CN106242548A - A kind of high-purity MgAl2o4the supersonically preparation method of nano-particle - Google Patents

A kind of high-purity MgAl2o4the supersonically preparation method of nano-particle Download PDF

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CN106242548A
CN106242548A CN201610624925.2A CN201610624925A CN106242548A CN 106242548 A CN106242548 A CN 106242548A CN 201610624925 A CN201610624925 A CN 201610624925A CN 106242548 A CN106242548 A CN 106242548A
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徐波
王骏
李生娟
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University of Shanghai for Science and Technology
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
    • C04B35/443—Magnesium aluminate spinel
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/624—Sol-gel processing
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/95—Products characterised by their size, e.g. microceramics

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Abstract

The invention provides a kind of high-purity MgAl2O4The supersonically preparation method of nano-particle, comprises the following steps: step one, is ground by aluminium powder；Step 2, carries out ultrasonic hydrolysis reaction respectively by the aluminium powder after magnesium powder and grinding, respectively obtains magnesium hydroxide colloidal solution and aluminium hydroxide gel liquid solution；Step 3, is dried magnesium hydroxide colloidal solution and aluminium hydroxide gel liquid solution, respectively obtains magnesium hydroxide xerogel and dried aluminum hydroxide gel；Step 4, grinds magnesium hydroxide xerogel and dried aluminum hydroxide gel, respectively obtains magnesium hydroxide powder and aluminium-hydroxide powder；Step 5, mixes magnesium hydroxide powder and aluminium-hydroxide powder, ultrasonic activation, obtains mixed sols；Step 6, by mixed sols roasting, obtains high-purity MgAl after grinding2O4Nano-particle.High-purity MgAl of the present invention2O4The supersonically preparation method raw material of nano-particle is easy to get, it is adaptable to industrialized production, the preparation method of the present invention MgAl prepared2O4Nano-particle purity is high, and even particle size distribution, without obvious agglomeration.

Description

A kind of high-purity MgAl2O4The supersonically preparation method of nano-particle
Technical field
The present invention relates to the technology of preparing of a kind of nano material, be specifically related to a kind of high-purity MgAl2O4Nano-particle ultrasonic Preparation method.
Background technology
Magnesium aluminate spinel (MgAl2O4) it is the important mixed-metal oxides of a class, non-metal inorganic material occupies pole Its consequence.The transparent polycrystalline ceramics material prepared by magnesium aluminate spinel nano granule, not only have fabulous high temperature resistant, Corrosion-resistant, wear-resistant, shock resistance, high rigidity, high intensity, good electrical insulation capability and less linear expansion coefficient, and have Sapphire crystal, the optical property of quartz glass, have good transmitance at ultraviolet light, visible ray and infrared band.Magnalium Spinel ceramic material, can be used for manufacturing guided missile head-shield, the insulation framework of transparent electron components and parts, the window material of infrared band Material, alloy and the ceramic protecting film of metallic article, refractory material, fine ceramics vessel, optical fiber and Fibre Optical Sensor material, also may be used As projection TV luminescence substrate.Obtain high-purity, ultra-fine, uniform, chemical composition is controlled and the monocrystalline magnalium of low-temperature sintering Spinel nano granule is significant.
At present, it is developed many methods and prepares MgAl2O4Nano-particle, including coprecipitation, sol-gel Method, polymer-network gel process, polymerization sequestration thing method and high-energy ball milling method, every kind of method is respectively arranged with advantage, but also has the part of deficiency.
Chinese invention patent (Publication No. CN102936022A) discloses the conjunction of a kind of High purity nano-scale magnesium-aluminum spinel One-tenth method, the light calcined magnesia of nanocrystalline level and boehmite are pressed MgO and Al by this synthetic method2O3Mol ratio 1:1 dispensing mixing Uniformly, ball milling, drying and moulding, obtain base substrate print；By 500 DEG C of pre-burning 1h of base substrate print, then it is warmed up to 850-1500 DEG C of insulation 2-3h, is cooled to room temperature, obtains High purity nano-scale magnesium-aluminum spinel.Although the magnesium aluminate spinel purity that the method obtains is high, contracting Short temperature retention time, but, this method is higher to ingredient requirement, and calcined temperature and sintering temperature higher, energy consumption is relatively big, Requirement to equipment is the highest.
Summary of the invention
The present invention is carried out for solving the problems referred to above, it is therefore intended that providing a kind of raw material to be easy to get, sintering temperature is the lowest High-purity MgAl in existing preparation method2O4The 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 MgAl2O4The supersonically preparation method of nano-particle, has the feature that, including Following steps:
Step one, grinds aluminium powder 1～3h under conditions of noble gas, obtains the aluminium powder of certain particle size；
Step 2, magnesium powder and the aluminium powder after grinding are respectively put into two equipped with in the beaker of deionized water, and surpass Sound hydrolysis 1～5h, respectively obtains magnesium hydroxide colloidal solution and aluminium hydroxide gel liquid solution；
Step 3, is dried 4～8h by magnesium hydroxide colloidal solution and aluminium hydroxide gel liquid solution under predetermined baking temperature After, respectively obtain magnesium hydroxide xerogel and dried aluminum hydroxide gel；
Step 4, grinds magnesium hydroxide xerogel and dried aluminum hydroxide gel, respectively obtains magnesium hydroxide powder and hydrogen Alumina powder；
Step 5, is 1:2 mix homogeneously by magnesium hydroxide powder and aluminium-hydroxide powder in molar ratio, put into equipped with go from After in the beaker of sub-water, ultrasonic activation 3～8h, obtain mixed sols；
Step 6, by mixed sols roasting 2～6h under predetermined sintering temperature, obtains high-purity MgAl after grinding2O4Nanometer Grain.
At high-purity MgAl 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 MgAl 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 grinds in roll-in oscillating mill.
At high-purity MgAl 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, after grinding, the particle diameter of aluminium powder is in the range of 0.5～0.8 μm.
At high-purity MgAl 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, and ultrasonic cleaner supersonic frequency is 40kHz。
At high-purity MgAl 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 60～120 DEG C.
At high-purity MgAl 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 6, predetermined sintering temperature is 400～500 DEG C.
Invention effect and effect
The invention provides a kind of high-purity MgAl2O4The supersonically preparation method of nano-particle, aluminium powder is first ground by this preparation method Mill；Then the aluminium powder after magnesium powder and grinding is carried out ultrasonic hydrolysis reaction respectively；Again by reacted for ultrasonic hydrolysis magnesium hydroxide Colloid solution is dried with aluminium hydroxide gel liquid solution；Further the magnesium hydroxide xerogel obtained after drying is done with aluminium hydroxide Gel abrasive；Magnesium hydroxide powder after finally grinding mixes with aluminium-hydroxide powder 1:2 in molar ratio, and ultrasonic activation is laggard Row roasting, grinding obtain high-purity MgAl2O4Nano-particle.High-purity MgAl of the present invention2O4The supersonically preparation method of nano-particle is former Material is easy to get, and preparation method is simple, it is adaptable to industrialized production, the preparation method of the present invention MgAl prepared2O4Nano-particle is pure Degree height, even particle size distribution, without obvious agglomeration.
Accompanying drawing explanation
Fig. 1 a is high-purity MgAl that the embodiment of the present invention one provides2O4Vibro-grinding in the supersonically preparation method of nano-particle After the transmission electron microscope picture of aluminium powder；Fig. 1 b is high-purity MgAl that the embodiment of the present invention one provides2O4The ultrasonic preparation side of nano-particle The high resolution TEM figure of aluminium powder after vibro-grinding in method；Fig. 1 c is high-purity MgAl that the embodiment of the present invention one provides2O4 The X-ray diffractogram of aluminium powder after business aluminium powder and vibro-grinding 2h in the supersonically preparation method of nano-particle；
Fig. 2 a is high-purity MgAl that the embodiment of the present invention one provides2O4Magnesium hydroxide in the supersonically preparation method of nano-particle The X-ray diffractogram of granule；Fig. 2 b is high-purity MgAl that the embodiment of the present invention one provides2O4The supersonically preparation method of nano-particle The X-ray diffractogram of middle aluminum hydroxide particles；
Fig. 3 a is high-purity MgAl that the embodiment of the present invention one provides2O4Magnesium hydroxide in the supersonically preparation method of nano-particle The scanning electron microscope (SEM) photograph of granule；Fig. 3 b is high-purity MgAl that the embodiment of the present invention one provides2O4In the supersonically preparation method of nano-particle The scanning electron microscope (SEM) photograph of aluminum hydroxide particles；
Fig. 4 a is high-purity MgAl that the embodiment of the present invention one provides2O4Aluminium hydroxide in the supersonically preparation method of nano-particle X-ray diffractogram with magnesium hydroxide mixed sols；Fig. 4 b is high-purity MgAl that the embodiment of the present invention one provides2O4Nano-particle Supersonically preparation method in the transmission electron microscope picture of aluminium hydroxide and magnesium hydroxide mixed sols；
Fig. 5 is high-purity MgAl that the embodiment of the present invention one provides2O4In the supersonically preparation method of nano-particle aluminium hydroxide with The thermogravimetric (TG) of magnesium hydroxide mixed sols and differential thermal (DSC) curve；
Fig. 6 a is high-purity MgAl that the embodiment of the present invention one provides2O4The supersonically preparation method of nano-particle prepares MgAl2O4The X-ray diffractogram of nano-particle；Fig. 6 b is high-purity MgAl that the embodiment of the present invention one provides2O4Surpassing of nano-particle The MgAl that sound preparation method prepares2O4The scanning electron microscope (SEM) photograph of nano-particle.
Detailed description of the invention
The high-purity MgAl 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 MgAl2O4The supersonically preparation method of nano-particle, comprises the following steps:
Step one, take 100g granularity be 300 μm business aluminium powders be placed in roll-in oscillating mill (power of motor 0.12kW, swash Vibration frequency 16Hz, amplitude 5mm) mill tube (volume 2.5L) in, vibro-grinding 2h under the protection of argon, obtaining granularity is 0.7 μ The aluminium powder of m.
Step 2, takes the aluminium powder after 2g business magnesium powder and 2g vibro-grinding and is respectively put into two equipped with 50ml deionized water In beaker (volume 100ml), two beakers are put in ultrasonic cleaner (supersonic frequency is 40kHz), carry out ultrasonic hydrolysis Reaction 3h, in the localized hyperthermia that ultrasonic cavitation produces, environment under high pressure, generates magnesium hydroxide particle and aluminium hydroxide respectively Grain, magnesium hydroxide particle and aluminum hydroxide particles form magnesium hydroxide colloidal solution and aluminium hydroxide gel liquid solution in the solution.
Step 3, takes magnesium hydroxide colloidal solution and aluminium hydroxide gel liquid solution and is dried 6h under the baking temperature of 80 DEG C After, respectively obtain magnesium hydroxide xerogel and dried aluminum hydroxide gel.
Step 4, takes magnesium hydroxide xerogel and dried aluminum hydroxide gel grinds, and respectively obtains magnesium hydroxide white powder With aluminium hydroxide white powder.
Step 5, takes 1.16g magnesium hydroxide white powder and 3.12g aluminium hydroxide white powder (mol ratio is 1:2), mixed After closing uniformly, put in the beaker equipped with 30ml deionized water (volume is 100ml), beaker is placed in ultrasonic cleaning tank ultrasonic Activation 5h, obtains mixture of white colloidal sol.
Step 6, is placed in mixture of white colloidal sol in chamber type electric resistance furnace and roasts under conditions of predetermined sintering temperature is 450 DEG C Burn 4h, after grinding, obtain high-purity MgAl2O4Nano-particle.
Fig. 1 a is high-purity MgAl that the embodiment of the present invention one provides2O4Vibro-grinding in the supersonically preparation method of nano-particle After the transmission electron microscope picture of aluminium powder；Fig. 1 b is high-purity MgAl that the embodiment of the present invention one provides2O4The ultrasonic preparation side of nano-particle The high resolution TEM figure of aluminium powder after vibro-grinding in method；Fig. 1 c is high-purity MgAl that the embodiment of the present invention one provides2O4 The X-ray diffractogram of aluminium powder after business aluminium powder and vibro-grinding 2h in the supersonically preparation method of nano-particle.
As shown in Fig. 1 a, 1b, after grinding 2h, the particle size distribution of aluminium powder is in 0.5～0.8 μ m, deposits inside granule At substantial amounts of dislocation defects, be conducive to mechano-chemical reation.
As illustrated in figure 1 c, business aluminium powder is after 2h grinds, and crystal structure does not change, and is still face-centered cubic lattice, But the aluminium powder after Yan Moing occurs in that a small amount of aluminium hydroxide.
Fig. 2 a is high-purity MgAl that the embodiment of the present invention one provides2O4Magnesium hydroxide in the supersonically preparation method of nano-particle The X-ray diffractogram of granule；Fig. 2 b is high-purity MgAl that the embodiment of the present invention one provides2O4The supersonically preparation method of nano-particle The X-ray diffractogram of middle aluminum hydroxide particles.
As shown in Fig. 2 a, 2b, magnesium hydroxide particle prepared by the ultrasonic hydrolysis of Fig. 2 a, 2b and the X of aluminum hydroxide particles Ray diffraction diagram, compares with X-ray standard diffraction card, the diffraction maximum position of magnesium hydroxide particle and aluminum hydroxide particles and hydrogen respectively Magnesium oxide and aluminium hydroxide standard diffraction card data fit like a glove, and hydrolysis prods is high purity magnesium hydroxide granule and aluminium hydroxide Grain, does not has other material to produce in course of reaction.
Fig. 3 a is high-purity MgAl that the embodiment of the present invention one provides2O4Magnesium hydroxide in the supersonically preparation method of nano-particle The scanning electron microscope (SEM) photograph of granule, Fig. 3 b is high-purity MgAl that the embodiment of the present invention one provides2O4In the supersonically preparation method of nano-particle The scanning electron microscope (SEM) photograph of aluminum hydroxide particles.
As shown in Figure 3 a, the pattern of magnesium hydroxide particle is disc-shaped, and diameter is about 100nm, and thickness is at about 5nm.
As shown in Figure 3 b, aluminum hydroxide particles is bladed structure, and distribution of lengths is in the range of 80-100nm, and thickness is about 5nm。
Fig. 4 a is high-purity MgAl that the embodiment of the present invention one provides2O4Aluminium hydroxide in the supersonically preparation method of nano-particle X-ray diffractogram with magnesium hydroxide mixed sols；Fig. 4 b is high-purity MgAl that the embodiment of the present invention one provides2O4Nano-particle Supersonically preparation method in the transmission electron microscope picture of aluminium hydroxide and magnesium hydroxide mixed sols.
As shown in fig. 4 a, after mixture ultrasonic activation 5h, the chemical composition of sample has occurred and that change, with X-ray mark Quasi-diffraction card compares, and essential element is MgAl2(OH)8And MgAl2(OH)7 +。
As shown in Figure 4 b, during ultrasonic activation, aluminium hydroxide and magnesium hydroxide mixture have formed colloidal sol, and size exists Between 50-500nm, particle size distribution is uneven, and pattern is irregular.
Fig. 5 is high-purity MgAl that the embodiment of the present invention one provides2O4In the supersonically preparation method of nano-particle aluminium hydroxide with The thermogravimetric (TG) of magnesium hydroxide mixed sols and differential thermal (DSC) curve.
As shown in Figure 5, it can be seen that when heating-up temperature is between 50 DEG C and 200 DEG C, aluminium hydroxide and the matter of magnesium hydroxide Amount loss is about 20%, and this is mainly due to the physical absorption water on aluminium hydroxide and magnesium hydroxide surface and a small amount of moisture of residual Volatilization causes.Between 200 DEG C and 450 DEG C, mass loss is about 17%, and corresponding DSC curve has respectively at 280.3 DEG C One bigger endothermic peak, is that mixed sols dehydration is transformed into γ-Al2O3And MgO, and the endothermic peak of 387.4 DEG C, then be γ- Al2O3Start reaction with MgO generate amorphous magnesia-alumina spinel structure and be gradually converted into caused by crystalline state spinelle.When temperature liter After 450 DEG C, chemical reaction tends towards stability, and mass loss is gradually reduced, and crystal grain starts to grow up.Select 450 DEG C as roasting Temperature, obtains high-purity MgAl after Muffle kiln roasting 4h2O4Nano-particle, owing to the homogenization degree of sample is higher, reaction temperature Degree is substantially reduced, and the response time shortens, and its reaction equation is: MgAl2(OH)8+MgAl2(OH)7 ++ OH=2MgAl2O4+ 8H2O。
Fig. 6 a is high-purity MgAl that the embodiment of the present invention one provides2O4The supersonically preparation method of nano-particle prepares MgAl2O4The X-ray diffractogram of nano-particle；Fig. 6 b is high-purity MgAl that the embodiment of the present invention one provides2O4Surpassing of nano-particle The MgAl that sound preparation method prepares2O4The scanning electron microscope (SEM) photograph of nano-particle.
As shown in Figure 6 a, it can be seen that aluminium hydroxide and the crystal structure of magnesium hydroxide mixed sols are that magnalium is sharp from Fig. 6 a Spinel structure, contrasts with X-ray standard diffraction card, and diffraction maximum position fits like a glove.
As shown in Figure 6 b, the pattern of the SEM image display granule of Fig. 6 b is lamellar, and length is at about 100nm, and thickness is about For 5nm, even particle size distribution, without obvious agglomeration, product is still amorphous spinel structure.
<embodiment two>
A kind of high-purity MgAl2O4The supersonically preparation method of nano-particle, comprises the following steps:
Step one, taking 100g granularity is that 10 μm business aluminium powders are placed in roll-in oscillating mill (power of motor 0.12kW, exciting Frequency 16Hz, amplitude 5mm) mill tube in, vibro-grinding 1h under the protection of argon, obtain the aluminium powder that granularity is 0.8 μm.
Step 2, takes the aluminium powder after 2g business magnesium powder and 2g vibro-grinding and is respectively put into two equipped with 50ml deionized water In beaker (volume 100ml), two beakers are put in ultrasonic cleaner (supersonic frequency is 40kHz), carry out ultrasonic hydrolysis Reaction 1h, in the localized hyperthermia that ultrasonic cavitation produces, environment under high pressure, generates magnesium hydroxide particle and aluminium hydroxide respectively Grain, magnesium hydroxide particle and aluminum hydroxide particles form magnesium hydroxide colloidal solution and aluminium hydroxide gel liquid solution in the solution.
Step 3, takes magnesium hydroxide colloidal solution and aluminium hydroxide gel liquid solution and is dried 4h under the baking temperature of 60 DEG C After, respectively obtain magnesium hydroxide xerogel and dried aluminum hydroxide gel.
Step 4, takes magnesium hydroxide xerogel and dried aluminum hydroxide gel grinds, and respectively obtains magnesium hydroxide white powder With aluminium hydroxide white powder.
Step 5, takes 1.16g magnesium hydroxide white powder and 3.12g aluminium hydroxide white powder (mol ratio is 1:2), mixed After closing uniformly, put in the beaker equipped with 30ml deionized water (volume is 100ml), beaker is placed in ultrasonic cleaning tank ultrasonic Activation 3h, obtains mixture of white colloidal sol.
Step 6, is placed in mixture of white colloidal sol in chamber type electric resistance furnace and roasts under conditions of predetermined sintering temperature is 400 DEG C Burn 2h, after grinding, obtain high-purity MgAl2O4Nano-particle.
<embodiment three>
A kind of high-purity MgAl2O4The supersonically preparation method of nano-particle, comprises the following steps:
Step one, take 100g granularity be 100 μm business aluminium powders be placed in roll-in oscillating mill (power of motor 0.12kW, swash Vibration frequency 16Hz, amplitude 5mm) mill tube (volume 2.5L) in, vibro-grinding 3h under the protection of argon, obtaining granularity is 0.5 μ The aluminium powder of m.
Step 2, takes the aluminium powder after 2g business magnesium powder and 2g vibro-grinding and is respectively put into two equipped with 50ml deionized water In beaker (volume 100ml), two beakers are put in ultrasonic cleaner (supersonic frequency is 40kHz), carry out ultrasonic hydrolysis Reaction 5h, in the localized hyperthermia that ultrasonic cavitation produces, environment under high pressure, generates magnesium hydroxide solid particle and aluminium hydroxide respectively Granule, magnesium hydroxide particle forms magnesium hydroxide colloidal solution in the solution with aluminum hydroxide particles and alumine hydroxide colloid is molten Liquid.
Step 3, takes magnesium hydroxide colloidal solution and aluminium hydroxide gel liquid solution and is dried 8h under the baking temperature of 120 DEG C After, respectively obtain magnesium hydroxide xerogel and dried aluminum hydroxide gel.
Step 4, takes magnesium hydroxide xerogel and dried aluminum hydroxide gel grinds, and respectively obtains magnesium hydroxide white powder With aluminium hydroxide white powder.
Step 5, takes 1.16g magnesium hydroxide white powder and 3.12g aluminium hydroxide white powder (mol ratio is 1:2), mixed After closing uniformly, put in the beaker equipped with 30ml deionized water (volume is 100ml), beaker is placed in ultrasonic cleaning tank ultrasonic Activation 8h, obtains mixture of white colloidal sol.
Step 6, is placed in mixture of white colloidal sol in chamber type electric resistance furnace and roasts under conditions of predetermined sintering temperature is 500 DEG C Burn 6h, after grinding, obtain high-purity MgAl2O4Nano-particle.
Embodiment effect and effect
Embodiment one to embodiment three provides a kind of high-purity MgAl2O4The supersonically preparation method of nano-particle, this preparation side Method is first by aluminium powder vibro-grinding under the conditions of argon；Then the aluminium powder obtained after magnesium powder and vibro-grinding is carried out ultrasonic water respectively Solve reaction；Again reacted for ultrasonic hydrolysis magnesium hydroxide colloidal solution is dried with aluminium hydroxide gel liquid solution；Further to dry The magnesium hydroxide xerogel obtained after dry grinds with dried aluminum hydroxide gel；Magnesium hydroxide powder after finally grinding and hydrogen-oxygen Change aluminium powder 1:2 in molar ratio mixing, carry out after ultrasonic activation roasting, grind obtain high-purity MgAl2O4Nano-particle.Embodiment High-purity MgAl of one to embodiment three2O4The supersonically preparation method raw material of nano-particle is easy to get, and preparation method is simple, it is adaptable to work Industry metaplasia is produced, the preparation method of the present invention MgAl prepared2O4Nano-particle purity is high, even particle size distribution, without substantially reuniting Phenomenon.
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 (7)

1. a high-purity MgAl2O4The supersonically preparation method of nano-particle, it is characterised in that comprise the following steps:
Step one, grinds aluminium powder 1～3h under conditions of noble gas, obtains the aluminium powder of certain particle size；
Step 2, by magnesium powder and after grinding described aluminium powder be respectively put into two equipped with in the beaker of deionized water, and surpass Sound hydrolysis 1～5h, respectively obtains magnesium hydroxide colloidal solution and aluminium hydroxide gel liquid solution；
Step 3, is dried 4 by described magnesium hydroxide colloidal solution and described aluminium hydroxide gel liquid solution under predetermined baking temperature ～after 8h, respectively obtain magnesium hydroxide xerogel and dried aluminum hydroxide gel；
Step 4, grinds described magnesium hydroxide xerogel and described dried aluminum hydroxide gel, respectively obtains magnesium hydroxide powder And aluminium-hydroxide powder；
Step 5, is 1:2 mix homogeneously by described magnesium hydroxide powder and described aluminium-hydroxide powder in molar ratio, put into equipped with After in the beaker of deionized water, ultrasonic activation 3～8h, obtain mixed sols；
Step 6, by described mixed sols roasting 2～6h under predetermined sintering temperature, obtains described high-purity MgAl after grinding2O4Receive Rice grain.
The high-purity MgAl 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 MgAl 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 grinds in roll-in oscillating mill.
The high-purity MgAl of one the most according to claim 12O4The supersonically preparation method of nano-particle, it is characterised in that:
Wherein, in described step one, after grinding, the particle diameter of described aluminium powder is in the range of 0.5～0.8 μm.
The high-purity MgAl 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 Groove supersonic frequency is 40kHz.
The high-purity MgAl 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 60～120 DEG C.
The high-purity MgAl of one the most according to claim 12O4The supersonically preparation method of nano-particle, it is characterised in that:
Wherein, in described step 6, described predetermined sintering temperature is 400～500 DEG C.
CN201610624925.2A 2016-08-02 2016-08-02 A kind of high-purity MgAl2o4the supersonically preparation method of nano-particle Pending CN106242548A (en)

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CN102107910A (en) * 2011-03-23 2011-06-29 上海理工大学 Preparation method of nano magnesium ferrite
CN103420428A (en) * 2012-09-28 2013-12-04 上海理工大学 Preparation method of magnesium ferrite nano-particles

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102107910A (en) * 2011-03-23 2011-06-29 上海理工大学 Preparation method of nano magnesium ferrite
CN103420428A (en) * 2012-09-28 2013-12-04 上海理工大学 Preparation method of magnesium ferrite nano-particles

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