CN101748474B - Simple method for preparing linear zinc oxide whiskers - Google Patents
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- CN101748474B CN101748474B CN2010100100976A CN201010010097A CN101748474B CN 101748474 B CN101748474 B CN 101748474B CN 2010100100976 A CN2010100100976 A CN 2010100100976A CN 201010010097 A CN201010010097 A CN 201010010097A CN 101748474 B CN101748474 B CN 101748474B
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- zinc powder
- alms bowl
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000000919 ceramic Substances 0.000 claims abstract description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 20
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 235000011837 pasties Nutrition 0.000 claims description 6
- 238000007669 thermal treatment Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 9
- 239000013078 crystal Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 230000003750 conditioning effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 229910010272 inorganic material Inorganic materials 0.000 abstract 1
- 239000011147 inorganic material Substances 0.000 abstract 1
- 229910052749 magnesium Inorganic materials 0.000 abstract 1
- 239000011777 magnesium Substances 0.000 abstract 1
- 229910001092 metal group alloy Inorganic materials 0.000 abstract 1
- 239000002861 polymer material Substances 0.000 abstract 1
- 239000012779 reinforcing material Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002265 electronic spectrum Methods 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009997 thermal pre-treatment Methods 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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Abstract
The invention discloses a simple method for preparing linear zinc oxide whiskers, which belongs to preparation processes of inorganic crystal materials. The method comprises the steps of taking zinc powder as raw material, using deionized water solution of 0.1-1 per mill hydrogen peroxide for conditioning till paste state, grinding in a mortar for 10-30 minutes, placing for more than 48 hours at room temperature, and drying, thereby carrying out aging treatment on the zinc powder; placing the aged zinc powder in a ceramic mortar, placing in a high-temperature furnace, rapidly increasing the temperature to 1000-1100 DEG C, simultaneously introducing high-purity nitrogen at 0.3m3/h and compressed air at 0.01m3/h, and keeping the temperature for 1-1.5 hours; and taking out, naturally coolingto room temperature, and preparing the linear ZnO whiskers. The preparation device and the preparation process adopted by the method have the advantages of simple method, high production efficiency, good product quality, low preparation cost and industrial production. The linear zinc oxide whiskers can be used as function reinforcing materials of polymer materials, inorganic materials, aluminum, magnesium and other metal alloys, and can also be used for sensors, gas sensitive elements, light-emitting materials, piezoelectric materials and the like.
Description
Technical field
The present invention relates to a kind of inorganic crystal material preparation technology, particularly relate to a kind of easy method for preparing linear zinc oxide (ZnO) whisker.
Background technology
The ZnO whisker has excellent high-strength and characteristics such as high-modulus property, semiconductive, piezoelectricity, wave absorbtion, height ratio principal characteristic, bactericidal properties and thixotropy; The enhancing of polymer, inorganic and materials such as metal, alloy be can be widely used in, support of the catalyst, transmitter and gas sensor, luminescent material, piezoelectric, filtering material etc. also can be used for.The ZnO whisker has variform, comprising: four pin shapes, multiway, bar-shaped, wire, open tube, band shape, featheriness, array-like etc.; The ZnO whisker of linear/property (being also referred to as fibrous) is divided into nanometer and micron-sized again by its diameter dimension.Nanometer is linear/property ZnO whisker has a lot of reports, as: the nanometer that CN1252311C, CN100372776C and CN101319372A etc. are explained linear/diameter of property ZnO whisker is all in 100nm.On the other hand, because of well-known reason, whisker is a single crystal, and crystalline structure is complete, subsurface defect is few, large-sizedly relatively is difficult to obtain, and micron order is linear/and the pertinent literature of property ZnO whisker preparation is seldom.People such as Dai Ying have studied and have used alumina tube or crucible to be reaction vessel; And place silicon substrate (substrate) in its bottom, prepare linear ZnO whisker, several microns of its diameter 60～250nm, length (one dimension Preparation of Whiskers and growth mechanism. the Hubei chemical industry; 2003,4:8-9).Chinese invention patent CN1312324C discloses and has used Zinc oxide powder to be raw material, and graphite boat is a reaction vessel, and uses silicon, aluminum oxide etc. to be that substrate, prepared fibrous whisker length can reach the cms magnitude, and long-width ratio was up to 1000: 1.But its said method all need be reacted substrate, and used reaction vessel is less crucible of size or boat etc., the difficult large-scale commercial prodn that realizes.
Summary of the invention
The object of the present invention is to provide a kind of is the method for the linear ZnO whisker of feedstock production with the zinc powder easily, and prepared ZnO whisker is high-purity, uniform form, and diameter is 0.6～0.7 μ m, and mean length is 65 μ m, and length-to-diameter ratio is about 100, and productive rate is more than 95%.
The objective of the invention is to realize through following technical scheme:
A kind of easy method for preparing linear zinc oxide whiskers places the ceramic alms bowl of cleaning with aged zinc powder, puts into High Temperature Furnaces Heating Apparatus, is rapidly heated 1000～1100 ℃, feeds nitrogen and Air mixing gas simultaneously, is incubated 1～1.5 hour; Taking-up naturally cools to room temperature, makes linear ZnO whisker.
Described a kind of easy method for preparing linear zinc oxide whiskers; Its ageing zinc powder; Promptly can be raw material with zinc powder purity greater than 98%, the deionized water solution of the hydrogen peroxide with 0.1～1 ‰ transfers to pasty state, in mortar, grinds 10-30 minute; Put more than 48 hours at the stand under the room temperature, is dried and gets.
Described a kind of easy method for preparing linear zinc oxide whiskers; The ceramic alms bowl of its cleaning; The pottery alms bowl carries out bakingout process and cleaning in advance; Be about to ceramic alms bowl in High Temperature Furnaces Heating Apparatus, press following temperature programming thermal treatment: 500 ℃/30 minutes, 800 ℃/30 minutes, 1100 ℃/30 minutes, in stove, cool to room temperature then naturally; Heat treated ceramic alms bowl cleans in ultrasonic cleaner with deionized water, in loft drier, dries again, and is for use.
Described a kind of easy method for preparing linear zinc oxide whiskers, its nitrogen and Air mixing gas, high pure nitrogen 0.3m
3/ h and pressurized air 0.01m
3/ h.
Described a kind of easy method for preparing linear zinc oxide whiskers, its linear ZnO whisker, product is high-purity, uniform form, diameter is 0.6～0.7 μ m, and mean length is 65 μ m, and length-to-diameter ratio is about 100, and productive rate is more than 95%.
Advantage of the present invention and effect are:
Directly use zinc powder to be raw material; X-ray diffraction spectra (XRD) and electronic spectrum (EDS) confirm that this whisker has the hexagonal system wurtzite crystal structure, and are high-purity ZnO whisker, and ESEM (SEM) confirms that prepared ZnO whisker all is linear; And uniform form, and productive rate is high;
Used preparation facilities (conventional ceramic alms bowl and High Temperature Furnaces Heating Apparatus) and high-temperature roasting process method are simple, stable, good reproducibility, and production efficiency is high; Constant product quality, quality better, preparation cost is low, but suitability for industrialized production.
Linear ZnO whisker of the present invention has excellent high-strength and characteristics such as high-modulus property, semiconductive, piezoelectricity, wave absorbtion, height ratio principal characteristic, bactericidal properties and thixotropy; The enhancing of polymer, inorganic and materials such as metal, alloy be can be widely used in, support of the catalyst, transmitter and gas sensor, luminescent material, piezoelectric, filtering material etc. also can be used for.
Description of drawings
Fig. 1 is wire ZnO whisker SEM (line bunch);
Fig. 2 is wire ZnO whisker SEM (single);
Fig. 3 is the XRD figure spectrum of wire ZnO whisker;
Fig. 4 is the EDS spectrogram of wire ZnO.
Annotate: accompanying drawing of the present invention is a form effect synoptic diagram (photo), literal among the figure or the unintelligible understanding that does not influence technical scheme of the present invention of numeral.
Embodiment
(1) zinc powder ageing: zinc powder is transferred to pasty state with the deionized water solution of hydrogen peroxide, in mortar, ground 10-30 minute, put more than 48 hours at the stand under the room temperature, is dried again;
(2) ceramic alms bowl thermal pretreatment: ceramic alms bowl is placed High Temperature Furnaces Heating Apparatus, press following temperature programming thermal treatment: 500 ℃/30 minutes, 800 ℃/30 minutes, 1100 ℃/30 minutes, in stove, cool to room temperature then naturally;
(3) ceramic alms bowl cleaning: heat treated ceramic alms bowl is dried in loft drier after in ultrasonic cleaner, cleaning 10 minutes with deionized water;
(4) high-temperature roasting: aged zinc powder is placed the ceramic alms bowl of cleaning, put into High Temperature Furnaces Heating Apparatus then, be rapidly heated 1000～1100 ℃, feed high pure nitrogen 0.3m simultaneously
3/ h and pressurized air 0.01m
3/ h is incubated 1～1.5 hour; Taking-up naturally cools to room temperature, makes linear ZnO whisker.
Embodiment 1
Commercially available purity 98% zinc powder transfers to pasty state with the deionized water solution of 0.1 ‰ hydrogen peroxide, in mortar, grinds 30 minutes, and put 48 hours at the stand under the room temperature, is dried again; Ceramic alms bowl is placed High Temperature Furnaces Heating Apparatus, press following temperature programming thermal treatment: 500 ℃/30 minutes, 800 ℃/30 minutes, 1100 ℃/30 minutes, in stove, cool to room temperature then naturally; Heat treated ceramic alms bowl is dried in loft drier after in ultrasonic cleaner, cleaning 10 minutes with deionized water; Aged zinc powder is placed the ceramic alms bowl of cleaning, put into High Temperature Furnaces Heating Apparatus, be rapidly heated 1100 ℃, feed high pure nitrogen 0.3m simultaneously
3/ h and pressurized air 0.01m
3/ h is incubated 1.5 hours; Taking-up naturally cools to room temperature, and prepared ZnO whisker uniform form, dimensional stabilizing all are linear.
Use purity 99.99% zinc powder instead and transfer to pasty state with the deionized water solution of 1 ‰ hydrogen peroxide, in mortar, only ground 10 minutes, other ageing conditions and ceramic alms bowl pre-treatment are with embodiment 1; 1000 ℃ of high-temperature roasting temperature are incubated 1 hour, and other processing condition are with embodiment 1, and product is with embodiment 1 indistinction.
Embodiment 3
Use purity 99.5% zinc powder instead and transfer to pasty state with the deionized water solution of 0.5 ‰ hydrogen peroxide, in mortar, only ground 20 minutes, cleaned 20 minutes, other ageing conditions and ceramic alms bowl pre-treatment are with embodiment 1; 1050 ℃ of high-temperature roasting temperature are incubated 1 hour, and other processing condition are with embodiment 1, and product is with embodiment 1 indistinction.
Comparative example 1
Press embodiment 1 step and implement, but used zinc powder purity is 97% that obtained product also has part platelet and multiway whisker except that linear ZnO whisker size is inhomogeneous, linear whisker productive rate is about 70%.
Comparative example 2
Press embodiment 1 step and implement, but zinc powder is only used the deionized water ageing, obtained product is the mixture of various form whiskers and platelet.Comparative example 3
Press embodiment 1 step and implement, but ceramic alms bowl is not done thermal treatment, after high-temperature roasting, ceramic alms bowl bursts, and linear whisker is scattered in the High Temperature Furnaces Heating Apparatus, the dimensional homogeneity variation.
Comparative example 3
Press embodiment 1 step and implement, but change high pure nitrogen and pressurized air amount ratio, the linear whisker amount of obtained product reduces, and the whisker and the platelet of other forms of part are arranged.
Claims (1)
1. method for preparing easily linear zinc oxide whiskers is characterized in that: aged zinc powder is placed the ceramic alms bowl of cleaning, put into High Temperature Furnaces Heating Apparatus, be rapidly heated 1000～1100 ℃, feed nitrogen and Air mixing gas simultaneously, be incubated 1～1.5 hour; Taking-up naturally cools to room temperature, makes linear ZnO whisker;
Said ageing zinc powder promptly can be raw material with zinc powder purity greater than 98%, and the deionized water solution of the hydrogen peroxide with 0.1～1 ‰ transfers to pasty state, in mortar, grinds 10-30 minute, and put more than 48 hours at the stand under the room temperature, is dried and gets;
The ceramic alms bowl of said cleaning, ceramic alms bowl carry out bakingout process and cleaning in advance, are about to ceramic alms bowl in High Temperature Furnaces Heating Apparatus, press following temperature programming thermal treatment: 500 ℃/30 minutes, 800 ℃/30 minutes, 1100 ℃/30 minutes, in stove, cool to room temperature then naturally; Heat treated ceramic alms bowl cleans in ultrasonic cleaner with deionized water, in loft drier, dries again, and is for use;
Said nitrogen and Air mixing gas, high pure nitrogen 0.3m
3/ h and pressurized air 0.01m
3/ h;
The linear ZnO whisker of gained, product is high-purity, uniform form, diameter is 0.6～0.7 μ m, and mean length is 65 μ m, and length-to-diameter ratio is about 100, and productive rate is more than 95%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010100100976A CN101748474B (en) | 2010-01-12 | 2010-01-12 | Simple method for preparing linear zinc oxide whiskers |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010100100976A CN101748474B (en) | 2010-01-12 | 2010-01-12 | Simple method for preparing linear zinc oxide whiskers |
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| CN101748474A CN101748474A (en) | 2010-06-23 |
| CN101748474B true CN101748474B (en) | 2012-06-27 |
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| CN105543962A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Method for preparing zinc oxide whiskers without lead oxide aid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5066475A (en) * | 1987-12-29 | 1991-11-19 | Matsushita Electric Industrial Co., Ltd. | Zinc oxide whiskers having a novel crystalline form and method for making same |
| CN1566417A (en) * | 2003-06-17 | 2005-01-19 | 中南大学 | Process for preparing zinc oxide crystal whisker |
| CN1814864A (en) * | 2005-01-31 | 2006-08-09 | 中南大学 | Method for preparing nano four-needle-shape zinc oxide crystal whisker |
-
2010
- 2010-01-12 CN CN2010100100976A patent/CN101748474B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5066475A (en) * | 1987-12-29 | 1991-11-19 | Matsushita Electric Industrial Co., Ltd. | Zinc oxide whiskers having a novel crystalline form and method for making same |
| CN1566417A (en) * | 2003-06-17 | 2005-01-19 | 中南大学 | Process for preparing zinc oxide crystal whisker |
| CN1814864A (en) * | 2005-01-31 | 2006-08-09 | 中南大学 | Method for preparing nano four-needle-shape zinc oxide crystal whisker |
Non-Patent Citations (4)
| Title |
|---|
| <>陈尔凡等.四脚状氧化锌晶须的制备及微观形态研究.<<高等学校化学学报>>.2000,第21卷(第2期),172-176. * |
| 税安泽等.氧化锌晶须的制备及生长机理研究.<<材料导报>>.2006,第20卷124-126. * |
| 陈尔凡等.不同形态低维ZnO晶须的制备及表征.<<材料工程>>.2008,(第6期),1-4. * |
| 陈尔凡等.四脚状氧化锌晶须的制备及微观形态研究.<<高等学校化学学报>>.2000,第21卷(第2期),172-176. |
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