CN104973615A - Microwave burning preparation method of nano gadolinium oxide powder - Google Patents
Microwave burning preparation method of nano gadolinium oxide powder Download PDFInfo
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- CN104973615A CN104973615A CN201510364481.9A CN201510364481A CN104973615A CN 104973615 A CN104973615 A CN 104973615A CN 201510364481 A CN201510364481 A CN 201510364481A CN 104973615 A CN104973615 A CN 104973615A
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Abstract
The invention relates to a microwave burning preparation method of nano gadolinium oxide powder. The preparation method comprises the following steps: (1) mixing gadolinium oxide powder with a nitric acid solution to prepare a gadolinium nitrate solution; (2) evenly mixing the gadolinium nitrate solution with a critic acid solution according to a mole ratio of Gd3+ to citric acid of 4:(1-2) to obtain a precursor solution; (3) adjusting the pH value of the precursor solution to 8-10; (4) burning the precursor solution with an adjusted pH value by microwaves to obtain white powder; (5) burning the white powder for 2 to 5 hours at a constant temperature of 450 to 800 DEG C; (6) ball-grinding the burned white powder, and drying to obtain the target product. The preparation method adopts a microwave burning synthesis method, the microwave energy is utilized to vibrate the inner molecules in the precursor so as to generate heat, and the heat energy is evenly distributed.
Description
(1) technical field
The present invention relates to a kind of nanoscale gadolinium raw powder's production technology, belong to field of material preparation.
(2) background technology
The preparation of nano-ceramic powder is the matter of utmost importance of nano ceramic material nanometer material industry relevant with other, and main preparation methods has solid phase method, liquid phase method and vapor phase process.Since the nineties in 20th century, nano-ceramic powder enters the stage of industrialization.Current China mainly adopts wet chemistry method and vapour deposition process to carry out the preparation of industrialized nano ceramic powder, and main products comprises CaCO
3, ZnO, Al
2o
3, SiO
x, TiO
2, Si
3n
4with SiC etc.
Nano oxidized gadolinium powder can be used for various fluorescent material, the neutron absorber material in reactor, magnetic bubble material, intensifying screen material.In opticglass, electronic industry etc., also there is certain application, also can be used as gadolinium gallium garnet material.
For the synthesis of nano oxidized gadolinium powder, commonplace method is used to be sol-gel method, chemical precipitation method at present." syntheses and properties of the micro-nano gadolinium sesquioxide matrix material of electrically conductive polyaniline " Lixia ZHANG etc., Guangxi Teachers College's journal (natural science edition), 2007,66-68, adopt chemical precipitation method to prepare the gadolinium sesquioxide flaky powder of micro/nano level, but the powder prepared easily is reunited, adopt ethanol as dispersion agent, dispersion effect is more effective than polyoxyethylene glycol, but the gadolinium sesquioxide size obtained is comparatively large, at about 50 ~ 800nm; Adopt polyoxyethylene glycol as dispersion agent, dispersion effect is slightly poorer than ethanol, and gadolinium sesquioxide size is less, but still at about 200nm." preparation of nano oxidized gadolinium/NBR matrix material and shielding properties research thereof " Zhao Yongfeng etc., rubber industry, 2010,581-585, adopt coprecipitation method and spray-drying process to combine and prepare nanoscale gadolinium through high-temperature calcination, but preparation process duration comparatively speaking, technique is relatively loaded down with trivial details.
(3) summary of the invention
For the deficiencies in the prior art, the shortcoming that especially gadolinium sesquioxide powder synthesis cost is higher, the invention provides a kind of method of microwave burning synthesis of nano gadolinium sesquioxide powder.
Technical scheme of the present invention is as follows:
A microwave burning preparation method for nano oxidized gadolinium powder, comprises step as follows:
(1) Gadolinium trinitrate solution is configured: mixed with salpeter solution by gadolinium sesquioxide powder, obtained Gadolinium trinitrate solution; Described gadolinium sesquioxide: the mol ratio of nitric acid is 1:(5-9);
(2) Gadolinium trinitrate solution mixes with citric acid: by Gadolinium trinitrate solution and citric acid solution by Gd
3+: citric acid mol ratio is 4:(1-2) mix, obtained precursor solution;
(3) adjust ph: the pH value of precursor solution is adjusted to 8 ~ 10;
(4) microwave burning synthesis: by the precursor solution microwave burning synthesis after adjust ph, obtained white powder;
(5) calcine: by white powder 450 DEG C ~ 800 DEG C insulation calcining 2-5h in retort furnace;
(6) ball milling: by the material ball milling after calcining, dry, i.e. obtained nano oxidized gadolinium powder.
According to the present invention, preferably, gadolinium sesquioxide described in step (1): the mol ratio of nitric acid is 1:(6-7), preferred further, the concentration of described salpeter solution is 30-40wt%, and salpeter solution usable concentration is that the concentrated nitric acid deionized water dilution of 65 ~ 69wt% obtains.
According to the present invention, preferably, the citric acid described in step (2) is monohydrate potassium (C
6h
8o
7h
2o), Gd
3+: C
6h
8o
7h
2the mol ratio of O is 4:(1-1.5).
According to the present invention, preferably, pH is regulated with ammoniacal liquor in step (3).
According to the present invention, preferably, described in step (4), the equipment of microwave burning is microwave oven.Moisture evaporate to dryness in precursor solution in microwave burning process, solute reacts.The temperature of microwave oven is set to middle temperature or middle high temperature, and the reaction times is 40min ~ 60min, reaction times visual response thing amount and determining, and after moisture evaporate to dryness, pulverulent product changes white powder into by yellow is cellular.
According to the present invention, preferably, in step (5), the equipment of calcining is retort furnace, and retort furnace calcining heat-up rate is 5 ~ 10 DEG C/min; Preferred further, described calcining temperature is 500 DEG C ~ 800 DEG C.By further calcining, make C unnecessary in powder, N element voloxidation, thus purification powder, meanwhile make the further crystallization of powder obtain more full die.
According to the present invention, preferably, in step (6), ball milling adopts wet ball grinding, and wet ball grinding adopts ethanol to be dispersion medium, and employing polyvinylpyrrolidone is dispersion agent.
Principle of the present invention:
The present invention uses nitric acid, gadolinium sesquioxide, citric acid, ammoniacal liquor etc. as raw material, household microwave oven can be used as Reaktionsofen, adopt the precursor solution of chemical method synthesis of nano gadolinium sesquioxide, afterwards precursor solution is placed in household microwave oven to burn, combustion time is depending on precursor solution volume, by moisture evaporate to dryness in precursor solution, solute reacts.After conbustion synthesis, powder dissolve with ethanol is added polyvinylpyrrolidone as dispersion agent, lapping using star lapping machine, dried by batch mixing, be nano oxidized gadolinium powder after grinding, particle diameter is at 50 ~ 100nm.
The present invention adopts microwave combusion method, and microwave has certain katalysis to chemical reaction; The heat transfer theory of microwave heating is different from traditional heat transfer theory and HEAT TRANSFER LAW, and microwave has certain penetration to material, and be that the molecule inhaling ripple material produces the direct heat release of thermal vibration by energy supply material, therefore, heated material is heated very even; Microwave energy supply does not bring any secondary pollution because of thermal source or exothermic material into heated material.Add citric acid in precursor power of the present invention and participate in reaction, make full use of the superiority of organic-inorganic material hybridization reaction, citric acid can ionize out 3 H as a kind of stronger organic acid
+, can with Gd in Gadolinium trinitrate solution
3+hydridization, utilizes the skeleton construction of citric acid molecule herein, and make to vibrate heat production in microwave burning process more even, powder granule is not easily reunited, and does not bring the difficult impurity element removed into simultaneously.In addition for promoting that reaction is carried out use ammoniacal liquor and promoted that reaction is carried out as catalyzer, visualize is adjust ph.For promoting powder crystallization, crystal grain thinning to a certain extent, finds trim point between the easy cluster of nano-powder and the too high grain growth of calcining temperature, determines calcining temperature at 450 DEG C ~ 800 DEG C for best after the present invention probes into.The elements such as C, N in calcination process in powder can voloxidation make nano oxidized gadolinium powder be purified.
(4) beneficial effect:
(1) the present invention adopts microwave combustion synthesizing method, utilizes microwave energy, makes presoma vibrate heat production by interior molecules, uniform heat distribution.
(2) the present invention adopt organism citric acid participate in reaction, with Gadolinium trinitrate generation organic inorganic hybridization, as a kind of stronger organic acid, 1mol citric acid ionizable go out 3molH
+, Gd under ionic linkage effect
3+h can be replaced
+, thus using citric acid as medium, form organic inorganic hybrid.
(3) the nano oxidized gadolinium diameter of particle of the present invention's synthesis is between 50 ~ 100nm, and the powder granularity prepared relative to additive method is less and be uniformly dispersed.
(5) accompanying drawing explanation
Fig. 1 is the SEM figure of the low enlargement ratio of gadolinium sesquioxide powder that the embodiment of the present invention 1 obtains;
Fig. 2 is the SEM figure of the gadolinium sesquioxide powder high magnification that the embodiment of the present invention 1 obtains;
Fig. 3 is the XRD figure of the gadolinium sesquioxide powder that the embodiment of the present invention 1 obtains.
(6) embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described further, but institute of the present invention protection domain is not limited thereto.
Raw materials usedly in embodiment be convenient source, commercial products.
Embodiment 1:
A microwave burning preparation method for nano oxidized gadolinium powder, comprises step as follows:
(1) Gd (NO is configured
3)
3solution: take 20g micron order gadolinium sesquioxide powder, is diluted to 35wt%, Gd in molar ratio by massfraction 69% concentrated nitric acid 31.2g 28.2g deionized water
2o
3: HNO
3=1:6, configuration Gd (NO
3)
3solution, is placed in 500ml beaker and dissolves in magnetic stirrer, ultrasonic disperse 5min by solution;
(2) Gadolinium trinitrate solution mixes with citric acid: take 92.4g monohydrate potassium and be dissolved in 150ml water, Gd in molar ratio
3+: C
6h
8o
7h
2o=4:1 configures precursor solution, is placed in 50 DEG C of constant temperature water baths, magnetic agitation 10min;
(3) adjust ph: dripping ammoniacal liquor adjust ph in precursor solution is 8;
(4) microwave burning synthesis: precursor solution is placed in household microwave oven conbustion synthesis, use moderate heat, the time is about 30min, and goods change white powder into by yellow is cellular;
(5) retort furnace calcining: white powder is placed in retort furnace, is warming up to 500 DEG C in 50min, insulation 3h, removes the elements such as C, N excessive in powder, with CO
2, N
2o
4form remove;
(6) planetary ball mill: use 300ml dehydrated alcohol as dispersion medium, by the material planetary ball mill 2h after calcining, dries 12h vacuum drying oven 80 DEG C, obtains gadolinium sesquioxide nano-powder.
As shown in Figure 1, 2, from Fig. 1,2, gadolinium sesquioxide particle diameter of nanometer powder is 50 ~ 100nm to the gadolinium sesquioxide nano-powder that the present embodiment obtains, and is evenly distributed.
Embodiment 2:
A microwave burning preparation method for nano oxidized gadolinium powder, comprises step as follows:
(1) Gd (NO is configured
3)
3solution: take 20g micron order gadolinium sesquioxide powder, concentrated nitric acid is diluted to 35wt%, Gd in molar ratio by 36.6g massfraction 68% concentrated nitric acid 32.9g deionized water
2o
3: HNO
3=1:7 configures Gd (NO
3)
3solution, is placed in 500ml beaker and dissolves in magnetic stirrer, ultrasonic disperse 5min by solution;
(2) Gadolinium trinitrate solution mixes with citric acid: take 92.4g monohydrate potassium and be dissolved in 150ml water, Gd in molar ratio
3+: C
6h
8o
7h
2o=4:1 configures precursor solution, is placed in 50 DEG C of constant temperature water baths, magnetic agitation 10min;
(3) adjust ph: dripping ammoniacal liquor adjust ph in precursor solution is 10;
(4) microwave burning synthesis: precursor solution is placed in household microwave oven conbustion synthesis, use moderate heat, the time is about 30min, and goods change white powder into by yellow is cellular;
(5) retort furnace calcining: white powder is placed in retort furnace, is warming up to 500 DEG C in 50min, insulation 3h, removes the elements such as C, N excessive in powder, with CO
2, N
2o
4form remove;
(6) planetary ball mill: use 300ml dehydrated alcohol as dispersion medium, polyvinylpyrrolidone, as dispersion agent, by the material planetary mills 2h after calcining, is dried 12h vacuum drying oven 80 DEG C, is obtained gadolinium sesquioxide nano-powder.
Embodiment 3:
A microwave burning preparation method for nano oxidized gadolinium powder, comprises step as follows:
(1) Gd (NO is configured
3)
3solution: take 20g micron order gadolinium sesquioxide powder, concentrated nitric acid is diluted to 35wt%, Gd in molar ratio by 36.6g massfraction 68% concentrated nitric acid 28.2g deionized water
2o
3: HNO
3=1:8 configures Gd (NO
3)
3solution, is placed in 500ml beaker and dissolves in magnetic stirrer, ultrasonic disperse 5min by solution;
(2) Gadolinium trinitrate solution mixes with citric acid: take 92.4g monohydrate potassium and be dissolved in 150ml, Gd in molar ratio
3+: C
6h
8o
7h
2o=4:1.5 configures precursor solution, is placed in 50 DEG C of constant temperature water baths, magnetic agitation 10min;
(3) adjust ph: dripping ammoniacal liquor adjust ph in precursor solution is 9;
(4) microwave burning synthesis: precursor solution is placed in household microwave oven conbustion synthesis, use moderate heat, the time is about 30min, and goods change white powder into by yellow is cellular;
(5) retort furnace calcining: white powder is placed in retort furnace, is warming up to 800 DEG C in 50min, insulation 2h, removes the elements such as C, N excessive in powder, with CO
2, N
2o
4form remove;
(6) planetary ball mill: use 300ml dehydrated alcohol as dispersion medium, polyvinylpyrrolidone, as dispersion agent, by the material planetary mills 2h after calcining, is dried 12h vacuum drying oven 80 DEG C, is obtained gadolinium sesquioxide nano-powder.
Embodiment 4:
A microwave burning preparation method for nano oxidized gadolinium powder, comprises step as follows:
(1) Gd (NO is configured
3)
3solution: take 20g micron order gadolinium sesquioxide powder, 36.6g massfraction 68% concentrated nitric acid 32.9g deionized water is diluted to 35wt%, Gd in molar ratio
2o
3: HNO
3=1:9 configures Gd (NO
3)
3solution, is placed in 500ml beaker and dissolves in magnetic stirrer, ultrasonic disperse 5min;
(2) Gadolinium trinitrate solution mixes with citric acid: take 92.4g monohydrate potassium and be dissolved in 150ml water, Gd in molar ratio
3+: C
6h
8o
7h
2o=4:2 configures precursor solution, is placed in 50 DEG C of constant temperature water baths, magnetic agitation 10min;
(3) adjust ph: dripping ammoniacal liquor adjust ph in precursor solution is 10;
(4) microwave burning synthesis: precursor solution is placed in household microwave oven conbustion synthesis, use moderate heat, the time is about 30min, and goods change white powder into by yellow is cellular;
(5) retort furnace calcining: white powder is placed in retort furnace, is warming up to 600 DEG C in 50min, insulation 2h, removes the elements such as C, N excessive in powder, with CO
2, N
2o
4form remove;
(6) planetary ball mill: use 300ml dehydrated alcohol as dispersion medium, polyvinylpyrrolidone, as dispersion agent, by the material planetary mills 2h after calcining, is dried 12h vacuum drying oven 80 DEG C, is obtained gadolinium sesquioxide nano-powder.
Comparative example 1:
As described in Example 1, unlike not adopting step (4) microwave burning to synthesize, dinectly bruning after adjustment pH.
The gadolinium sesquioxide nano-powder obtained after dinectly bruning is because of inequality of being heated, and size distribution is uneven.Because reaction is too violent, in the easy direct oxidation volatilization of the elements such as C, N and solution, oxygen element reacts, and Cd
3+can not get matching O
2+can not get reduction simultaneously, so reaction is not exclusively, poor effect.
Comparative example 2:
As described in Example 1, unlike not adjust ph in step (3).
The gadolinium sesquioxide nano-powder crystal grain obtained becomes large, and preparation cycle is elongated.Under the condition not having catalyzer, precursor solution is in microwave burning process, and the reaction times is elongated, after preparing white forerunner's solid mixture, has a large amount of black C powder residue in the powder of retort furnace calcining, needs calcining further except C.After increasing reaction time, also easily make crystal grain burning and grow up.
Claims (10)
1. a microwave burning preparation method for nano oxidized gadolinium powder, comprises step as follows:
(1) Gadolinium trinitrate solution is configured: mixed with salpeter solution by gadolinium sesquioxide powder, obtained Gadolinium trinitrate solution; Described gadolinium sesquioxide: the mol ratio of nitric acid is 1:(5-9);
(2) Gadolinium trinitrate solution mixes with citric acid: by Gadolinium trinitrate solution and citric acid solution by Gd
3+: citric acid mol ratio is 4:(1-2) mix, obtained precursor solution;
(3) adjust ph: the pH value of precursor solution is adjusted to 8 ~ 10;
(4) microwave burning synthesis: by the precursor solution microwave burning synthesis after adjust ph, obtain white powder;
(5) calcine: by white powder in 450 DEG C ~ 800 DEG C insulation calcining 2-5h;
(6) ball milling: by the material ball milling after calcining, dry, i.e. obtained nano oxidized gadolinium powder.
2. the microwave burning preparation method of nano oxidized gadolinium powder according to claim 1, is characterized in that, the gadolinium sesquioxide described in step (1): the mol ratio of nitric acid is 1:(6-7).
3. the microwave burning preparation method of nano oxidized gadolinium powder according to claim 1, is characterized in that, the concentration of the salpeter solution described in step (1) is 30-40wt%.
4. the microwave burning preparation method of nano oxidized gadolinium powder according to claim 1, is characterized in that, the citric acid described in step (2) is monohydrate potassium (C
6h
8o
7h
2o), Gd
3+: C
6h
8o
7h
2the mol ratio of O is 4:(1-1.5).
5. the microwave burning preparation method of nano oxidized gadolinium powder according to claim 1, is characterized in that, step regulates pH with ammoniacal liquor in (3).
6. the microwave burning preparation method of nano oxidized gadolinium powder according to claim 1, is characterized in that, described in step (4), the equipment of microwave burning is microwave oven.
7. the microwave burning preparation method of nano oxidized gadolinium powder according to claim 1, is characterized in that, in step (5), the equipment of calcining is retort furnace, and retort furnace calcining heat-up rate is 5 ~ 10 DEG C/min.
8. the microwave burning preparation method of nano oxidized gadolinium powder according to claim 1, is characterized in that, the calcining temperature described in step (5) is 500 DEG C ~ 800 DEG C.
9. the microwave burning preparation method of nano oxidized gadolinium powder according to claim 1, is characterized in that, in step (6), ball milling adopts wet ball grinding.
10. the microwave burning preparation method of nano oxidized gadolinium powder according to claim 9, is characterized in that, in step (6), wet ball grinding adopts ethanol to be dispersion medium, and employing polyvinylpyrrolidone is dispersion agent.
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Cited By (7)
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| CN108483480A (en) * | 2018-04-11 | 2018-09-04 | 内蒙古科技大学 | The method for preparing gadolinium oxide with plant precipitating reagent |
| CN109231254A (en) * | 2018-11-20 | 2019-01-18 | 常州市卓群纳米新材料有限公司 | A kind of preparation method of the gadolinium oxide particle of the D50:0.4-0.6 micron of high-purity high dispersive |
| CN109399689A (en) * | 2018-12-17 | 2019-03-01 | 中铝广西国盛稀土开发有限公司 | A method of rare earth oxide is prepared using microwave technology |
| CN111018527A (en) * | 2019-12-26 | 2020-04-17 | 江西鑫泰功能材料科技有限公司 | Preparation method of nano gadolinium oxide for dielectric ceramic capacitor |
| CN111533158A (en) * | 2020-04-24 | 2020-08-14 | 广西科学院 | Microwave calcination preparation method of dysprosium oxide nano powder |
| CN111533157A (en) * | 2020-04-24 | 2020-08-14 | 广西科学院 | Microwave calcination preparation method of gadolinium oxide nano powder |
| CN111634935A (en) * | 2020-04-24 | 2020-09-08 | 广西科学院 | Microwave preparation method of nano rare earth oxide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108483480A (en) * | 2018-04-11 | 2018-09-04 | 内蒙古科技大学 | The method for preparing gadolinium oxide with plant precipitating reagent |
| CN109231254A (en) * | 2018-11-20 | 2019-01-18 | 常州市卓群纳米新材料有限公司 | A kind of preparation method of the gadolinium oxide particle of the D50:0.4-0.6 micron of high-purity high dispersive |
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| CN111018527A (en) * | 2019-12-26 | 2020-04-17 | 江西鑫泰功能材料科技有限公司 | Preparation method of nano gadolinium oxide for dielectric ceramic capacitor |
| CN111533158A (en) * | 2020-04-24 | 2020-08-14 | 广西科学院 | Microwave calcination preparation method of dysprosium oxide nano powder |
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| CN111634935A (en) * | 2020-04-24 | 2020-09-08 | 广西科学院 | Microwave preparation method of nano rare earth oxide |
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