CN104528799A - Preparation method of ultrafine magnesium-based rare earth hexaaluminate powder - Google Patents
Preparation method of ultrafine magnesium-based rare earth hexaaluminate powder Download PDFInfo
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- CN104528799A CN104528799A CN201410756682.9A CN201410756682A CN104528799A CN 104528799 A CN104528799 A CN 104528799A CN 201410756682 A CN201410756682 A CN 201410756682A CN 104528799 A CN104528799 A CN 104528799A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
- C01F17/34—Aluminates, e.g. YAlO3 or Y3-xGdxAl5O12
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention relates to a preparation method of ultrafine magnesium-based rare earth hexaaluminate powder, which comprises the following steps: (1) preparation of precursor colloid: a, uniformly mixing an aluminum salt solution, a magnesium salt solution and a rare earth solution in a certain proportion; and b, adding the mixed solution obtained in the step a into ammonium hydroxide, stirring the obtained mixture, keeping the pH value of the obtained mixture not less than 12, and standing for ageing, so that the precursor colloid is obtained; (2) impurity removal: carrying out centrifugal solid-liquid separation on the obtained precursor colloid, washing and concentrating the obtained object, so that wet precursor gel is obtained; (3) drying: drying the wet precursor gel, so that precursor powder is obtained; and (4) heat treatment: calcinating the precursor powder, so that ultrafine magnesium-based rare earth hexaaluminate powder is obtained. The method is low in sintering temperature, the purity of the obtained powder is high, and the obtained powder can achieve nanoscale without being processed, the preparation process is simple, and required equipment is simple, therefore, the method is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of magnesium base rare earth hexa-aluminate superfine powder, belong to ceramic preparation and application field.
Background technology
The magnesium base rare earth hexa-aluminate with six side's magnetoplumbite types is current very important a kind of functional materialss, studied widely in a lot of fields, as: can superconducting material be done, the crystal substrate of fluorescent material, laserable material, also can be used for the aspects such as nuclear waste disposal.Simultaneously because this material has higher thermostability, thus also obtain certain progress as the catalyzer of high temperature catalytic combustion reaction and the applied research of heat barrier coat material in recent years.
The method of current synthesis magnesium base rare earth hexa-aluminate powder mainly contains: high-temperature solid phase reaction method, chemical coprecipitation, sol-gel method, hydrothermal synthesis method, reverse microemulsion process etc.These methods are all used to the preparation of hexa-aluminate, and due to the difference of preparating mechanism and processing condition, the material obtained shows very large difference in surface property, structure and catalytic activity.
Mainly oxide compound, oxyhydroxide or carbonate are as raw material for high-temperature solid phase reaction method, and after Homogeneous phase mixing, namely high-temperature roasting obtains target product.The people such as Li Qilian are with La
2o
3, MgO, Al
2o
3for raw material, after adding binding agent by a certain percentage through ball mill blend together slurry and dry, broken, sieve, prepared LaMgAl finally by spraying agglomeration granulation, high temperature sintering
11o
19powdered material, this method raw material is inexpensive, and technique is simple, but the temperature needed is higher, thus cause the mesophase spherule compound ramp of generation, slow down and continue to be obtained by reacting final composite oxides with other component, and easy-sintering, easily reunites, and size distribution is uneven.Therefore, the usual specific surface area of the powder obtained by high-temperature solid phase reaction method is less, and temperature of reaction is too high, and the reaction times is long, is unfavorable for industrialization promotion, and is mixed with dephasign more, affects the performance of material.
Artizzur Duart etc. adopt sol-gel method to obtain serial BaM through 1200 DEG C of high-temperature roastings
xal
12-xo
19(M is Mn
3+or Fe
3+).Liu Yan etc. adopt the sol-gel method improved to prepare nickel replacement lanthanum hexaaluminate LaAl
11o
19, this method is 1:1:11 according to La/Ni/Al atomic ratio, takes a certain amount of La (NO
3)
36H
2o, Ni (NO
3)
22H
2o and Al (NO
3)
39H
2o is dissolved in distilled water, is then slowly added drop-wise in the polyoxyethylene glycol aqueous isopropanol of heat; Add citric acid and cellulose solution as jelling agent and stablizer, regulator solution pH value, makes colloidal sol at 80 DEG C of heating in water bath, after aging, transfer gel to; 120 DEG C of oven dry, 400 DEG C of roasting 4h, respectively at 1000,1150,1300 DEG C of roasting 5h after fully grinding, obtained nickel replaces lanthanum hexaaluminate LaAl
11o
19.Sol-gel method can realize the Homogeneous phase mixing in each component molecular level, gained hexa-aluminate specific surface area is comparatively large, is the main preparation methods of current hexa-aluminate, but this preparation method's complex process, and organic reagent is used in a large number in preparation process, cost is higher.
Zarur etc. adopt reverse micro emulsion to synthesize bigger serface barium aluminates BaAl in conjunction with Supercritical Drying Technology
12o
19.Similar, Xu Jinguang etc. adopt hydro-thermal-supercritical drying to prepare manganese replacement barium aluminates LaMnAl
11o
19.Stoichiometric lanthanum nitrate, manganous nitrate and aluminum nitrate are dissolved in a certain amount of deionized water by this method, add urea by the amount of per unit positive charge 4mol, stir and make it dissolve, be transferred in autoclave, inflated with nitrogen keeps pressure at 10 ~ 30MPa, is heated to 393 ~ 403K and reacts 2h; Be down to room temperature, with deionized water wash 3 times, then adopt supercritical drying dry.Supercritical drying drying method can obtain the more excellent catalyzer of performance than oven drying, under the condition of supercritical drying, because liquid-gas interface disappears, eliminate wicking action, make formed aerogel remain structure loosely, the Homogeneous phase mixing degree of reactant molecule level can be kept, the sample therefore finally obtained has higher specific surface area, but it is high that the shortcoming of this method is production cost, severe reaction conditions.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that exists for above-mentioned prior art and provides a kind of preparation method of magnesium base rare earth hexa-aluminate superfine powder, firing temperature is low, gained powder purity is high, and does not need to carry out process and can reach nano level, and preparation technology is simple.
The technical scheme that the problem that the present invention is the above-mentioned proposition of solution adopts is:
A preparation method for magnesium base rare earth hexa-aluminate superfine powder, comprises the steps:
(1) presoma colloid preparation:
A, according to rare earth ion Re
3+with Al
3+mol ratio be 1:(100 ~ 10), and Al
3+with Re
3+total mole number and Mg
2+mole ratio is 12:1, aluminum salt solution, magnesium salt solution and earth solution is mixed, obtains solution A;
B, step a gained solution A to be joined in ammoniacal liquor and mix, keep gained mixing solutions pH value to be not less than 12, still aging more than 10h after stirring, prepares presoma colloid;
(2) solid-liquid separation: step (1) gained presoma colloid is separated by centrifugal solid-liquid, and ion, then centrifugal concentrating obtains presoma wet gel;
(3) dry: to obtain presoma powder by after the drying of step (2) gained presoma wet gel;
(4) thermal treatment: by step (3) gained presoma powder calcination, obtains superfine magnesium base rare earth hexa-aluminate powder.
By such scheme, aluminum salt solution described in step a is Al
3+the inorganic salt solution of the aluminium of concentration 0.1 ~ 1.0mol/L.Wherein, the inorganic salt of described aluminium are the aluminum soluble salts such as aluminum nitrate, Tai-Ace S 150, aluminum chloride or its hydrate.
By such scheme, magnesium salt solution described in step a is Mg
2+the inorganic salt solution of the magnesium of concentration 0.1 ~ 1.0mol/L.Wherein, the inorganic salt of described magnesium are the solubility magnesium salts such as magnesium chloride, magnesium nitrate or its hydrate or its alkali formula compound.
By such scheme, earth solution described in step a is rare earth ion Re
3+concentration is the aqueous solution of 0.02 ~ 0.5mol/L.
By such scheme, described rare earth ion Re
3+for La
3+, Nd
3+, Sm
3+, Gd
3+deng.Described earth solution adopts rare earth oxide Re
2o
3be dissolved in dust technology and prepare; Or employing rare-earth salts is water-soluble or prepare in dust technology.Wherein, rare earth oxide Re
2o
3for lanthanum trioxide, Neodymium trioxide, Samarium trioxide, gadolinium sesquioxide etc.; Soluble rare-earth salt is rare earth nitrate, rare earth chloride or its hydrate etc.
By such scheme, the massfraction of ammoniacal liquor described in step b is 5% ~ 25%.
By such scheme, stir described in step b as high-speed stirring or strong stirring, rotating speed is greater than 5000r/min, is beneficial to like this and obtains the less magnesium base rare earth hexa-aluminate product of particle diameter.
By such scheme, temperature dry described in step (3) is 90 ~ 150 DEG C.
By such scheme, described in step (3), the temperature of calcining is 1100 ~ 1600 DEG C, and the time is 1 ~ 6 hour.
Present invention also offers a kind of preferred technical scheme, namely above-mentioned steps (3) operates as follows: step (2) gained presoma wet gel is added centrifugation after absolute ethanol washing; Then add alcohols dispersant evenly after 90 ~ 150 DEG C of dryings, obtain presoma powder.Wherein, the consumption of dehydrated alcohol is 1 ~ 1.5 times of solid masses in presoma wet gel; The consumption of alcohols dispersion agent is 30 ~ 80% of solid masses in presoma wet gel.
By such scheme, described alcohols dispersion agent is one or more mixtures in any proportion in propyl carbinol, n-propyl alcohol, ethylene glycol, isopropylcarbinol.
Compared with prior art, the invention has the beneficial effects as follows:
1, the present invention adopts the method for anti-phase precipitation, and the mixing solutions of aluminum salt solution, magnesium salt solution and earth solution is joined ammoniacal liquor, by controlling the pH in precipitation process, efficiently solves Mg
2+, Al
3+and Re
3+the fractional precipitation problem of ion, thus ensure the precipitation from homogeneous solution of each ion, and significantly reduce the firing temperature (calcining temperature namely during thermal treatment) of magnesium base rare earth hexa-aluminate;
2, in the present invention, solid-liquid separation and pre-treatment are carried out to presoma colloid, ensure that the dispersiveness of powder after drying and thermal treatment, powder after thermal treatment does not need to carry out milled processed can reach nano level, can the purity of effective guarantee product magnesium base rare earth hexa-aluminate and fineness;
3, the present invention prepares magnesium base rare earth hexa-aluminate superfine powder, and except thermal treatment, other technological process is carried out all at normal temperatures, and technique is simple, cost is low, energy consumption is low, is convenient to large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is X-ray powder diffraction (XRD) collection of illustrative plates of magnesium base rare earth hexa-aluminate prepared by embodiment 1.
Fig. 2 is transmission electron microscope (TEM) collection of illustrative plates of magnesium base rare earth hexa-aluminate prepared by embodiment 1.
Fig. 3 is X-ray powder diffraction (XRD) collection of illustrative plates of magnesium base rare earth hexa-aluminate prepared by embodiment 2.
Embodiment
For a better understanding of the present invention, set forth content of the present invention further below by embodiment, but the present invention is not only confined to the following examples.
Stir described in step b as high-speed stirring or strong stirring in following embodiment, rotating speed is all greater than 5000r/min.
Embodiment 1
A preparation method for magnesium base rare earth hexa-aluminate superfine powder, comprises the steps:
(1) presoma colloid preparation:
A, 375g nine water aluminum nitrate is dissolved in the water to be stirred to and dissolves completely, be mixed with 1L aluminum nitrate solution, wherein Al
3+concentration is 1mol/L; 203g magnesium chloride hexahydrate is dissolved in the water to be stirred to and dissolves completely, be mixed with 1L magnesium chloride solution, wherein Mg
2+concentration is 1mol/L; Lanthanum trioxide is dissolved in the dust technology of 5mol/L, is mixed with La
3+concentration is the earth solution of 0.05mol/L;
B, aluminum nitrate solution, magnesium chloride solution and the earth solution prepared by step a mix, and obtain solution A, La in gained solution A
3+with Al
3+mol ratio be 1:11, Al
3+with La
3+total mole number and Mg
2+mole ratio is 12:1;
C, step b gained solution A is joined massfraction is mix in 20% ammoniacal liquor and stir, and obtain mixing solutions, mixing solutions pH value is 12; Then still aging 12h, prepares presoma colloid;
(2) solid-liquid separation: step (1) gained presoma colloid is separated by centrifugal solid-liquid, wash 6 removal of impurity, then centrifugal concentrating obtains presoma wet gel;
(3) Gel Pre process is with dry: step (2) gained presoma wet gel is added dehydrated alcohol, and centrifugation after dispersion, repeats 3 times; Then add propyl carbinol, 110 DEG C of dryings after being uniformly dispersed, obtain presoma powder; Wherein, the consumption of dehydrated alcohol is 1 times of solid masses in presoma wet gel, and the consumption of propyl carbinol is 50% of solid masses in presoma wet gel;
(4) thermal treatment: by step (3) gained presoma powder 1350 DEG C of thermal treatments 3 hours, obtains superfine magnesium base lanthanum hexaaluminate powder.
As shown in Figure 1, superfine magnesium base hexa-aluminate powder prepared by the present embodiment is single magnesium base lanthanum hexaaluminate crystalline phase, magnetoplumbite type, and particle diameter is 10-50nm; As shown in Figure 2, superfine magnesium base hexa-aluminate powder size uniform prepared by the present embodiment, narrow particle size distribution, regular appearance.
Embodiment 2
A preparation method for magnesium base rare earth hexa-aluminate superfine powder, comprises the steps:
(1) presoma colloid preparation:
A, 187.5g nine water aluminum nitrate is dissolved in the water to be stirred to and dissolves completely, be mixed with 1L aluminum nitrate solution, wherein Al
3+concentration is 0.5mol/L; 101.5g magnesium chloride hexahydrate is dissolved in the water to be stirred to and dissolves completely, be mixed with 1L magnesium chloride solution, wherein Mg
2+concentration is 0.5mol/L; Neodymium trioxide is dissolved in dust technology, is mixed with Nd
3+concentration is the earth solution of 0.1mol/L;
B, aluminum nitrate solution, magnesium chloride solution and the earth solution prepared by step a mix, and obtain solution A, Nd in gained solution A
3+with Al
3+mol ratio be 1:50, Al
3+with Nd
3+total mole number and Mg
2+mole ratio is 12:1;
C, step b gained solution A to be joined massfraction be in 25% ammoniacal liquor and high-speed stirring is even, and obtain mixing solutions, mixing solutions pH value is 12, then still aging 18h, prepares presoma colloid;
(2) solid-liquid separation: step (1) gained presoma colloid is separated by centrifugal solid-liquid, wash 5 removal of impurity, then centrifugal concentrating obtains presoma wet gel;
(3) Gel Pre process is with dry: step (2) gained presoma wet gel is added dehydrated alcohol, and centrifugation after dispersion, repeats 3 times; Then add n-propyl alcohol, 120 DEG C of dryings after being uniformly dispersed, obtain presoma powder; Wherein, the consumption of dehydrated alcohol is 1.2 times of solid masses in presoma wet gel, and the consumption of n-propyl alcohol is 80% of solid masses in presoma wet gel;
(4) thermal treatment: by step (3) gained presoma powder 1350 DEG C of thermal treatments 2 hours, obtains superfine magnesium base six aluminic acid neodymium powder.
As shown in Figure 3, superfine magnesium base six aluminic acid neodymium powder prepared by the present embodiment is single magnesium base six aluminic acid neodymium crystalline phase, and magnetoplumbite type, diameter of particle is 25-60nm.
Embodiment 3
A preparation method for magnesium base rare earth hexa-aluminate superfine powder, comprises the steps:
(1) presoma colloid preparation:
A, 96.4g Aluminum Chloride Hexahydrate is dissolved in the water to be stirred to and dissolves completely, be mixed with 1L liquor alumini chloridi, wherein Al
3+concentration is 0.4mol/L; 81.2g magnesium chloride hexahydrate is dissolved in the water to be stirred to and dissolves completely, be mixed with 1L magnesium chloride solution, wherein Mg
2+concentration is 0.4mol/L; Samarium trioxide is dissolved in dust technology, is mixed with Sm
3+concentration is the earth solution of 0.2mol/L;
B, liquor alumini chloridi, magnesium chloride solution and the earth solution prepared by step a mix, and obtain solution A, Sm in gained solution A
3+with Al
3+mol ratio be 1:100, Al
3+with Sm
3+total mole number and Mg
2+mole ratio is 12:1;
C, step b gained solution A to be joined massfraction be in 5% ammoniacal liquor and high-speed stirring is even, and obtain mixing solutions, mixing solutions pH value is 13, then still aging 24h, prepares presoma colloid;
(2) solid-liquid separation: step (1) gained presoma colloid is separated by centrifugal solid-liquid, wash 4 removal of impurity, then centrifugal concentrating obtains presoma wet gel;
(3) Gel Pre process is with dry: step (2) gained presoma wet gel is added dehydrated alcohol, and centrifugation after dispersion, repeats 2 times; Then add ethylene glycol, 130 DEG C of dryings after being uniformly dispersed, obtain presoma powder; Wherein, the consumption of dehydrated alcohol is 1.5 times of solid masses in presoma wet gel, and the consumption of ethylene glycol is 30% of solid masses in presoma wet gel;
(4) thermal treatment: by step (3) gained presoma powder 1200 DEG C of thermal treatments 4 hours, obtains superfine magnesium base six samarium aluminate powder.
Embodiment 4
A preparation method for magnesium base rare earth hexa-aluminate superfine powder, comprises the steps:
(1) presoma colloid preparation:
A, 342g Tai-Ace S 150 is dissolved in the water to be stirred to and dissolves completely, be mixed with 1L alum liquor, wherein Al
3+concentration is 1mol/L; 256g magnesium nitrate hexahydrate is dissolved in the water to be stirred to and dissolves completely, be mixed with 1L magnesium nitrate solution, wherein Mg
2+concentration is 1mol/L; Gadolinium sesquioxide is dissolved in dust technology, is mixed with Gd
3+concentration is the earth solution of 0.02mol/L;
B, alum liquor, magnesium nitrate solution and the earth solution prepared by step a mix, and obtain solution A, Gd in gained solution A
3+with Al
3+mol ratio be 1:10, Al
3+with Gd
3+total mole number and Mg
2+mole ratio is 12:1;
C, step b gained solution A to be joined massfraction be in 25% ammoniacal liquor and high-speed stirring is even, and obtain mixing solutions, mixing solutions pH value is 13, then still aging 12h, prepares presoma colloid;
(2) removal of impurity: be separated by centrifugal solid-liquid by step (1) gained presoma colloid, washes 3 removal of impurity, then centrifugally obtains presoma wet gel;
(3) Gel Pre process is with dry: step (2) gained presoma wet gel is added dehydrated alcohol, and centrifugation after dispersion, repeats 2 times; Then add isopropylcarbinol, 150 DEG C of dryings after being uniformly dispersed, obtain presoma powder; Wherein, the consumption of dehydrated alcohol is 1.3 times of solid masses in presoma wet gel, and the consumption of isopropylcarbinol is 35% of solid masses in presoma wet gel;
(4) thermal treatment: by step (3) gained presoma powder 1450 DEG C of thermal treatments 6 hours, obtains superfine magnesium base six aluminic acid gadolinium powder.
Embodiment 5
A preparation method for magnesium base rare earth hexa-aluminate superfine powder, comprises the steps:
(1) presoma colloid preparation:
A, 96.4g Aluminum Chloride Hexahydrate is stirred in dissolved water and dissolves completely, be mixed with 1L liquor alumini chloridi, wherein Al
3+concentration is 0.4mol/L; 123g magnesium sulfate heptahydrate is dissolved in the water to be stirred to and dissolves completely, be mixed with 1L Adlerika, wherein Mg
2+concentration is 0.5mol/L; Lanthanum trioxide is dissolved in dust technology, is mixed with La
3+concentration is the earth solution of 0.4mol/L;
B, liquor alumini chloridi, Adlerika and the earth solution prepared by step a mix, and obtain solution A, La in gained solution A
3+with Al
3+mol ratio be 1:10, Al
3+with La
3+total mole number and Mg
2+mole ratio is 12:1;
C, step b gained solution A to be joined massfraction be in 15% ammoniacal liquor and high-speed stirring is even, and obtain mixing solutions, mixing solutions pH value is 12, then still aging 12h, prepares presoma colloid;
(2) solid-liquid separation: be separated by centrifugal solid-liquid by step (1) gained presoma colloid, ion matter, then centrifugally obtains presoma wet gel;
(3) Gel Pre process is with dry: step (2) gained presoma wet gel is added dehydrated alcohol, and centrifugation after dispersion, repeats 3 times; Then add isopropylcarbinol and propyl carbinol mixed solution (both mass ratioes are 1:1), 150 DEG C of dryings after being uniformly dispersed, obtain presoma powder; Wherein, the consumption of dehydrated alcohol is 1 times of solid masses in presoma wet gel, and the consumption of isopropylcarbinol and propyl carbinol mixed solution is 60% of solid masses in presoma wet gel;
(4) thermal treatment: by step (3) gained presoma powder 1200 DEG C of thermal treatments 5.5 hours, obtains superfine magnesium base lanthanum hexaaluminate powder.
Embodiment 6
A preparation method for magnesium base rare earth hexa-aluminate superfine powder, comprises the steps:
(1) presoma colloid preparation:
A, 192.8g Aluminum Chloride Hexahydrate is dissolved in the water to be stirred to and dissolves completely, be mixed with 1L liquor alumini chloridi, wherein Al
3+concentration is 0.8mol/L; 81.2g magnesium chloride hexahydrate is dissolved in the water to be stirred to and dissolves completely, be mixed with 1L magnesium chloride brine, wherein Mg
2+concentration is 0.4mol/L; Samarium trioxide is dissolved in dust technology, is mixed with Sm
3+concentration is the earth solution of 0.08mol/L;
B, liquor alumini chloridi, magnesium chloride solution and the earth solution prepared by step a mix, and obtain solution A, Sm in gained solution A
3+with Al
3+mol ratio be 1:11, Al
3+with Sm
3+total mole number and Mg
2+mole ratio is 12:1;
C, step b gained solution A to be joined massfraction be in 25% ammoniacal liquor and high-speed stirring is even, and obtain mixing solutions, mixing solutions pH value is 12, then still aging 12h, prepares presoma colloid;
(2) solid-liquid separation: be separated by centrifugal solid-liquid by step (1) gained presoma colloid, ion matter, is then concentrated and obtains presoma wet gel;
(3) dry: to obtain presoma powder by after the drying of step (2) gained presoma wet gel;
(4) thermal treatment: by step (3) gained presoma powder 1350 DEG C of thermal treatments 5.5 hours, obtains superfine magnesium base six samarium aluminate powder.
Above-described embodiment, all can prepare corresponding magnesium base rare earth hexa-aluminate superfine powder, and purity is high, is magnetoplumbite type, the equal 10 ~ 500nm of particle diameter, size uniform, narrow particle size distribution, regular appearance; In addition, gained magnesium base rare earth hexa-aluminate dispersion of ultrafine powder of the present invention is good, does not need to carry out milled processed and can reach nano level, can form the colloidal sol of stable homogeneous in water and alcohol.
Certainly, those skilled in the art can by regulating each processing parameter, prepare magnesium base rare earth hexa-aluminate superfine powder, such as by stirring velocity in regulating step b, control the particle size range of products therefrom magnesium base rare earth hexa-aluminate superfine powder, the time of ageing can also be changed, control the growth of crystal grain in ageing process, etc., like this, when can not depart from technical conceive of the present invention, various change and distortion are carried out to the present invention.
The above is only the preferred embodiment of the present invention, it should be pointed out that for the person of ordinary skill of the art, and without departing from the concept of the premise of the invention, can also make some improvement and conversion, these all belong to protection scope of the present invention.
Claims (10)
1. a preparation method for magnesium base rare earth hexa-aluminate superfine powder, is characterized in that it comprises the steps:
(1) presoma colloid preparation:
A, according to rare earth ion Re
3+with Al
3+mol ratio be 1:(100 ~ 10), and Al
3+with Re
3+total mole number and Mg
2+mole ratio is 12:1, aluminum salt solution, magnesium salt solution and earth solution is mixed, obtains solution A;
B, step a gained solution A to be joined in ammoniacal liquor and mix, keep gained mixing solutions pH value to be not less than 12, still aging more than 10h after stirring, prepares presoma colloid;
(2) solid-liquid separation: be separated by centrifugal solid-liquid by step (1) gained presoma colloid, ion, then centrifugal concentrating obtains presoma wet gel;
(3) dry: to obtain presoma powder by after the drying of step (2) gained presoma wet gel;
(4) thermal treatment: after step (3) gained presoma powder calcination, obtains superfine magnesium base rare earth hexa-aluminate powder.
2. a preparation method for magnesium base rare earth hexa-aluminate superfine powder, is characterized in that it comprises the steps:
(1) presoma colloid preparation:
A, according to rare earth ion Re
3+with Al
3+mol ratio be 1:(100 ~ 10), and Al
3+with Re
3+total mole number and Mg
2+mole ratio is 12:1, aluminum salt solution, magnesium salt solution and earth solution is mixed, obtains solution A; ;
B, step a gained solution A joined in ammoniacal liquor mix, keep gained mixing solutions pH value to be not less than 12, stir still aging more than 10h all, prepare presoma colloid;
(2) solid-liquid separation: be separated by centrifugal solid-liquid by step (1) gained presoma colloid, ion, then centrifugal concentrating obtains presoma wet gel;
(3) Gel Pre process is with dry: step (2) gained presoma wet gel is added centrifugation after absolute ethanol washing; Then add alcohols dispersant evenly rear dry, obtain presoma powder;
(4) thermal treatment: after step (3) gained presoma powder calcination, obtains superfine magnesium base rare earth hexa-aluminate powder.
3. according to claim 1 and 2. a kind of preparation method of magnesium base rare earth hexa-aluminate superfine powder, is characterized in that aluminum salt solution described in step a is Al
3+the inorganic salt solution of the aluminium of concentration 0.1 ~ 1.0mol/L.
4. according to claim 1 and 2. a kind of preparation method of magnesium base rare earth hexa-aluminate superfine powder, is characterized in that magnesium salt solution described in step a is Mg
2+the inorganic salt solution of the magnesium of concentration 0.1 ~ 1.0mol/L.
5. according to claim 1 and 2. a kind of preparation method of magnesium base rare earth hexa-aluminate superfine powder, is characterized in that earth solution described in step a is rare earth ion Re
3+concentration is the aqueous solution of 0.02 ~ 0.5mol/L.
6. according to claim 1 and 2. a kind of preparation method of magnesium base rare earth hexa-aluminate superfine powder, is characterized in that described earth solution adopts rare earth oxide Re
2o
3be dissolved in dust technology and prepare; Or employing rare-earth salts is water-soluble or prepare in dust technology.
7. according to claim 1 and 2. a kind of preparation method of magnesium base rare earth hexa-aluminate superfine powder, is characterized in that the massfraction of ammoniacal liquor described in step b is 5% ~ 25%.
8. according to claim 1 and 2. a kind of preparation method of magnesium base rare earth hexa-aluminate superfine powder, is characterized in that temperature dry described in step (3) is 90 ~ 150 DEG C.
9. according to claim 1 and 2. a kind of preparation method of magnesium base rare earth hexa-aluminate superfine powder, it is characterized in that the temperature of calcining described in step (3) is 1100 ~ 1600 DEG C, the time is 1 ~ 6 hour.
10. according to claim 2. a kind of preparation method of magnesium base rare earth hexa-aluminate superfine powder, is characterized in that described alcohols dispersion agent is one or more mixtures in any proportion in propyl carbinol, n-propyl alcohol, ethylene glycol, isopropylcarbinol.
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