 3:
the preparation method of ZnO nanoparticles described in example 1 comprises the first step of taking 3 ml of ZnO sol 0.6 mol/L by micropipette, then taking 0.1 ml according to the reaction stoichiometric ratioPreparing 0.2 mol/L, dropping NaOH into ZnO sol to generate milky flocculent deposit, transferring the mixed solution to reactor, sealing, heating in 60 deg.C constant-temperature water bath for 20 hr, adding OH-contained solution, and forming ZnO nanoparticles2A first step and a second step of rapid nucleation and growth of ZnO particles under an excess condition; the other is a first step, a third step and a fourth step of slow nucleation and growth process under the condition of excessive OH, after the reaction is finished, taking out the reaction kettle, naturally cooling the reaction kettle to room temperature, and pouring out the supernatant to obtain a mixed substance of white Zn O nano particles and some organic residues; drying at 40 deg.C for 20 min to volatilize organic substances to obtain white powder; and centrifuging, washing with water and alcohol, and ultrasonically oscillating the obtained particle product for multiple times to obtain pure white ZnO nanoparticles, and ultrasonically dispersing into absolute ethyl alcohol for later use.
Example 4:
a process for preparing ZnO nanoparticles as described in example 1 includes such steps as taking 7 ml of ZnO sol (1.0 mol/L mol/0.3 ml of 0.8 mol/L (0.3 mol/0 mol/100 mol/0-mol/02A first step and a second step of rapid nucleation and growth of ZnO particles under an excess condition; the other is a first step, a third step and a fourth step of slow nucleation and growth process under the condition of excessive OH, after the reaction is finished, taking out the reaction kettle, naturally cooling the reaction kettle to room temperature, and pouring out the supernatant to obtain a mixed substance of white Zn O nano particles and some organic residues; drying at 60 deg.C for 40min to volatilize organic substances to obtain white powder; and centrifuging, washing with water and alcohol, and ultrasonically oscillating the obtained particle product for multiple times to obtain pure white ZnO nanoparticles, and ultrasonically dispersing into absolute ethyl alcohol for later use.
Claims (4)
1. A process for preparing nano ZnO particles includes such steps as taking 3-7 ml of 0.6-1.0 mol/L ZnO sol by micropipette, taking 0.1-0.3 ml of 0.2-0.8 mol/L prepared according to reaction metering ratio, dropping NaOH to ZnO sol to generate milky flocculent deposit, transferring the mixed solution to reactor, sealing, heating in 60-100 deg.C water bath for 20-28 hr, adding OH solution to the solution containing ZnO particles, and preparing nano ZnO particles by one step2A first step and a second step of rapid nucleation and growth of ZnO particles under an excess condition; the other is a first step, a third step and a fourth step of slow nucleation and growth process under the condition of excessive OH, after the reaction is finished, taking out the reaction kettle, naturally cooling the reaction kettle to room temperature, and pouring out the supernatant to obtain a mixed substance of white Zn O nano particles and some organic residues; drying at 40-60 deg.C for 20-40min to volatilize organic substances to obtain white powder; and centrifuging, washing with water and alcohol, and ultrasonically oscillating the obtained particle product for multiple times to obtain pure white ZnO nanoparticles, and ultrasonically dispersing into absolute ethyl alcohol for later use.
2. The process of claim 1, wherein the ZnO nanoparticles are prepared by the steps of taking 5 ml of 0.8 mol/L ZnO sol by a micropipette, taking 0.2 ml 0.5 mol/L prepared according to the reaction stoichiometric ratio, dripping NaOH into the ZnO sol to form milky flocculent precipitate, transferring the mixed solution into a reaction kettle, covering and sealing the reaction kettle, heating the reaction kettle in a constant-temperature water bath kettle at 80 ℃ for 24 hours, and forming the ZnO nanoparticles in the OH-containing solution by a third step2A first step and a second step of rapid nucleation and growth of ZnO particles under an excess condition; the other is the first step, the third step and the fourth step of slow nucleation and growth process under the condition of excessive OH, after the reaction is finished, the reaction kettle is taken out, and the reaction kettle is naturally cooled to the temperature ofAt room temperature, pouring out the supernatant to obtain a mixed substance of white Zn O nano particles and some organic residues; drying at 50 deg.C for 30 min to volatilize organic substances to obtain white powder; and centrifuging, washing with water and alcohol, and ultrasonically oscillating the obtained particle product for multiple times to obtain pure white ZnO nanoparticles, and ultrasonically dispersing into absolute ethyl alcohol for later use.
3. The process of claim 1, wherein the ZnO nanoparticles are prepared by the steps of firstly taking 3 ml of 0.6 mol/L ZnO sol by using a micropipette, then taking 0.1 ml 0.2 mol/L prepared according to the reaction stoichiometric ratio, secondly dropping NaOH into the ZnO sol to form milky flocculent precipitate, transferring the mixed solution into a reaction kettle, covering and sealing the reaction kettle, and heating the reaction kettle in a 60 ℃ constant temperature water bath for 20 hours, and thirdly in the solution containing OH, forming the ZnO nanoparticles by two ways, namely, in the first step, in the second step, in the third step, in the second step, in the2A first step and a second step of rapid nucleation and growth of ZnO particles under an excess condition; the other is a first step, a third step and a fourth step of slow nucleation and growth process under the condition of excessive OH, after the reaction is finished, taking out the reaction kettle, naturally cooling the reaction kettle to room temperature, and pouring out the supernatant to obtain a mixed substance of white Zn O nano particles and some organic residues; drying at 40 deg.C for 20 min to volatilize organic substances to obtain white powder; and centrifuging, washing with water and alcohol, and ultrasonically oscillating the obtained particle product for multiple times to obtain pure white ZnO nanoparticles, and ultrasonically dispersing into absolute ethyl alcohol for later use.
4. The process of claim 1, wherein the first step is carried out by taking 1.0 mol/L mol/7 ml ZnO sol by micropipette, taking 0.3 ml 0.8 mol/L prepared according to reaction metering ratio, the second step is carried out by dropping NaOH into ZnO sol, milky flocculent precipitate appears during dropping, the mixed solution is transferred into reactor, covered and sealed, and put into 100 ℃ constant temperature water bath for heating for 28 hours, the third step is carried out in OH-containing solution, and the fourth step is carried out by adding ZnO nanoparticles into OH-containing solutionThere are two ways of formation of (a): one is in Zn2A first step and a second step of rapid nucleation and growth of ZnO particles under an excess condition; the other is a first step, a third step and a fourth step of slow nucleation and growth process under the condition of excessive OH, after the reaction is finished, taking out the reaction kettle, naturally cooling the reaction kettle to room temperature, and pouring out the supernatant to obtain a mixed substance of white Zn O nano particles and some organic residues; drying at 60 deg.C for 40min to volatilize organic substances to obtain white powder; and centrifuging, washing with water and alcohol, and ultrasonically oscillating the obtained particle product for multiple times to obtain pure white ZnO nanoparticles, and ultrasonically dispersing into absolute ethyl alcohol for later use.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4282191A (en) * | 1980-07-25 | 1981-08-04 | Reynolds Metals Company | Zinc removal from aluminate solutions |
| CN101319371A (en) * | 2008-05-14 | 2008-12-10 | 陕西科技大学 | Production method of spindle-shaped nano ZnO monocrystal |
| CN106519306A (en) * | 2016-10-09 | 2017-03-22 | 浙江理工大学 | Cellulose based Ag @ ZnO nano composite hydrogel and preparation method thereof |
| CN106732793A (en) * | 2017-01-18 | 2017-05-31 | 浙江理工大学 | A kind of photocatalysis composite membrane material and preparation method thereof |
| CN109476496A (en) * | 2016-07-29 | 2019-03-15 | 荷兰联合利华有限公司 | Habit modified zincite crystal |
-
2020
- 2020-04-30 CN CN202010362607.XA patent/CN111392764A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4282191A (en) * | 1980-07-25 | 1981-08-04 | Reynolds Metals Company | Zinc removal from aluminate solutions |
| CN101319371A (en) * | 2008-05-14 | 2008-12-10 | 陕西科技大学 | Production method of spindle-shaped nano ZnO monocrystal |
| CN109476496A (en) * | 2016-07-29 | 2019-03-15 | 荷兰联合利华有限公司 | Habit modified zincite crystal |
| CN106519306A (en) * | 2016-10-09 | 2017-03-22 | 浙江理工大学 | Cellulose based Ag @ ZnO nano composite hydrogel and preparation method thereof |
| CN106732793A (en) * | 2017-01-18 | 2017-05-31 | 浙江理工大学 | A kind of photocatalysis composite membrane material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| SHWETA JAGTAP ET AL.: ""Evaluation of ZnO nanoparticles and study of ZnO–TiO2 composites for lead freehumidity sensors"", 《SENSORS AND ACTUATORS B: CHEMICAL》 * |
| 孙健等: "PEG软模板水热合成纳米氧化锌粉的研究", 《陶瓷学报》 * |
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