CN106315639A - Ultrasonic preparation method of high-purity ZnAl2O4 nano particles - Google Patents
Ultrasonic preparation method of high-purity ZnAl2O4 nano particles Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
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Abstract
The invention provides an ultrasonic preparation method of high-purity ZnAl2O4 nano particles. The method comprises the following steps that 1, aluminum powder and zinc powder are ground; 2, the ground zinc powder and zinc powder are subjected to ultrasonic hydrolysis, and an aluminum hydroxide colloidal solution and a zinc hydroxide colloidal solution are obtained; 3, the aluminum hydroxide colloidal solution and the zinc hydroxide colloidal solution are ground after being dried, and aluminum hydroxide powder and zinc oxide powder are obtained; 4, the aluminum hydroxide powder is calcined and ground, and gamma-Al2O3 powder is obtained; 5, the gamma-Al2O3 powder and the zinc oxide powder are mixed, then ultrasonic activation is carried out, and mixed sol is obtained; 6, the mixed sol is dried, and mixed powder is obtained after grinding; 7, the mixed powder is calcined and ground, and the ZnAl2O4 nano particles are obtained. According to the ultrasonic preparation method of the high-purity ZnAl2O4 nano particles, the raw materials are easy to obtain, the method is suitable for industrial production, the ZnAl2O4 nano particles prepared through the preparation method are high in purity and even in granularity distribution, and the obvious agglomeration phenomenon is avoided.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, be specifically related to a kind of high-purity ZnAl2O4The ultrasonic system of nano-particle
Preparation Method.
Background technology
Bimetal composite oxide is the calcined product of a class inorganic lamellar material, wherein ZnAl2O4There is high-melting-point
(1950 DEG C), and low thermal coefficient of expansion (25-900 DEG C, 7.0x 106/ DEG C), the feature such as Mohs' hardness big (8), to alkaline and acid
It is provided simultaneously with stronger resistant function, has that preferable heat stability, mechanical resistance be hot, a performance such as hydrophilic and ultraviolet impedance,
Be catalyzed, adsorb, the field such as sensing is increasingly paid close attention to by expert, scholar.ZnAl2O4Existing certain application, example in the industry
As the filter of copper in molten steel, as the auxiliary agent of reduction sulfur content of catalytic cracking gasoline, substitute mullite raw material system
Standby blast furnace ceramic cup material etc..Along with the development of nanotechnology, when particle size reaches nanometer scale, nano material is distinctive
Small-size effect, skin effect, quantum size effect and macro quanta tunnel effect, widened ZnAl further2O4Application model
Enclose.
At present, ZnAl2O4The preparation method of nano-particle is predominantly: solid-phase synthesis, coprecipitation, sol-gal process,
Hydro-thermal method, microemulsion and template etc..Every kind of method has one's own knack, but also has the place of deficiency.
Chinese invention patent (Publication No. CN102583467A) discloses one
Precursor prepares the method for gahnite, and the method is by the divalent zinc salt of different mol ratio, trivalent aluminium salt and CO (NH2)2Mixing
Rear addition deionized water obtains mixing salt solution, 70 DEG C of-110 DEG C of oil baths heating, and stirring stands, cooling, after the grinding of gained filter cake
Zinc-aluminum gavite presoma.Gained zinc-aluminum gavite presoma is placed in Muffle furnace, is warming up to 700 DEG C-1000 DEG C, protect
Temperature 1-5 hour, is cooled to room temperature, obtains ZnAl2O4Spinelle.Although the gahnite component that this method obtains is homogeneous, grain
Spending little, raw material availability is higher；But this method ingredient requirement is higher, and impurity is the most more.
Summary of the invention
The present invention is carried out for solving the problems referred to above, it is therefore intended that provide a kind of raw material to be easy to get, the ZnAl obtained2O4
High-purity ZnAl that nano-particle purity is high2O4The supersonically preparation method of nano-particle.
The technical solution used in the present invention is as follows:
The invention provides a kind of high-purity ZnAl2O4The supersonically preparation method of nano-particle, has the feature that, including
Following steps:
Step one, grinds aluminium powder and zinc powder certain time under conditions of noble gas respectively, respectively obtains certain grain
The aluminium powder in footpath and zinc powder；
Step 2, aluminium powder after grinding and after grinding zinc powder be respectively put into two equipped with in the beaker of deionized water, and
Carry out ultrasonic hydrolysis reaction, respectively obtain aluminium hydroxide gel liquid solution and zinc hydroxide colloid solution；
Step 3, grinds under predetermined baking temperature after drying by aluminium hydroxide gel liquid solution and zinc hydroxide colloid solution
Mill, respectively obtains aluminium-hydroxide powder and Zinc oxide powder；
Step 4, by aluminium-hydroxide powder roasting under certain sintering temperature, grinds after insulation and obtains γ-Al2O3Powder；
Step 5, by γ-Al2O3Powder and Zinc oxide powder are 1:1 mix homogeneously in molar ratio, put into equipped with deionization
After in the beaker of water, ultrasonic activation 3～8h, obtain mixed sols；
Step 6, is dried mixed sols 4～8h at a temperature of 60～120 DEG C, obtains γ-Al after grinding2O3With zinc oxide
Mixed-powder；
Step 7, by mixed-powder roasting at a predetermined temperature, takes out after insulation and grinds, obtain ZnAl2O4Nano-particle.
At high-purity ZnAl that the present invention provides2O4In the supersonically preparation method of nano-particle, it is also possible to there is such spy
Levying: wherein, in step one, noble gas is argon.
At high-purity ZnAl that the present invention provides2O4In the supersonically preparation method of nano-particle, it is also possible to there is such spy
Levying: wherein, in step one, aluminium powder and zinc powder grind in roll-in oscillating mill, and the milling time of aluminium powder is 1～3h, zinc
The milling time of powder is 10～15h.
At high-purity ZnAl that the present invention provides2O4In the supersonically preparation method of nano-particle, it is also possible to there is such spy
Levying: wherein, in step one, the particle diameter of the aluminium powder after grinding is in 0.5～0.8 μ m, and the particle diameter of the zinc powder after grinding is 5
～10 in the range of μm.
At high-purity ZnAl that the present invention provides2O4In the supersonically preparation method of nano-particle, it is also possible to there is such spy
Levying: wherein, in step 2, ultrasonic hydrolysis reaction is to carry out in ultrasonic cleaner, the supersonic frequency of ultrasonic cleaner
For 22kHz, the deionized water ultrasonic time containing aluminium powder is 2～4h, the deionized water ultrasonic time containing zinc powder be 18～
30h。
At high-purity ZnAl that the present invention provides2O4In the supersonically preparation method of nano-particle, it is also possible to there is such spy
Levying: wherein, in step 3, predetermined baking temperature is in the range of 60～120 DEG C.
At high-purity ZnAl that the present invention provides2O4In the supersonically preparation method of nano-particle, it is also possible to there is such spy
Levying: wherein, in step 4, the sintering temperature of aluminium-hydroxide powder is in the range of 250～350 DEG C.
At high-purity ZnAl that the present invention provides2O4In the supersonically preparation method of nano-particle, it is also possible to there is such spy
Levying: wherein, in step 7, predetermined temperature is in the range of 600～900 DEG C.
Invention effect and effect
The invention provides a kind of high-purity ZnAl2O4The supersonically preparation method of nano-particle, this preparation method first by aluminium powder and
Zinc powder vibro-grinding；Then aluminium powder and zinc powder after grinding carry out ultrasonic carrying out ultrasonic hydrolysis reaction respectively；Again by ultrasonic water
Solve reacted aluminium hydroxide gel liquid solution to grind after drying with zinc hydroxide colloid solution, obtain aluminium-hydroxide powder and oxidation
Zinc powder；Further aluminium-hydroxide powder roasting is ground and obtain γ-Al2O3Powder, after finally grinding
γ-Al2O3It is dried after powder and Zinc oxide powder 1:1 in molar ratio mixing ultrasonic activation, roasting, grinds
To high-purity ZnAl2O4Nano-particle.High-purity ZnAl of the present invention2O4The supersonically preparation method raw material of nano-particle is easy to get, preparation side
Method is simple, it is adaptable to industrialized production, the preparation method of the present invention ZnAl prepared2O4Nano-particle purity is high, particle size distribution
Uniformly, without obvious agglomeration.
Accompanying drawing explanation
Fig. 1 a is high-purity ZnAl that the embodiment of the present invention one provides2O4Vibro-grinding in the supersonically preparation method of nano-particle
The scanning electron microscope (SEM) photograph of the aluminium powder after 2h；Fig. 1 b is high-purity ZnAl that the embodiment of the present invention one provides2O4The ultrasonic preparation of nano-particle
The X-ray diffractogram of aluminium powder after vibro-grinding in method；Fig. 1 c is high-purity ZnAl that the embodiment of the present invention one provides2O4Nanometer
The scanning electron microscope (SEM) photograph of zinc powder after vibro-grinding 13h in the supersonically preparation method of granule；Fig. 1 d is that the embodiment of the present invention one provides
High-purity ZnAl2O4The X-ray diffractogram of zinc powder after vibro-grinding 13h in the supersonically preparation method of nano-particle；
Fig. 2 a is high-purity ZnAl that the embodiment of the present invention one provides2O4γ-Al in the supersonically preparation method of nano-particle2O3
The scanning electron microscope (SEM) photograph of powder；Fig. 2 b is high-purity ZnAl that the embodiment of the present invention one provides2O4In the supersonically preparation method of nano-particle
γ-Al2O3The X-ray diffractogram of powder；Fig. 2 c is high-purity ZnAl that the embodiment of the present invention one provides2O4Nano-particle ultrasonic
The scanning electron microscope (SEM) photograph of Zinc oxide powder in preparation method；Fig. 2 d is high-purity ZnAl that the embodiment of the present invention one provides2O4Nano-particle
Supersonically preparation method in the X-ray diffractogram of Zinc oxide powder；
Fig. 3 is high-purity ZnAl that the embodiment of the present invention one provides2O4γ-Al in the supersonically preparation method of nano-particle2O3With
The thermogravimetric (TG) of zinc oxide mixed sols and difference quotient thermogravimetric (DTG) curve；
Fig. 4 is high-purity ZnAl that the embodiment of the present invention one to embodiment four provides2O4The supersonically preparation method system of nano-particle
The standby ZnAl obtained2O4The X-ray diffractogram of nano-particle；
Fig. 5 is high-purity ZnAl that the embodiment of the present invention one to embodiment four provides2O4The supersonically preparation method system of nano-particle
The standby ZnAl obtained2O4The scanning electron microscope (SEM) photograph of nano-particle.
Detailed description of the invention
The high-purity ZnAl to the present invention below in conjunction with embodiment and accompanying drawing2O4The supersonically preparation method of nano-particle enters
One step explanation.
<embodiment one>
A kind of high-purity ZnAl2O4The supersonically preparation method of nano-particle, comprises the following steps:
Step one, takes the business aluminium powder 100g that purity is 99.5%, evenly laid out at roll-in oscillating mill (power of motor
0.12kW, excited frequency 16Hz, amplitude 5mm) grinding pipe in (volume 2.5L), under the protection of argon after vibro-grinding 2h
To the superfine aluminium power that particle diameter is 0.7 μm；Separately take the business zinc powder 150g that purity is 99%, evenly laid out at roll-in oscillating mill
Grinding pipe in, under the protection of argon, after vibro-grinding 13h, obtain the super-fine zinc dust that particle diameter is 7 μm.
Step 2, takes 5.40g superfine aluminium power and 3.25g super-fine zinc dust is respectively put into two deionized waters equipped with 25ml
Beaker (volume 50ml) mixes with deionized water, two beakers is put in ultrasonic cleaner (supersonic frequency is 22kHz),
Beaker continuous ultrasound 3h containing superfine aluminium power obtains aluminium hydroxide gel liquid solution, the beaker continuous ultrasound containing super-fine zinc dust
24h obtains zinc hydroxide colloid solution.
Step 3, is dried aluminium hydroxide gel liquid solution 6h in the thermostatic drying chamber that temperature is 80 DEG C, obtains after grinding
Aluminium-hydroxide powder；And zinc hydroxide colloid solution is dried in the thermostatic drying chamber that temperature is 80 DEG C 12h, obtain after grinding
Zinc oxide powder.
Step 4, puts into roasting under the conditions of temperature is 300 DEG C in chamber type electric resistance furnace, after insulation 4h by aluminium-hydroxide powder
Grinding obtains γ-Al2O3Powder.
Step 5, weighsPowder and 1.62g Zinc oxide powder, put in the beaker of 50ml together,
Add mix homogeneously after 25ml deionized water, beaker is placed in ultrasonic activation 5h in ultrasonic cleaner, obtains mixed sols.
Step 6, is dried mixed sols 6h in the thermostatic drying chamber of 80 DEG C, obtains after grindingWith oxidation
The mixed-powder of zinc.
Step 7, takes out mixed-powder after 600 DEG C of roasting temperatures, insulation 6h and grinds, obtain ZnAl2O4Nanometer
Grain.
Fig. 1 a is high-purity ZnAl that the embodiment of the present invention one provides2O4Vibro-grinding in the supersonically preparation method of nano-particle
The scanning electron microscope (SEM) photograph of the aluminium powder after 2h；Fig. 1 b is high-purity ZnAl that the embodiment of the present invention one provides2O4The ultrasonic preparation of nano-particle
The X-ray diffractogram of aluminium powder after vibro-grinding in method；Fig. 1 c is high-purity ZnAl that the embodiment of the present invention one provides2O4Nanometer
The scanning electron microscope (SEM) photograph of zinc powder after vibro-grinding 13h in the supersonically preparation method of granule；Fig. 1 d is that the embodiment of the present invention one provides
High-purity ZnAl2O4The X-ray diffractogram of zinc powder after vibro-grinding 13h in the supersonically preparation method of nano-particle.
As shown in Figure 1a, the particle size distribution of the aluminium powder after grinding 2h is in 0.5-0.8 μ m, and the pattern of granule is big
Mostly being short cylindrical, part is irregularly shaped.
As shown in Figure 1 b, after 2h grinds, the crystal structure of aluminium powder is still face-centered cubic lattice, and diffraction peak intensity substantially drops
Low, containing a small amount of aluminium hydroxide composition in product.
As illustrated in figure 1 c, grinding the zinc powder particle size after 13h and be distributed in 5-10 μ m, pattern is spheroidal particle.
As shown in Figure 1 d, comparing with raw material business zinc powder, the chemical composition grinding the zinc powder after 13h does not change, but spreads out
Penetrating peak intensity to be declined slightly, crystal structure is still close-packed hexagonal lattice.
Fig. 2 a is high-purity ZnAl that the embodiment of the present invention one provides2O4γ-Al in the supersonically preparation method of nano-particle2O3
The scanning electron microscope (SEM) photograph of powder；Fig. 2 b is high-purity ZnAl that the embodiment of the present invention one provides2O4In the supersonically preparation method of nano-particle
γ-Al2O3The X-ray diffractogram of powder；Fig. 2 c is high-purity ZnAl that the embodiment of the present invention one provides2O4Nano-particle ultrasonic
The scanning electron microscope (SEM) photograph of Zinc oxide powder in preparation method；Fig. 2 d is high-purity ZnAl that the embodiment of the present invention one provides2O4Nano-particle
Supersonically preparation method in the X-ray diffractogram of Zinc oxide powder.
As shown in Figure 2 a, γ-Al2O3Granule in powder is flake nano structure, without obvious agglomeration, mean diameter
In the range of 30-50nm.
As shown in Figure 2 b, γ-Al2O3The X-ray diffractogram of the granule in powder and γ-Al2O3XRD standard diffraction card
Comparison, diffraction maximum position is identical.
As shown in Figure 2 c, in Zinc oxide powder, granule-morphology is short cylindrical shape, and the average diameter of granule is at 10-20nm model
In enclosing, also without obvious agglomeration.
As shown in Figure 2 d, spread out with zinc oxide standard in the diffraction maximum position of the X-ray diffractogram of the granule in Zinc oxide powder
Penetrate card to fit like a glove.
Fig. 3 is high-purity ZnAl that the embodiment of the present invention one provides2O4γ-Al in the supersonically preparation method of nano-particle2O3With
The thermogravimetric (TG) of zinc oxide mixed sols and difference quotient thermogravimetric (DTG) curve.
As it is shown on figure 3, when heating-up temperature is 50 DEG C, mixed sols has obvious mass change, the matter of about 2%
Amount loss, should be the evaporation of granule contained humidity and is consumed.Within the temperature range of 200-400 DEG C, there are about the weightlessness of 10%, can
Zinc oxide and γ-Al can be because2O3Starting chemical reaction slowly heat release, water of crystallization gasifies rapidly.At 400-800 DEG C
Between, mass loss is gradually reduced, and when temperature rises to 800 DEG C, mass change tends towards stability, along with response time and the increasing of temperature
Adding, solid state reaction is gradually completing, zinc oxide and γ-Al2O3Generate ZnAl2O4。
<embodiment two>
A kind of high-purity ZnAl2O4The supersonically preparation method of nano-particle, comprises the following steps:
Step one, takes the business aluminium powder 100g that purity is 99.5%, evenly laid out at roll-in oscillating mill (power of motor
0.12kW, excited frequency 16Hz, amplitude 5mm) grinding pipe in (volume 2.5L), under the protection of argon after vibro-grinding 1h
To the superfine aluminium power that particle diameter is 0.8 μm；Separately take the business zinc powder 150g that purity is 99%, evenly laid out at roll-in oscillating mill
Grinding pipe in, under the protection of argon, after vibro-grinding 10h, obtain the super-fine zinc dust that particle diameter is 10 μm.
Step 2, takes 5.40g superfine aluminium power and 3.25g super-fine zinc dust is respectively put into two deionized waters equipped with 25ml
Beaker (volume 50ml) mixes with deionized water, two beakers is put in ultrasonic cleaner (supersonic frequency is 22kHz),
Beaker continuous ultrasound 2h containing superfine aluminium power obtains aluminium hydroxide gel liquid solution, the beaker continuous ultrasound containing super-fine zinc dust
18h obtains zinc hydroxide colloid solution.
Step 3, is dried aluminium hydroxide gel liquid solution 6h in the thermostatic drying chamber that temperature is 60 DEG C, obtains after grinding
Aluminium-hydroxide powder；And zinc hydroxide colloid solution is dried in the thermostatic drying chamber that temperature is 60 DEG C 12h, obtain after grinding
Zinc oxide powder.
Step 4, puts into roasting under the conditions of temperature is 250 DEG C in chamber type electric resistance furnace, after insulation 4h by aluminium-hydroxide powder
Grinding obtains γ-Al2O3Powder.
Step 5, weighs 2.04g γ-Al2O3Powder and 1.62g Zinc oxide powder, put into together in the beaker of 50ml, add
Enter mix homogeneously after 25ml deionized water, beaker is placed in ultrasonic activation 3h in ultrasonic cleaner, obtains mixed sols.
Step 6, is dried mixed sols 4h in the thermostatic drying chamber of 60 DEG C, obtains γ-Al after grinding2O3With zinc oxide
Mixed-powder.
Step 7, takes out mixed-powder after 700 DEG C of roasting temperatures, insulation 6h and grinds, obtain ZnAl2O4Nanometer
Grain.
<embodiment three>
A kind of high-purity ZnAl2O4The supersonically preparation method of nano-particle, comprises the following steps:
Step one, takes the business aluminium powder 100g that purity is 99.5%, evenly laid out at roll-in oscillating mill (power of motor
0.12kW, excited frequency 16Hz, amplitude 5mm) grinding pipe in (volume 2.5L), under the protection of argon after vibro-grinding 3h
To the superfine aluminium power that particle diameter is 0.5 μm；Separately take the business zinc powder 150g that purity is 99%, evenly laid out at roll-in oscillating mill
Grinding pipe in, under the protection of argon, after vibro-grinding 15h, obtain the super-fine zinc dust that particle diameter is 5 μm.
Step 2, takes 5.40g superfine aluminium power and 3.25g super-fine zinc dust is respectively put into two deionized waters equipped with 25ml
Beaker (volume 50ml) mixes with deionized water, two beakers is put in ultrasonic cleaner (supersonic frequency is 22kHz),
Beaker continuous ultrasound 4h containing superfine aluminium power obtains aluminium hydroxide gel liquid solution, the beaker continuous ultrasound containing super-fine zinc dust
30h obtains zinc hydroxide colloid solution.
Step 3, is dried aluminium hydroxide gel liquid solution 6h in the thermostatic drying chamber that temperature is 120 DEG C, obtains after grinding
Aluminium-hydroxide powder；And zinc hydroxide colloid solution is dried in the thermostatic drying chamber that temperature is 120 DEG C 12h, after grinding
To Zinc oxide powder.
Step 4, puts into roasting under the conditions of temperature is 350 DEG C in chamber type electric resistance furnace, after insulation 4h by aluminium-hydroxide powder
Grinding obtains γ-Al2O3Powder.
Step 5, weighs 2.04g γ-Al2O3Powder and 1.62g Zinc oxide powder, put into together in the beaker of 50ml, add
Enter mix homogeneously after 25ml deionized water, beaker is placed in ultrasonic activation 8h in ultrasonic cleaner, obtains mixed sols.
Step 6, is dried mixed sols 6h in the thermostatic drying chamber of 120 DEG C, obtains γ-Al after grinding2O3With oxidation
The mixed-powder of zinc.
Step 7, takes out mixed-powder after 800 DEG C of roasting temperatures, insulation 6h and grinds, obtain ZnAl2O4Nanometer
Grain.
<embodiment four>
A kind of high-purity ZnAl2O4The supersonically preparation method of nano-particle, comprises the following steps:
Step one, takes the business aluminium powder 100g that purity is 99.5%, evenly laid out at roll-in oscillating mill (power of motor
0.12kW, excited frequency 16Hz, amplitude 5mm) grinding pipe in (volume 2.5L), under the protection of argon after vibro-grinding 2.5h
Obtain the superfine aluminium power that particle diameter is 0.6 μm；Separately take the business zinc powder 150g that purity is 99%, evenly laid out at roll-in vibro-grinding
In the grinding pipe of machine, under the protection of argon, after vibro-grinding 12h, obtain the super-fine zinc dust that particle diameter is 8 μm.
Step 2, takes 5.40g superfine aluminium power and 3.25g super-fine zinc dust is respectively put into two deionized waters equipped with 25ml
Beaker (volume 50ml) mixes with deionized water, two beakers is put in ultrasonic cleaner (supersonic frequency is 22kHz),
Beaker continuous ultrasound 3h containing superfine aluminium power obtains aluminium hydroxide gel liquid solution, the beaker continuous ultrasound containing super-fine zinc dust
30h obtains zinc hydroxide colloid solution.
Step 3, is dried aluminium hydroxide gel liquid solution 6h in the thermostatic drying chamber that temperature is 100 DEG C, obtains after grinding
Aluminium-hydroxide powder；And zinc hydroxide colloid solution is dried in the thermostatic drying chamber that temperature is 100 DEG C 12h, after grinding
To Zinc oxide powder.
Step 4, puts into roasting under the conditions of temperature is 320 DEG C in chamber type electric resistance furnace, after insulation 4h by aluminium-hydroxide powder
Grinding obtains γ-Al2O3Powder.
Step 5, weighs 2.04g γ-Al2O3Powder and 1.62g Zinc oxide powder, put into together in the beaker of 50ml, add
Enter mix homogeneously after 25ml deionized water, beaker is placed in ultrasonic activation 6h in ultrasonic cleaner, obtains mixed sols.
Step 6, is dried mixed sols 6h in the thermostatic drying chamber of 100 DEG C, obtains γ-Al after grinding2O3With oxidation
The mixed-powder of zinc.
Step 7, takes out mixed-powder after 900 DEG C of roasting temperatures, insulation 6h and grinds, obtain ZnAl2O4Nanometer
Grain.
Fig. 4 is high-purity ZnAl that the embodiment of the present invention one to embodiment four provides2O4The supersonically preparation method system of nano-particle
The standby ZnAl obtained2O4The X-ray diffractogram of nano-particle.
As shown in Figure 4, the ZnAl prepared under different sintering temperatures2O4Nano-particle X-ray diffractogram, ties detection
Fruit compares with standard diffraction card, obtained ZnAl2O4Nano-particle in (220), (311), (422), (511), (440) crystal face
, all there is ZnAl at place2O4Characteristic peak.In identical roasting time, along with sintering temperature increases, the conversion ratio of sample increases therewith,
Degree of crystallinity is become better and better.Being calculated from Scherrer formula, when 800 DEG C, the crystallite dimension of sample is 16.69nm, with 2 θ=36.82 °
(311) calculate.
Fig. 5 is high-purity ZnAl that the embodiment of the present invention one to embodiment four provides2O4The supersonically preparation method system of nano-particle
The standby ZnAl obtained2O4The scanning electron microscope (SEM) photograph of nano-particle.
As it is shown in figure 5, when sintering temperature is 600 DEG C, zinc oxide and γ-Al2O3Reaction be basically completed, pattern is clear
Clear laminated structure, distribution of sizes is in 0.2-0.5 μ m.When being increased to 700-800 DEG C along with temperature, degree of crystallinity progressively carries
Height, particle size is reduced to 40-100nm, and pattern is also changed to column by lamellar.When temperature reaches 900 DEG C, its pattern is post
Body, diameter is about 10nm, and length is about 100nm, has preferable dispersibility.Scanning electron microscope image test result and X-ray
The atlas analysis of diffraction pattern is the most identical.
Embodiment effect and effect
Embodiment one to embodiment four provides a kind of high-purity ZnAl2O4The supersonically preparation method of nano-particle, this preparation side
Method is first by aluminium powder and zinc powder vibro-grinding；Then aluminium powder after grinding and zinc powder carry out that ultrasonic to carry out ultrasonic hydrolysis anti-respectively
Should；Again reacted for ultrasonic hydrolysis aluminium hydroxide gel liquid solution is ground after drying with zinc hydroxide colloid solution, obtain hydrogen-oxygen
Change aluminium powder and Zinc oxide powder；Further aluminium-hydroxide powder roasting is ground and obtain γ-Al2O3Powder, after finally grinding
γ-Al2O3Be dried after powder and Zinc oxide powder 1:1 in molar ratio mixing ultrasonic activation, roasting, grinding obtain high-purity
ZnAl2O4Nano-particle.High-purity ZnAl of embodiment one to embodiment four2O4The supersonically preparation method raw material of nano-particle is easy to get,
Preparation method is simple, it is adaptable to industrialized production, the preparation method of embodiment one to embodiment four ZnAl prepared2O4Nanometer
Particle purity is high, and even particle size distribution, without obvious agglomeration.
Above example is only the basic explanation under present inventive concept, does not limits the invention.And according to the present invention
Any equivalent transformation of being made of technical scheme, belong to protection scope of the present invention.
Claims (8)
1. a high-purity ZnAl2O4The supersonically preparation method of nano-particle, it is characterised in that comprise the following steps:
Step one, grinds aluminium powder and zinc powder certain time under conditions of noble gas respectively, respectively obtains certain particle diameter
Aluminium powder and zinc powder；
After step 2, aluminium powder described after grinding and grinding, described zinc powder is respectively put into two beakers equipped with deionized water
In, and carry out ultrasonic hydrolysis reaction, respectively obtain aluminium hydroxide gel liquid solution and zinc hydroxide colloid solution；
Step 3, by described aluminium hydroxide gel liquid solution and described zinc hydroxide colloid solution under predetermined baking temperature dried
Grind, respectively obtain aluminium-hydroxide powder and Zinc oxide powder；
Step 4, by the roasting under certain sintering temperature of described aluminium-hydroxide powder, grinds after insulation and obtains γ-Al2O3Powder；
Step 5, by described γ-Al2O3Powder and described Zinc oxide powder are 1:1 mix homogeneously in molar ratio, put into equipped with going
After in the beaker of ionized water, ultrasonic activation 3～8h, obtain mixed sols；
Step 6, is dried described mixed sols 4～8h at a temperature of 60～120 DEG C, obtains described γ-Al after grinding2O3With institute
State the mixed-powder of zinc oxide；
Step 7, by the roasting at a predetermined temperature of described mixed-powder, takes out after insulation and grinds, obtain described ZnAl2O4Nanometer
Grain.
The high-purity ZnAl of one the most according to claim 12O4The supersonically preparation method of nano-particle, it is characterised in that:
Wherein, in described step one, described noble gas is argon.
The high-purity ZnAl of one the most according to claim 12O4The supersonically preparation method of nano-particle, it is characterised in that:
Wherein, in described step one, described aluminium powder and described zinc powder grind in roll-in oscillating mill, grinding of described aluminium powder
Time consuming is 1～3h, and the milling time of described zinc powder is 10～15h.
The high-purity ZnAl of one the most according to claim 12O4The supersonically preparation method of nano-particle, it is characterised in that:
Wherein, in described step one, the particle diameter of the described aluminium powder after grinding in 0.5～0.8 μ m, described after grinding
The particle diameter of zinc powder is in the range of 5～10 μm.
The high-purity ZnAl of one the most according to claim 12O4The supersonically preparation method of nano-particle, it is characterised in that:
Wherein, in described step 2, the reaction of described ultrasonic hydrolysis is to carry out in ultrasonic cleaner, described ultrasonic waves for cleaning
The supersonic frequency of device is 22kHz, and the deionized water ultrasonic time containing described aluminium powder is 2～4h, containing described zinc powder go from
Sub-water ultrasonic time is 18～30h.
The high-purity ZnAl of one the most according to claim 12O4The supersonically preparation method of nano-particle, it is characterised in that:
Wherein, in described step 3, described predetermined baking temperature is in the range of 60～120 DEG C.
The high-purity ZnAl of one the most according to claim 12O4The supersonically preparation method of nano-particle, it is characterised in that:
Wherein, in described step 4, the sintering temperature of described aluminium-hydroxide powder is in the range of 250～350 DEG C.
The high-purity ZnAl of one the most according to claim 12O4The supersonically preparation method of nano-particle, it is characterised in that:
Wherein, in described step 7, described predetermined temperature is in the range of 600～900 DEG C.
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| CN115521731A (en) * | 2022-10-11 | 2022-12-27 | 江苏联瑞新材料股份有限公司 | Functional filler with high heat conductivity and low machining abrasiveness and preparation method thereof |
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