CN102874878B - Manganese acid yttrium nano powder preparation method according to microwave-hydrothermal method - Google Patents

Manganese acid yttrium nano powder preparation method according to microwave-hydrothermal method Download PDF

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CN102874878B
CN102874878B CN201210344646.2A CN201210344646A CN102874878B CN 102874878 B CN102874878 B CN 102874878B CN 201210344646 A CN201210344646 A CN 201210344646A CN 102874878 B CN102874878 B CN 102874878B
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hydrothermal
powder
acid yttrium
solution
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CN102874878A (en
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蒲永平
刘丹
石轩
罗玥玥
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JIANGSU SUR LIGHTING CO LTD
Shenzhen Pengbo Information Technology Co ltd
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Shaanxi University of Science and Technology
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Abstract

The invention provides a manganese acid yttrium nano powder preparation method according to a microwave-hydrothermal method. The preparation method comprises the following steps: using yttrium nitrate, potassium permanganate and manganese nitrate as the precursor, and dissolving the materials into deionized water according to that the molar ratio of Y and Mn is 1:(0.8 to 1.25) and the molar ratio of the Mn<7+> and Mn<2+> is 1:(3 to 4); then dripping sodium hydroxide into solution and adjusting pH to 14 to form uniform precursor solution; pouring the precursor solution into a hydrothermal reaction still and sealing the hydrothermal reaction still; putting the hydrothermal reaction still into a microwave digestion system for microwave-hydrothermal synthesis; cooling to room temperature; washing the generated materials with deionized water and absolute ethyl alcohol for a plurality of times; and calcining the washed materials at 800 to 1100 DEG C to obtain manganese acid yttrium nano powder. The preparation method provided by the invention prepares manganese acid yttrium nano powder according to the microwave-hydrothermal method, so that not only the preparation cost is low, the operation is simple, the reaction period is short, but also the generated material after calcinations is high in purity, the development of crystalline grains is complete and the distribution of the crystalline grains is uniform.

Description

A kind of microwave-hydrothermal method is prepared the method for mangaic acid yttrium nano-powder
Technical field
The present invention relates to a kind of preparation method of nano-powder, particularly a kind of microwave-hydrothermal method is prepared the method for mangaic acid yttrium nano-powder.
Background technology
YMn 2o 5a kind of typical single-phase multi-ferroic material, the ferroelectric transformation Curie temperature T of its crystal c≈ 20K, and antiferromagnetic transition temperature T n≈ 45K.In recent years, YMn 2o 5also cause researchist's attention as a kind of novel visible light catalyst.
As everyone knows, the physical properties of material and their pattern, dimension, size and defect etc. are closely related, and especially, under nanoscale, photocatalyst can show the photocatalytic activity of enhancing.The method of preparing nano material is a lot, and wherein microwave-hydrothermal method is that traditional hydrothermal synthesis method and microwave field are combined, and expectation can embody the uniqueness of microwave and the advantage of hydrothermal method itself, is a kind of novel method with huge applications potentiality.The distinguishing feature of microwave hydrothermal is the reaction times can be reduced greatly, temperature of reaction also declines to some extent, thereby can carry out formation and the growth of nucleus with lower temperature and shorter time in water-heat process, the reduction of temperature of reaction and time, limit further growing up of product microcrystallite, be conducive to prepare superfine powdery material.This has directive significance for preparing nano level photocatalysis powder.
At present, bibliographical information is prepared YMn 2o 5the method of crystal mainly contains three kinds, and a kind of is traditional solid sintering technology, and the method is first by high-purity initial feed Y 2o 3, Mn 3o 4after powder mixes, be incubated two hours and carry out drying treatment at 500 ℃ of temperature, then within two hours, carry out presintering in 900 ℃ of insulations, finally sintering 16h under the air of 1000-1400 ℃ respectively, obtains YMn 2o 5ceramics sample.Find by research, in the time of 1100 ℃, made the YMn of orthohormbic structure 2o 5pottery, and in the time of 1400 ℃, be transformed into the YMn of hexagonal structure 2o 5pottery.Another kind of conventional preparation YMn 2o 5method be flux method, by the manganous nitrate of certain mol proportion and Y 2o 3mixture melting in solvent, dissolve reach saturated after with the transpiration cooling of solvent, reach after supersaturation YMn 2o 5crystal is separated out thereupon.Also there is people to prepare YMn by hydrothermal synthesis method 2o 5powder, this method adopts Y (NO 3) 36H 2o, Mn (NO 3) 2and KMnO 4for starting material, by the processing of various processing condition, prepare YMn 2o 5powder, although synthesized YMn 2o 5crystal, but its crystallinity is bad, and there is certain adhesion agglomeration.
Summary of the invention
The object of the present invention is to provide a kind of microwave-hydrothermal method to prepare the method for mangaic acid yttrium nano-powder, to solve YMn 2o 5crystal structure is bad, and the problem that exists certain adhesion to reunite.
For achieving the above object, the present invention adopts following technical scheme:
Microwave-hydrothermal method is prepared a method for mangaic acid yttrium nano-powder, comprises the following steps:
Step 1: get Yttrium trinitrate homogeneous solution A, potassium permanganate homogeneous solution B and manganese nitrate solution C;
Step 2: according to Y/Mn mol ratio 1:(0.8-1.5), Mn 7+: Mn 2+mol ratio 1:(3-4) solution B and C are joined in solution A, add deionized water and stirring even, be adjusted to alkalescence, form uniform Co-precipitation Precursor D;
Step 3: Co-precipitation Precursor D is poured in microwave hydrothermal reaction kettle, and sealed reaction, after having reacted, is cooled to room temperature;
Step 4: the material water taking out in reactor rinses to neutrality, calcines and obtain the mangaic acid yttrium nano-powder of needle-like.
The present invention further improves and is: in step 2, solution B and C are joined in solution A, then add deionized water and stirring even, the concentration that makes Yttrium trinitrate is 0.0625mol/L.
The present invention further improves and is: the pH while being adjusted to alkalescence in described step 2 is 14.
The present invention further improves and is: the compactedness of step 3 hydrothermal reaction kettle is 40%.
The present invention further improves and is: in described step 3, in microwave hydrothermal reaction kettle, the step of sealed reaction is: first at 100 ℃ of insulation 5min, then at 125 ℃ of insulation 5min, then at 150 ℃ of insulation 10min, again at 175 ℃ of insulation 15min, finally at 200 ℃ of insulation 30min.
The present invention further improves and is: the calcining temperature of described step 4 is 800 ~ 1100 ℃.
The present invention further improves and is: the concentration of the homogeneous solution of Yttrium trinitrate described in step 1 is 0.1mol/L; The concentration of described potassium permanganate homogeneous solution is 0.1mol/L; Described manganese nitrate solution is 50% manganese nitrate solution.
The present invention further improves and is: in step 2, Y/Mn mol ratio is 1:1-1.5.
The present invention further improves and is: in step 2, Y/Mn mol ratio is 1:1.5.
The present invention further improves and is: in step 2, and Mn 7+: Mn 2+mol ratio is 1:4.
With respect to prior art, the method that microwave-hydrothermal method of the present invention is prepared mangaic acid yttrium nano-powder at least has the following advantages: the present invention adopts microwave-hydrothermal method to prepare mangaic acid yttrium nano-powder; Due to microwave reaction, to have speed fast, and without advantages such as thermogrades, not only preparation cost is low, simple to operate, reaction time is short, product purity is high, crystal grain is grown complete and is evenly distributed.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of the different Y/Mn mol ratio mangaic acid yttrium nano-powders prepared by the present invention;
Fig. 2 is X-ray diffraction (XRD) figure of the mangaic acid yttrium nano-powder prepared by the embodiment of the present invention 3;
Fig. 3 is that the SEM of the mangaic acid yttrium nano-powder prepared by the embodiment of the present invention 3 schemes.
Embodiment
Embodiment 1:
In the precursor liquid of the mangaic acid yttrium nano-powder of preparing in the present embodiment, Y/Mn mol ratio is: 1:1, Mn 7+: Mn 2+mol ratio is: 1:3.
Step 1: getting concentration is the Yttrium trinitrate homogeneous solution A of 0.1mol/L, the potassium permanganate homogeneous solution B that concentration is 0.1mol/L and 50% manganese nitrate solution C;
Step 2: be according to Y/Mn mol ratio: 1:1, Mn 7+: Mn 2+mol ratio is: 1:3; Solution B and C are joined in solution A, add deionized water and stirring even, the concentration that makes Yttrium trinitrate is 0.0625mol/L; Then being adjusted to pH is 14, forms uniform Co-precipitation Precursor D;
Step 3: Co-precipitation Precursor D is poured in microwave hydrothermal reaction kettle, and controlling compactedness is 40%, sealed reaction, first at 100 ℃ of insulation 5min, then at 125 ℃ of insulation 5min, then at 150 ℃ of insulation 10min, again at 175 ℃ of insulation 15min, finally at 200 ℃ of insulation 30min.After having reacted, be cooled to room temperature;
Step 4: the material water taking out in reactor rinses to neutrality, and 1100 ℃ of calcinings obtain the mangaic acid yttrium nano-powder of needle-like.
Embodiment 2:
In the precursor liquid of the mangaic acid yttrium nano-powder of preparing in the present embodiment, Y/Mn mol ratio is: 1:1, Mn 7+: Mn 2+mol ratio is: 1:4.
Step 1: getting concentration is the Yttrium trinitrate homogeneous solution A of 0.1mol/L, the potassium permanganate homogeneous solution B that concentration is 0.1mol/L and 50% manganese nitrate solution C;
Step 2: be according to Y/Mn mol ratio: 1:1, Mn 7+: Mn 2+mol ratio is: 1:4 joins solution B and C in solution A, adds deionized water and stirring even, and the concentration that makes Yttrium trinitrate is 0.0625mol/L; Then being adjusted to pH is 14, forms uniform Co-precipitation Precursor D;
Step 3: Co-precipitation Precursor D is poured in microwave hydrothermal reaction kettle, and controlling compactedness is 40%, sealed reaction, first at 100 ℃ of insulation 5min, then at 125 ℃ of insulation 5min, then at 150 ℃ of insulation 10min, again at 175 ℃ of insulation 15min, finally at 200 ℃ of insulation 30min.After having reacted, be cooled to room temperature;
Step 4: the material water taking out in reactor rinses to neutrality, and 1100 ℃ of calcinings obtain the mangaic acid yttrium nano-powder of needle-like.
Embodiment 3:
In the precursor liquid of the mangaic acid yttrium nano-powder of preparing in the present embodiment, Y/Mn mol ratio is: 1:1.5, Mn 7+: Mn 2+mol ratio is: 1:4.
Step 1: getting concentration is the Yttrium trinitrate homogeneous solution A of 0.1mol/L, the potassium permanganate homogeneous solution B that concentration is 0.1mol/L and 50% manganese nitrate solution C;
Step 2: be according to Y/Mn mol ratio: 1:1.5, Mn 7+: Mn 2+mol ratio is: 1:4 joins solution B and C in solution A, adds deionized water and stirring even, and the concentration that makes Yttrium trinitrate is 0.0625mol/L; Then being adjusted to pH is 14, forms uniform Co-precipitation Precursor D;
Step 3: Co-precipitation Precursor D is poured in microwave hydrothermal reaction kettle, and controlling compactedness is 40%, sealed reaction, first at 100 ℃ of insulation 5min, then at 125 ℃ of insulation 5min, then at 150 ℃ of insulation 10min, again at 175 ℃ of insulation 15min, finally at 200 ℃ of insulation 30min.After having reacted, be cooled to room temperature;
Step 4: the material water taking out in reactor rinses to neutrality, and 1100 ℃ of calcinings obtain the mangaic acid yttrium nano-powder of needle-like.
Embodiment 4:
In the precursor liquid of the mangaic acid yttrium nano-powder of preparing in the present embodiment, Y/Mn mol ratio is: 1:0.8, Mn 7+: Mn 2+mol ratio is: 1:4.
Step 1: getting concentration is the Yttrium trinitrate homogeneous solution A of 0.1mol/L, the potassium permanganate homogeneous solution B that concentration is 0.1mol/L and 50% manganese nitrate solution C;
Step 2: be according to Y/Mn mol ratio: 1:0.8, Mn 7+: Mn 2+mol ratio is: 1:4 joins solution B and C in solution A, adds deionized water and stirring even, and the concentration that makes Yttrium trinitrate is 0.0625mol/L; Then being adjusted to pH is 14, forms uniform Co-precipitation Precursor D;
Step 3: Co-precipitation Precursor D is poured in microwave hydrothermal reaction kettle, and controlling compactedness is 40%, sealed reaction, first at 100 ℃ of insulation 5min, then at 125 ℃ of insulation 5min, then at 150 ℃ of insulation 10min, again at 175 ℃ of insulation 15min, finally at 200 ℃ of insulation 30min.After having reacted, be cooled to room temperature;
Step 4: the material water taking out in reactor rinses to neutrality, and 800 ℃ of calcinings obtain the mangaic acid yttrium nano-powder of needle-like.
Refer to shown in Fig. 1, the mangaic acid yttrium nano-powder of the different Y/Mn mol ratios that prepared by the inventive method, in the time that Y/Mn is 1:1, is conducive to Y (OH) 3the formation of phase, and in the time that reactant concn is relatively high, the crystal property of sample is better; In the time that Y is excessive, be also unfavorable for the formation of mangaic acid yttrium; In the time that Mn content is relatively high, contribute to the formation of mangaic acid yttrium, especially YMn 2o 5phase.Therefore embodiment 3 is preference of the present invention.Refer to shown in Fig. 2, the mangaic acid yttrium nano-powder crystallinity after 1100 ℃ of calcinings is good, refer to shown in Fig. 3, and the mangaic acid yttrium nano-powder being prepared by the inventive method, surface is regular needle-like, and particle is grown complete, and component is even.
The foregoing is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of any equivalence that the logical technician in this area takes technical solution of the present invention by reading specification sheets of the present invention, is claim of the present invention and contains.

Claims (7)

1. microwave-hydrothermal method is prepared a method for mangaic acid yttrium nano-powder, it is characterized in that: comprise the following steps:
Step 1: get Yttrium trinitrate homogeneous solution A, potassium permanganate homogeneous solution B and manganese nitrate solution C;
Step 2: according to Y/Mn mol ratio 1:(0.8-1.5), Mn 7+: Mn 2+mol ratio 1:(3-4) solution B and C are joined in solution A, add deionized water and stirring even, regulating pH is 14, forms uniform Co-precipitation Precursor D;
Step 3: Co-precipitation Precursor D is poured in microwave hydrothermal reaction kettle, and sealed reaction, after having reacted, is cooled to room temperature;
Step 4: the material water taking out in reactor rinses to neutrality, calcines and obtain the mangaic acid yttrium nano-powder of needle-like;
In step 2, solution B and C are joined in solution A, then add deionized water and stirring even, the concentration that makes Yttrium trinitrate is 0.0625mol/L;
The compactedness of step 3 hydrothermal reaction kettle is 40%.
2. microwave-hydrothermal method as claimed in claim 1 is prepared the method for mangaic acid yttrium nano-powder, it is characterized in that: in described step 3, in microwave hydrothermal reaction kettle, the step of sealed reaction is: first at 100 ℃ of insulation 5min, then at 125 ℃ of insulation 5min, then at 150 ℃ of insulation 10min, again at 175 ℃ of insulation 15min, finally at 200 ℃ of insulation 30min.
3. microwave-hydrothermal method as claimed in claim 1 is prepared the method for mangaic acid yttrium nano-powder, it is characterized in that: the calcining temperature of described step 4 is 800～1100 ℃.
4. microwave-hydrothermal method as claimed in claim 1 is prepared the method for mangaic acid yttrium nano-powder, it is characterized in that: the concentration of the homogeneous solution of Yttrium trinitrate described in step 1 is 0.1mol/L; The concentration of described potassium permanganate homogeneous solution is 0.1mol/L; Described manganese nitrate solution is 50% manganese nitrate solution.
5. microwave-hydrothermal method as claimed in claim 1 is prepared the method for mangaic acid yttrium nano-powder, it is characterized in that: in step 2, Y/Mn mol ratio is 1:1-1.5.
6. microwave-hydrothermal method as claimed in claim 1 is prepared the method for mangaic acid yttrium nano-powder, it is characterized in that: in step 2, Y/Mn mol ratio is 1:1.5.
7. the microwave-hydrothermal method as described in claim 1,5 or 6 is prepared the method for mangaic acid yttrium nano-powder, it is characterized in that: in step 2, and Mn 7+: Mn 2+mol ratio is 1:4.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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CN102079543A (en) * 2011-02-24 2011-06-01 西北工业大学 Preparation method of hexagonal manganese acid yttrium nanofiber

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101310898A (en) * 2007-05-22 2008-11-26 中国科学院宁波材料技术与工程研究所 Solid-oxide fuel battery cathode powder preparation method
CN102079543A (en) * 2011-02-24 2011-06-01 西北工业大学 Preparation method of hexagonal manganese acid yttrium nanofiber

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