CN1101952A - Process for controlling zinc oxide crystal whisker growth by carbon reducer - Google Patents
Process for controlling zinc oxide crystal whisker growth by carbon reducer Download PDFInfo
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- CN1101952A CN1101952A CN 94111823 CN94111823A CN1101952A CN 1101952 A CN1101952 A CN 1101952A CN 94111823 CN94111823 CN 94111823 CN 94111823 A CN94111823 A CN 94111823A CN 1101952 A CN1101952 A CN 1101952A
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- zinc oxide
- crystal whisker
- oxide crystal
- zinc
- whisker growth
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Abstract
The technological method for growing zinc oxide crystal whisker mainly features use of powdered metal zinc as raw material and powdered coke as solid reducer. The zinc oxide crystal whisker comprising 4 needle-type monocrystals with 109 deg. crossing angle, each being 10-100 micrometers in length and 0.2-2 micrometers in root diameter, is prepared by controlling oxidation reaction speed of zinc vapour at 950-1050 deg.C and atmosphere pressure for 10-15 min. Said crystal wrisker may be used in metal, ceramic and high-molecular compound materials.
Description
The present invention relates to the investigation of materials field, relate generally to metal, pottery and polymer-based composite preparation and Application Areas.
At present, the whisker of having prepared in the world reaches tens of kinds, and its principal item is SiC, Si
3N
4, Al
2O
3Deng.Because its preparation temperature height, for example, β-SiC whisker preparation temperature is at 1400-1500 ℃, and the 2H-SiC whisker is 1900 ℃; The Processes and apparatus complexity; The influence of factors such as productivity is low costs an arm and a leg, and prospects for commercial application is remote.Above-mentioned in addition crystal whisker materials purposes is limited, only can be as the SiC whisker as metal, and the enhancing body of ceramic structure material uses.The ZnOw that PANASONIC industry company succeeds in developing, cost is lower, and has important application prospects on multi-functional field, thereby this kind material is the type material that marketable value is arranged in the present crystal whisker materials most.PANASONIC industry company prepares in the technology of ZnOw; be control ZnO whisker growth speed; metal zinc is carried out special warfare to be handled; for example melt and spray powder with pure Zn silk arc; place ion exchanged water to use mortar type mixing and kneading machine stir process 25 minutes in the Zn powder that makes; in 20 ℃ of water, placed 75 hours then; environment is an air atmosphere; removed moisture in 3 hours in 130 ℃ of dryings again; purpose is to allow the zinc powder surface form the stopping property oxide film; control whisker growth speed obtains the bigger high-quality crystal whisker materials of length-to-diameter ratio.This complex technical process has increased great amount of manpower and equipment input.
The purpose of this invention is to provide a kind of easy processing method of making high-performance four acicular type zinc oxide crystal whisker material.
Technical scheme of the present invention is: with zinc powder and coke powder is mixing raw material, is laid on container bottom, is heated to certain temperature in the atmosphere, and metallic zinc steam is at CO
2, CO, O
2In the mixed atmosphere, under promptly certain oxygen bias condition, slow oxidation, deposition growing, thus form the big four acicular type zinc oxide crystal whisker of length-to-diameter ratio.
The raw material of making the ZnOw use is a metal zinc, and its fusing point is 692.7K(420 ℃).Under comparatively high temps, zinc evaporation equilibrium partial pressure is very high, contacts very easily oxidation with the oxygen of air and grows up into granular zinc oxide rapidly.In the PANASONIC industry corporate system fabrication technique, the stopping property oxide film control zinc velocity of evaporation of utilizing the zinc powder surface to form slow down the speed of growth, but its treatment process is comparatively complicated.The present invention adopts the solid carbon reductive agent, oxygen partial pressure in the control stove, thus obtained better growth effect.
Fig. 1 is the thermodynamic principles figure of ZnO whisker growth of the present invention.
Fig. 2 is a ZnO whisker component X PS collection of illustrative plates.
Fig. 3 is a ZnO whisker polymer SEM shape appearance figure.
The invention will be further described below in conjunction with accompanying drawing: Fig. 1 is the thermodynamic principles figure of Atmosphere Control, is found out by figure, and solid carbon is combined with oxygen and is generated carbon dioxide, and the free energy of reaction system is low, and reaction expends a considerable amount of oxygen. Secondly, be combined the free energy of reaction that generates carbon monoxide with oxygen at 950 ℃ of above solid carbons of (about 1220K) temperature and also be lower than the oxidation reaction ability of zinc fume or solid zinc, so further reduce the partial pressure of oxygen in the furnace atmosphere, be conducive to the growth of ZnOw. As can be seen from Figure 1, be higher than 950 ℃, solid carbon is conducive to the formation of weak oxide atmosphere, thereby the speed of growth of control ZnOw obtains the big whisker of draw ratio.
Fig. 2 is the whisker fingerprints of measuring at XSAM-800 electron spectrometer (XPS), only occurs strong Zn(2p among the figure) peak, O(IS) peak shows that this material is the ZnOw material of based on very high purity.
Fig. 3 is ZnO whisker condensate ESEM shape appearance figure. ZnOw is made up of four whiskers bodies that middle mind-set three-dimensional launches as seen from the figure, and the length of every pin is 10-100 μ m, and angle is approximate 109 ° between per two adjacent needles of root diameter (RD) 0.2-2 μ m. For improving whisker morphology photograph definition, this sample carried out vacuum metallizing to be processed, and the white blocks sheet on the part pin is gold plaque.
Processing method having thus described the invention can produce high-purity and the big four acicular type zinc oxide crystal whisker of length-to-diameter ratio easily.This material is used to metal-base composites, and reinforced effects is remarkable; Make polymer composite, have strong microwave absorbing effect, have significant damping damping action simultaneously.
Embodiment:
Getting 100 gram particle degree is 60-120 purpose zinc powder, sneaks into the coke powder of the same granularity of 20 grams, is laid on the bottom of container, and the container that compound is housed is placed the high temperature cabinet-type electric furnace, and under the atmospheric environment, 950-1050 ℃ was heated 10-20 minute.Container bottom and cabinet-type electric furnace bottom grow the long 20-100 μ of pin m, the ZnOw of base diameter 0.2-2 μ m.About 100 grams of whisker yield, the outward appearance loose powdery accumulation body that is white in color, the about 0.04-0.1g/cm of proportion
3, press volumetric shrinkage on time, flexible sense.Except that container bottom had a little yellow meal, microscopic examination showed that whisker growth is all right, did not have thin part particle and occurred.
Claims (5)
1, a kind of process for controlling zinc oxide crystal whisker growth by carbon reducer is characterized in that metal zinc is mixed in the container of packing into the coke powder, and in air atmosphere, ZnOw is made in heating.
2, controlling zinc oxide crystal whisker growth by carbon reducer method according to claim 1 is characterized in that the metal zinc ingot fusion, is carrier with the atmosphere, sprays in the water, makes 60-120 order granularity zinc powder.
3, controlling zinc oxide crystal whisker growth by carbon reducer method according to claim 1 is characterized in that coke is ground to form fine powder, and its granularity is the 60-120 order.
4, controlling zinc oxide crystal whisker growth by carbon reducer method according to claim 1 is characterized in that zinc powder coke powder was prepared burden by 5: 1, mixes, and is laid on container bottom.
5, controlling zinc oxide crystal whisker growth by carbon reducer method according to claim 1 is characterized in that and will the container of mixed powder be housed, and under atmospheric condition Heating temperature 950-1050 ℃, 10-20 minute, is fired into ZnOw.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94111823 CN1031895C (en) | 1994-07-05 | 1994-07-05 | Process for controlling zinc oxide crystal whisker growth by carbon reducer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94111823 CN1031895C (en) | 1994-07-05 | 1994-07-05 | Process for controlling zinc oxide crystal whisker growth by carbon reducer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1101952A true CN1101952A (en) | 1995-04-26 |
| CN1031895C CN1031895C (en) | 1996-05-29 |
Family
ID=5035654
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94111823 Expired - Fee Related CN1031895C (en) | 1994-07-05 | 1994-07-05 | Process for controlling zinc oxide crystal whisker growth by carbon reducer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1031895C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1086211C (en) * | 1999-04-22 | 2002-06-12 | 中国科学院金属研究所 | Process for preparing four-leg crystal whisker of zinc oxide |
| CN101172044B (en) * | 2006-10-31 | 2010-06-16 | 株式会社东芝 | Ultrasonic probe and ultrasonic diagnostic apparatus |
| CN105200519A (en) * | 2015-10-20 | 2015-12-30 | 唐山建华科技发展有限责任公司 | Preparation method of sepiolite-tetrapod zinc oxide whisker composite material |
| CN105543962A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Method for preparing zinc oxide whiskers without lead oxide aid |
| CN105926029A (en) * | 2016-05-09 | 2016-09-07 | 郑州云江科技有限公司 | Method for quick synthesis of zinc oxide whiskers by means of microwaves |
| CN108505120A (en) * | 2018-04-04 | 2018-09-07 | 慈溪市嘉和新材料科技有限公司 | The production technology that zinc oxide composite crystal must be synthesized disposably |
| CN114150380A (en) * | 2021-10-29 | 2022-03-08 | 中广核研究院有限公司 | Zinc oxide crystal and preparation method thereof |
-
1994
- 1994-07-05 CN CN 94111823 patent/CN1031895C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1086211C (en) * | 1999-04-22 | 2002-06-12 | 中国科学院金属研究所 | Process for preparing four-leg crystal whisker of zinc oxide |
| CN101172044B (en) * | 2006-10-31 | 2010-06-16 | 株式会社东芝 | Ultrasonic probe and ultrasonic diagnostic apparatus |
| CN105200519A (en) * | 2015-10-20 | 2015-12-30 | 唐山建华科技发展有限责任公司 | Preparation method of sepiolite-tetrapod zinc oxide whisker composite material |
| CN105200519B (en) * | 2015-10-20 | 2017-10-31 | 唐山建华科技发展有限责任公司 | The preparation method of sepiolite four acicular type zinc oxide crystal whisker composite |
| CN105543962A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Method for preparing zinc oxide whiskers without lead oxide aid |
| CN105926029A (en) * | 2016-05-09 | 2016-09-07 | 郑州云江科技有限公司 | Method for quick synthesis of zinc oxide whiskers by means of microwaves |
| CN108505120A (en) * | 2018-04-04 | 2018-09-07 | 慈溪市嘉和新材料科技有限公司 | The production technology that zinc oxide composite crystal must be synthesized disposably |
| CN114150380A (en) * | 2021-10-29 | 2022-03-08 | 中广核研究院有限公司 | Zinc oxide crystal and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1031895C (en) | 1996-05-29 |
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