CN101899708B - Tetrapod-like zinc oxide/ferrite film material and preparation method thereof - Google Patents
Tetrapod-like zinc oxide/ferrite film material and preparation method thereof Download PDFInfo
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- CN101899708B CN101899708B CN2010102349983A CN201010234998A CN101899708B CN 101899708 B CN101899708 B CN 101899708B CN 2010102349983 A CN2010102349983 A CN 2010102349983A CN 201010234998 A CN201010234998 A CN 201010234998A CN 101899708 B CN101899708 B CN 101899708B
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Abstract
The invention discloses a tetrapod-like zinc oxide whisker/ferrite film material and a preparation method thereof. The tetrapod-like zinc oxide whisker/ferrite film material has good wave absorbing performance. The preparation method for the tetrapod-like zinc oxide whisker/ferrite film material realizes chemical plating of ferrite on the surface of the tetrapod-like zinc oxide whisker under the condition of the low temperature of between 60 and 80DEG C, and successfully prepares a layer of ferrite film on the surface of the tetrapod-like zinc oxide whisker.
Description
Technical field
The present invention relates to a kind of four horn shape zinc oxide/ferrite thin film materials and preparation method thereof, particularly relate to a kind of method for preparing four horn shape ZnOw/ferrite thin film materials at four horn shape ZnOw surface chemistry coating ferrite films.
Background technology
Zinc oxide is a kind of multi-function metal oxide material, is widely used in each field such as chemical industry, light industry, electronics.Four horn shape ZnOws except that the semi-conductor similar with the ZnO powder body material, piezoelectricity and function such as antibiotic are arranged, functional performances such as high temperature, wear-resisting, damping, noise reduction also owing to the singularity of its structure has HS, high-modulus.In the 5-18GHz wave band, it inhales the ripple amount is 5-16.68dB, is the dielectric loss type material.In addition, the apparent specific gravity Gongwei 0.01-0.5 of ZnOw makes absorbing material with it, will be than the light 1-2 one magnitude of other most absorbing materials.
Ferrite is present the most widely used a kind of absorbing material, but because its density is big, and range of application has received certain restriction, and ferrite and other light material compound is one of effective way that obtains the light high performance absorbing material.Ferritic preparation mainly contains sintering process, self-propagating combustion etc. at present, generally needs high temperature.
Ferrite chemical plating is a kind of technology that is different from traditional chemical plating, and it is a kind ofly can under low temperature (less than 1O0 ℃) condition, from solution, directly ferrite be plated on the chemical plating method on the matrix.This makes on the particle of resistance toheat difference or Powdered matrix plating ferrite film and then preparation high-performance wave-absorbing material become possibility.
Carrying out electroless plating plating ferrite film on the surface of four horn shape ZnOws, prepare four horn shape ZnOw/ferrite thin film materials at low temperatures, is the effective ways of preparation high-performance wave-absorbing material.
Summary of the invention
The present invention has successfully prepared a kind of well behaved absorbing material, and concrete summary of the invention is following:
Four horn shape ZnOws can adopt oxidation style to make.Basic technology is heated to 1000 ℃ for ceramic crucible is put into retort furnace.Zinc powder and iron powder are put into crucible by a certain percentage, behind the insulation 5min, close retort furnace, take out the crucible air cooling, can obtain product to room temperature.Four horn shape ZnOws also can be bought through businessman and obtain.
The size of general four horn shape ZnOws is at the 0.5-10 micron, preferably at the 1-8 micron, particularly preferably in the 2-4 micron.
The present invention has obtained a kind of surface and has been covered with the ferritic four horn shape ZnOws of one deck through chemical plating method, and the thickness of ferrite layer is 1-100nm, is preferably 10-90nm, is preferably 30-50nm especially;
Above-mentioned surface is covered with one deck ferrite (Fe
3O
4) the chemical plating method of four horn shape ZnOws do
(1) get four horn shape ZnOw 0.2-1g, water washes repeatedly;
(2) in the reaction vessel that has whipping appts, add 100-150mL water, and feed protective gas, be heated to 60-80 ℃;
(3) be incubated and add four horn shape ZnOws, stir;
(4) drip the FeCl of 0.2～0.4mol/L respectively with the interpolation speed of 1～2ml/min and 4～5ml/min
24H
2O solution 10mL, and 60mL is with the CH of 1: 2 volume ratio blended 3～5mol/L
3COONH
4The NaNO of solution and 2-3g/L
2Solution, and the pH that controls reaction solution in the reaction vessel in real time is between 7-8;
(5) more than the insulation reaction 10min, after having reacted repeatedly filtration and washing obtain product.
Wherein reaction vessel is preferably four-hole boiling flask in the step (2), and protective gas is nitrogen or rare gas element;
Stirring velocity is 200-500r/min in the step (3), preferably uses 300-400r/min;
During step (4) control pH, use pH meter to measure the feedback bath pH value, pH value of solution is in specifying the pH scope in the whole electroless plating process to keep to drip pH adjustment agent, and pH adjustment agent is a NaOH solution, and ammoniacal liquor or other do not influence the basic soln that technology is carried out;
The water that uses in steps be deionized water.
The some samples that prepare are carried out the XRD test, relevant for Fe
3O
4With the obvious characteristic peak of zinc oxide, show and contain ferrite and zinc oxide in this product that carry out SEM thereafter and observe, can obviously observe the whisker surface has ferrite film to generate, through measuring the ferrite thickness that can obtain four horn shape ZnOws surface.
The present invention has realized under low temperature (60-80 ℃), four horn shape ZnOws being carried out ferrite chemical plating, and at four horn shape ZnOw surface preparation ferrite films, four horn shape ZnOw/Ferrite Materials of preparation have microwave absorbing property.The filler that this product can be used as microwave absorbing coating uses, and has broad application prospects.
Description of drawings
Fig. 1 is the XRD figure of the crystal whisker materials of four horn shape ZnOw/Ferrite Materials of preparing;
Fig. 2 is the SEM photo of crystal whisker materials of four horn shape ZnOw/Ferrite Materials of embodiment 1 preparation;
Fig. 3 is the SEM photo of crystal whisker materials of four horn shape ZnOw/Ferrite Materials of embodiment 2 preparation;
Fig. 4 is the SEM photo of crystal whisker materials of four horn shape ZnOw/Ferrite Materials of embodiment 3 preparation;
Fig. 5 is that four horn shape ZnOw/Ferrite Materials and the paraffin volume ratio of embodiment 1 preparation is to mix at 9: 1; Process coaxial sample; The reflectance curve figure of product under the different thickness of testing its electromagnetic parameter and calculating according to transmission line theory, range of frequency is 2～18GHz;
Fig. 6 is that four horn shape ZnOw/Ferrite Materials and the paraffin volume ratio of embodiment 2 preparation is to mix at 9: 1; Process coaxial sample; The reflectance curve figure of product under the different thickness of testing its electromagnetic parameter and calculating according to transmission line theory, range of frequency is 2～18GHz;
Fig. 7 is that four horn shape ZnOw/Ferrite Materials and the paraffin volume ratio of embodiment 3 preparation is to mix at 9: 1; Process coaxial sample; The reflectance curve figure of product under the different thickness of testing its electromagnetic parameter and calculating according to transmission line theory, range of frequency is 2～18GHz.
Embodiment
To combine accompanying drawing and embodiment that the present invention is done further detailed description below.
(1) get four horn shape ZnOw 0.2g, it is subsequent use to wash the back repeatedly with deionized water;
(2) in four-hole boiling flask, add the 100ml deionized water, magnetic agitation also feeds protective gas nitrogen, is heated to 80C;
(3) be incubated and add four horn shape ZnOws, stir (300r/min);
(4) drip the FeCl of 0.2mol/L respectively with the speed of 1mL/min and 4mL/min
24H
2O solution 10mL, and 60mL is with the CH of 1: 2 volume ratio blended 3mol/L
3COONH
4The NaNO of solution and 2g/L
2Solution uses pH meter to measure the feedback bath pH value simultaneously, drips NaOH solution simultaneously to keep in the whole electroless plating process in the four-hole boiling flask pH of reaction solution liquid between 7-8;
(5) reaction obtains product with the deionized water filtration and washing after 10 minutes repeatedly.
Product is after SEM observes, and the thickness of ferrite layer is 10-100nm.
(1) get four horn shape ZnOw 1g, it is subsequent use to wash the back repeatedly with deionized water;
(2) in four-hole boiling flask, add the 150ml deionized water, magnetic agitation also feeds protective gas nitrogen, is heated to 70 ℃;
(3) after the homo(io)thermism, add four horn shape ZnOws, stir (400r/min);
(4) drip the FeCl of 0.4mol/L respectively with the speed of 2mL/min and 5mL/min
24H
2O solution 10mL, and 60mL is with the CH of 1: 2 volume ratio blended 5mol/L
3COONH
4The NaNO of solution and 3g/L
2Solution uses pH meter to measure the feedback bath pH value, drips NaOH solution to keep in the whole electroless plating process in the four-hole boiling flask pH of reaction solution between 7-8;
(5) reaction is 30 minutes, obtains product with the deionized water filtration and washing repeatedly.
Product is after SEM observes, and the thickness of ferrite layer is 1-30nm.
Embodiment 3
(1) get four horn shape ZnOw 0.5g, it is subsequent use to wash the back repeatedly with deionized water;
(2) in reaction vessel, add the 100ml deionized water, magnetic agitation also feeds protective gas nitrogen, is heated to 60 ℃;
(3) after the homo(io)thermism, add four horn shape ZnOws, stir (300r/min);
(4) drip the FeCl of 0.4mol/L respectively with the speed of 2mL/min and 5mL/min
24H
2O solution 10mL, and 60mL is with the CH of 1: 2 volume ratio blended 3mol/L
3COONH
4The NaNO of solution and 2g/L
2Solution uses pH meter to measure the feedback bath pH value, and dropping ammonia solution is to keep in the whole electroless plating process in the reaction vessel pH of reaction solution between 7-8;
(5) reaction is 20 minutes, obtains product with the deionized water filtration and washing repeatedly.
Product is after SEM observes, and the thickness of ferrite layer is 30-40nm.
Claims (5)
1. one kind prepares the preparation method that coating surface has the ferritic four horn shape ZnOws of one deck, it is characterized in that, concrete preparing method's step is:
(1) get four horn shape ZnOw 0.2-1g, water washes repeatedly;
(2) in the reaction vessel that has whipping appts, add 100-150mL water, and feed protective gas, be heated to 60-80 ℃;
(3) be incubated and add four horn shape ZnOws, stir;
(4) drip the FeCl of 0.2～0.4mol/L respectively with the interpolation speed of 1～2mL/min and 4～5mL/min
24H
2O solution 10mL, and 60mL is with the CH of 1: 2 volume ratio blended 3～5mol/L
3COONH
4The NaNO of solution and 2-3g/L
2Solution, and the pH that controls reaction solution in the reaction vessel in real time is between 7-8;
(5) more than the insulation reaction 10min, after having reacted repeatedly filtration and washing obtain product.
2. preparation method according to claim 1, wherein step (4) when controlling pH in real time uses pH meter to measure the feedback bath pH value, drips pH adjustment agent simultaneously to keep in the whole electroless plating process in the reaction vessel pH of reaction solution in specifying the pH scope.
3. preparation method according to claim 2, pH adjustment agent is that NaOH solution, ammoniacal liquor or other do not influence the basic soln that technology is carried out.
4. preparation method according to claim 1, protective gas is nitrogen or rare gas element.
5. preparation method according to claim 1, the water that is used in steps is deionized water.
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| CN2010102349983A CN101899708B (en) | 2010-07-23 | 2010-07-23 | Tetrapod-like zinc oxide/ferrite film material and preparation method thereof |
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| CN101899708B true CN101899708B (en) | 2012-02-01 |
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| EP3049550B1 (en) * | 2013-09-25 | 2018-05-23 | ATOTECH Deutschland GmbH | Method for depositing a copper seed layer onto a barrier layer and copper plating bath |
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| CA2005746C (en) * | 1988-12-19 | 1994-05-31 | Minoru Yoshinaka | Soundproofing materials |
| CN1298039A (en) * | 1999-12-01 | 2001-06-06 | 肖猛 | Zinc oxide whisker coated with metal layer |
| JP3837540B2 (en) * | 2003-03-28 | 2006-10-25 | 独立行政法人物質・材料研究機構 | Method for producing single crystal tubular zinc oxide whisker |
| CN1320176C (en) * | 2005-05-08 | 2007-06-06 | 西南交通大学 | Magnetic modified nanometer zinc oxide whiskers and production thereof |
| CN101260567A (en) * | 2007-12-14 | 2008-09-10 | 华南理工大学 | Modified four-feet needle-shaped zinc oxide crystal whisker and preparation method thereof |
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