CN1807261A - Bismuth germanate nanometer powder preparation method - Google Patents

Bismuth germanate nanometer powder preparation method Download PDF

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CN1807261A
CN1807261A CN 200610023639 CN200610023639A CN1807261A CN 1807261 A CN1807261 A CN 1807261A CN 200610023639 CN200610023639 CN 200610023639 CN 200610023639 A CN200610023639 A CN 200610023639A CN 1807261 A CN1807261 A CN 1807261A
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bismuth
powder
germanium
preparation
nanometer powder
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顾明元
贺持缓
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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Abstract

The invention relates to a preparation method for nano bismuth germanate powder, which comprises: dissolving the bismuth salt into organic solvent with concentration as 0. 5~5M/L; adding Ge-contained compound by mole ratio to bismuth as 1: 12 into the solution; stirring and forming even sol; evaporating on normal or negative pressure to the sol to obtain the dried precursor powder; finally, sintering the powder on aerobic environment to obtain the final product. This invention needs low temperature and short time to prepare the Bi12GeO20 powder with high-efficient photocatalysis activation.

Description

The preparation method of bismuth germanate nanometer powder
Technical field
The present invention relates to a kind of bismuth germanium oxide (Bi 12GeO 20) preparation method of nano-powder, the bismuth germanate nanometer powder that makes can be used as photocatalyst, belongs to Materials science photocatalyst technology field.
Background technology
Bismuth germanium oxide (Bi 12GeO 20) be a kind of typical sillenite N-type waferN compound, belong to isometric system, the I23 point group.It has photoelectricity, electric light, fluorescence, magneto-optic, optically-active and piezoelectric properties, and particularly its good photoelectricity and electrooptical property make fields such as it is sold off at photoelectron, light, optical information processing material have extremely wide application prospect.
Traditional solid state reaction sintering method can be used to prepare Bi 12GeO 20Powder is promptly by Bi 2O 3And GeO 2Powder mixes, prepare by the solid state reaction sintering, it is even that the shortcoming of this method is that the mixing of two kinds of raw materials is difficult to reach, thereby solid state sintering obtains the higher temperature (being about 1000 ℃) and the long time (5～20 hours) of target product needs of single phase, grain growth, reunion at high temperature, thereby be difficult to obtain the powder of nanoscale, simultaneously because Bi 2O 3Surpassing under 800 ℃ the temperature and can appearance inevitably volatilize, thereby thermal treatment meeting at high temperature causes the synthetic product to depart from the ideal stoichiometric ratio.
Up to now, at preparation Bi 12GeO 20Nano-powder aspect, the open source literature that can retrieve are " Properties of nanoparticles of Bi 12GeO 20(BGO) obtained by ball milling, Journal of Materials Science Letters 2002,21 (12), pp.963-965 ", it has introduced a kind of by Bi 2O 3And GeO 2Powder prepares Bi through ball milling 12GeO 20The method of nano-powder.Compare with the solid state reaction sintering process, ball milled is to utilize mechanical activation reaction and the synthetic target product that two kinds of powders take place in ball milling, collision and crushing process, thereby does not need high-temperature heat treatment and obtain nano-powder.But the ball milled required time is long, and production efficiency is low.Bigger shortcoming is that introducing impurity causes pollution owing to can (comprising mill ball, grinding pot) from grinding system inevitably in the mechanical milling process, thereby is difficult to obtain high-purity Bi 12GeO 20Nano-powder.This is very disadvantageous for being used for light-catalysed semiconductor material.
And about Bi 12GeO 20Nano-powder does not also have relevant report in the application of photocatalyst.
In recent years, the application of conductor photocatalysis technology at aspects such as environmental improvement and photocatalytic hydrogen production by water decomposition obtained paying close attention to very widely.Spectral response, raising photochemical catalysis quantum yield and the light-catalyzed reaction speed of widening photocatalyst are the main directions of development of new photocatalyst.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of bismuth germanate nanometer powder is provided, adopt simple technology and equipment, the acquisition particle diameter is less, specific surface area is big and well-crystallized's bismuth germanate nanometer powder, can be used for photocatalysis degradation organic contaminant.
For realizing this purpose, in the technical solution used in the present invention, at first bismuth salt is dissolved in the organic solvent, forming the bismuth salt concn is the bismuth-containing solution of 0.5～5M, Bi: Ge=12 in molar ratio again: 1 joins germanium-containing compound in the bismuth-containing solution, fully stir, form uniform sol, colloidal sol is adopted atmospheric evaporation or negative pressure evaporation, obtain the dry precursor powder, at last in the environment of aerobic, precursor powder is carried out sintering, prepare purity and the good Bi of degree of crystallinity in lower temperature with in than the short time 12GeO 20Nano-powder.Bi 12GeO 20Nano-powder demonstrates photocatalytic activity efficiently, can be used for photocatalysis degradation organic contaminant.
Method of the present invention specifically may further comprise the steps:
1, bismuth salt is dissolved in the organic solvent, forming the bismuth salt concn is the bismuth-containing solution of 0.5～5M.
2, Bi: Ge=12 in molar ratio: 1, germanium-containing compound is joined in the bismuth-containing solution, fully stir, form uniform sol.
3, colloidal sol is adopted atmospheric evaporation or negative pressure evaporation, vaporization temperature is controlled at 100～350 ℃, obtains the dry precursor powder.
4, in the environment of aerobic precursor powder is carried out sintering, sintering temperature is 450～750 ℃, and sintering time is 0.5～4 hour, promptly gets bismuth germanate nanometer powder.
Bismuth salt of the present invention is the nitrate of bismuth, acetate or carbonate.If aforesaid bismuth salt contains crystal water, should remove crystal water by oven dry before use.When using Glacial acetic acid, can use the bismuth salt that contains crystal water, and needn't remove crystal water in advance as organic solvent.
Germanium-containing compound of the present invention is nitric acid germanium, Germanium tetraacetate, tetramethoxy germanium ((CH 2O) 4Ge), tetraethoxy germanium ((C 2H 5O) 4Ge) or organic germanium sesquioxide, as carboxyethyl germanium sesquioxide (O 3(GeCH 2CH 2COOH) 2).
Organic solvent of the present invention is a Glacial acetic acid, dehydrated alcohol or anhydrous propanone.Preferred Glacial acetic acid.Glacial acetic acid has good solubility to bismuth salt, and acetate has stronger complexing action to bismuth ion simultaneously, can suppress the hydrolysis of bismuth salt effectively, thereby when using Glacial acetic acid as organic solvent, can use the bismuth salt that contains crystal water.
Evaporation of the present invention is meant atmospheric evaporation or negative pressure evaporation, and vaporization temperature can be selected according to the boiling point of solvent is different, selects higher relatively vaporization temperature for the solvent that boiling point is lower, selects lower vaporization temperature for the solvent that boiling point is higher.Under the situation of negative pressure evaporation, can select than atmospheric evaporation lower vaporization temperature.Volatilization, nitrate radical and the reactions such as organic decomposition and burning of crystal water, small organic molecule take place in precursor sol in the evaporation drying course, thereby remove solvent and part organic group, obtain exsiccant solid precursor powder.
Outside the organic solvent that bismuth-containing solution of the present invention can also be stated before use, use glycol dimethyl ether (CH 3OCH 2CH 2OH) or diethylene glycol dimethyl ether (CH 3OCH 2CH 2) 2O is as cosolvent.Glycol dimethyl ether or diethylene glycol dimethyl ether can promote the dissolving of bismuth salt and germanium salt, can also play the effect of regulating dissolved adhesiveness simultaneously.The ratio of glycol dimethyl ether (diethylene glycol dimethyl ether) and aforementioned organic solvent can be regulated between 1: 2～1: 5.
Sintering of the present invention is to carry out in the environment of aerobic, therefore can be chosen in and carry out sintering in the air, also can carry out sintering in oxygen atmosphere.Sintering temperature can be between 450～750 ℃, and preferred 550～650 ℃, and sintering time is 0.8～1 hour.Temperature is too low, promptly is lower than 450 ℃, can not obtain the Bi of pure phase 12GeO 20Nano-powder, and temperature is when surpassing 750 ℃ because Bi volatilizees easily, thereby is difficult to obtain the Bi of strict stoichiometric ratio 12GeO 20Nano-powder.When selecting for use 550～650 ℃ to carry out sintering, can be no more than obtain in time of 1 hour the well-crystallized, be flaxen Bi 12GeO 20Nano-powder.When selecting for use lesser temps to carry out sintering, need the proper extension sintering time, with the purity of assurance crystalline phase and the quality of crystallization, the concrete time can be determined by the XRD analysis of final product.
Adopt method of the present invention can prepare the Bi of particle diameter between 20～200nm 12GeO 20Nano-powder.Diameter of particle is by sintering time and sintering temperature decision, and different sintering schedules can obtain the nano-powder of different-grain diameter.Increase sintering temperature and prolong sintering time, can cause growing up of crystal grain.Therefore, can determine suitable sintering schedule according to actual needs.
Adopt the Bi of method preparation of the present invention 12GeO 20Nano-powder, its semiconductor energy gap is about 2.6eV.Compare with traditional titanium dioxide (its semiconductor energy gap is about 3.2eV, can only absorb the following UV-light of 400nm), widened the photoresponse interval of photocatalyst widely, created good condition for utilizing sun natural light to carry out photochemical catalysis as light source.
Method technical process of the present invention is simple, less demanding to equipment, simultaneously because initial feed is the uniform mixing that Bi salt and Ge salt can reach molecular scale, overcome the characteristics of conventional solid-state method sintered compound inequality, thereby can in lower temperature and short time, obtain well-crystallized's target product.Simultaneously, adopt method of the present invention can obtain the nano-powder that particle diameter is less, specific surface area is bigger.
Bi of the present invention 12GeO 20Nano-powder is applied to photocatalyst, has excellent photocatalysis activity, and chemical stability is good, has a good application prospect at aspects such as organic pollutant degradation, indoor air purification, treating vehicle exhaust, photochemical catalyzing.
Description of drawings
Fig. 1 is the Bi with the inventive method preparation 12GeO 20The XRD figure spectrum of powder: (a) before the photochemical catalysis; (b) after the photochemical catalysis.
Fig. 2 is the Bi with the inventive method preparation 12GeO 20The TEM figure of powder.
Fig. 3 is the Bi with the inventive method preparation 12GeO 20The absorption spectrum of powder.
Fig. 4 is using Bi of the present invention 12GeO 20In the process of powder photocatalytic degraded methyl orange dye, the uv-visible absorption spectroscopy of methyl orange aqueous solution is with the variation of rayed time.
Embodiment
Below in conjunction with drawings and Examples technical scheme of the present invention is further described.Following examples do not constitute limitation of the invention.
Embodiment 1
0.12mol five nitric hydrate bismuth (Bi (NO 3) 35H 2O) be dissolved in 180ml Glacial acetic acid (CH 3COOH) in, dropwise add 0.01mol tetraethoxy germanium ((C then 2H 5O) 4Ge), add 60ml glycol dimethyl ether (CH simultaneously 3OCH 2CH 2OH), fully stir and form uniform sol as the viscosity of cosolvent regulator solution.Aforementioned colloidal sol 150 ℃ of evaporation oven dry down, is obtained precursor powder.Gained precursor powder under 650 ℃ temperature normal pressure-sintered 0.8 hour promptly obtains Bi 12GeO 20Nano-powder.
Embodiment 2
0.12mol Bismuth trinitrate (Bi (NO 3) 3) be dissolved in 30ml anhydrous propanone (CH 3COCH 3) in, dropwise add 0.01mol tetramethoxy germanium ((CH then 2O) 4Ge), add 15ml diethylene glycol dimethyl ether (CH simultaneously 3OCH 2CH 2) 2O fully stirs and forms uniform sol as the viscosity of cosolvent regulator solution.Aforementioned colloidal sol 350 ℃ of evaporation oven dry down, is obtained precursor powder.Gained precursor powder under 750 ℃ temperature normal pressure-sintered 0.5 hour promptly obtains Bi 12GeO 20Nano-powder.
Embodiment 3
0.12mol bismuth acetate (Bi (CH 3COO) 3) be dissolved in 100ml dehydrated alcohol (CH 3CH 2OH) in, add 0.01mol nitric acid germanium (Ge (NO then 3) 4), fully stir and form uniform sol.Aforementioned colloidal sol 100 ℃ of evaporation oven dry down, is obtained precursor powder.Gained precursor powder under 450 ℃ temperature normal pressure-sintered 4 hours promptly obtains Bi 12GeO 20Nano-powder.
Embodiment 4
0.24mol Bismuth carbonate (Bi (CO 3) 3) be dissolved in 100ml Glacial acetic acid (CH 3COOH) in, add 0.01mol carboxyethyl germanium sesquioxide (O then 3(GeCH 2CH 2COOH) 2), add 20ml glycol dimethyl ether (CH simultaneously 3OCH 2CH 2OH), fully stir and form uniform sol as the viscosity of cosolvent regulator solution.Aforementioned colloidal sol 200 ℃ of evaporation oven dry down, is obtained precursor powder.Gained precursor powder under 550 ℃ temperature normal pressure-sintered 1 hour promptly obtains Bi 12GeO 20Nano-powder.
Fig. 1 is the Bi that adopts the inventive method to obtain 12GeO 20The XRD figure spectrum of nano-powder, the position of each diffraction peak and JCPDS data card No.77-0861 meet well, and peak shape is sharp-pointed, represent that prepared sample is by single Bi 12GeO 20Phase composite, crystallization is good.From Bi of the present invention 12GeO 20Nano-powder before photochemical catalysis after (a) and the photochemical catalysis in the XRD figure of (b) spectrum as can be seen, its structure does not change before and after the photochemical catalysis, demonstrates satisfactory stability.
Fig. 2 is the Bi that adopts according to the embodiment of the invention 1 gained 12GeO 20The transmission electron microscope photo of nano-powder, as can be seen from Figure 2, it is irregular shape, and median size is about 50nm.Diameter of particle is by sintering time and sintering temperature decision, and different sintering schedules can obtain the nano-powder of different-grain diameter.Increase sintering temperature and prolong sintering time, can cause growing up of crystal grain.Therefore, can determine suitable sintering schedule according to actual needs.
Adopt the Bi of method preparation of the present invention 12GeO 20Nano-powder, its semiconductor energy gap is about 2.6eV.Fig. 3 is the Bi with the inventive method preparation 12GeO 20The absorption spectrum of powder as can be seen from Figure 3, adopts the Bi of method preparation of the present invention 12GeO 20Nano-powder can absorb the visible light of wavelength region between 400～550nm.(its semiconductor energy gap is about 3.2eV, can only absorb the following UV-light of 400nm, and good condition has been created for utilizing sun natural light to carry out photochemical catalysis as light source in the photoresponse interval of having widened photocatalyst widely with traditional titanium dioxide.
For estimating the Bi that adopts the inventive method preparation 12GeO 20Nano-powder is as the photocatalytic activity of photocatalyst, with than the typical nitrogenous dyestuff organic compound tropeolin-D of difficult degradation as the model organic pollutant, with embodiment 1 prepared Bi 12GeO 20Nano-powder is that photocatalyst carries out the photocatalytic degradation experiment to methyl orange aqueous solution.Accurately take by weighing the Bi of 5g/l 12GeO 20Nano powder photocatalyst, add in the beaker of the methyl orange aqueous solution that fills 25mg/l, the dark place ultra-sonic dispersion made to reach the adsorption-desorption balance between catalyzer and methyl orange solution after 30 minutes under the room temperature, carried out photocatalytic degradation experiment under the situation of magnetic agitation having then.Used light source is the 250W high voltage mercury lamp, and light source is about 10cm apart from liquid level.Under light source irradiation, every sampling in 15 minutes once, get part solution after high speed centrifugation separates, get upper solution again and on 756MC type spectrophotometer, detects degraded front and back methyl orange solution (～the absorbancy 465nm) located over time having maximum absorption band.
Fig. 4 is using Bi of the present invention 12GeO 20In the process of powder photocatalytic degraded methyl orange dye, the uv-visible absorption spectroscopy of methyl orange aqueous solution over time.Actual conditions is: methyl orange solution concentration is 25mg/l, Bi 12GeO 20Loading capacity 6g/l.The pairing rayed time of each curve is (a) 0 minute among the figure; (b) 10 minutes; (c) 20 minutes; (d) 30 minutes; (e) 40 minutes; (f) 50 minutes.As can see from Figure 4, (～the absorbancy 465nm) located increases and reduces gradually with irradiation time the charateristic avsorption band of methyl orange solution, until last completely dissolve, show that the azo bond in the methyl orange molecule (N=N-) destroyed by photochemical catalytic oxidation, the color of solution also to the last becomes water white solution by orange-yellow shoaling gradually simultaneously, shows at Bi 12GeO 20Under the effect of nano powder photocatalyst, methyl orange molecule is degraded really effectively.

Claims (7)

1, a kind of preparation method of bismuth germanate nanometer powder is characterized in that may further comprise the steps:
1) bismuth salt is dissolved in the organic solvent, forming the bismuth salt concn is the bismuth-containing solution of 0.5～5M;
2) Bi: Ge=12 in molar ratio: 1, germanium-containing compound is joined in the bismuth-containing solution, fully stir, form uniform sol;
3) colloidal sol is adopted atmospheric evaporation or negative pressure evaporation, vaporization temperature is controlled at 100～350 ℃, obtains the dry precursor powder;
4) in the environment of aerobic precursor powder is carried out sintering, sintering temperature is 450～750 ℃, and sintering time is 0.5～4 hour, promptly gets bismuth germanate nanometer powder.
2, according to the preparation method of the bismuth germanate nanometer powder of claim 1, it is characterized in that described bismuth salt is the nitrate of bismuth, acetate or carbonate.
3, according to the preparation method of the bismuth germanate nanometer powder of claim 1, it is characterized in that described germanium-containing compound is nitric acid germanium, Germanium tetraacetate, tetramethoxy germanium, tetraethoxy germanium or organic germanium sesquioxide.
4, according to the preparation method of the bismuth germanate nanometer powder of claim 1, it is characterized in that described organic solvent is a Glacial acetic acid, dehydrated alcohol or anhydrous propanone.
5, according to the preparation method of the bismuth germanate nanometer powder of claim 1, it is characterized in that described sintering temperature is 550～650 ℃, sintering time is 0.8～1 hour.
6, according to the preparation method of the bismuth germanate nanometer powder of claim 1, it is characterized in that described bismuth-containing solution also uses glycol dimethyl ether or diethylene glycol dimethyl ether as cosolvent, the ratio control of cosolvent and aforementioned organic solvent is between 1: 2～1: 5.
7, a kind of application of bismuth germanate nanometer powder of the method preparation of adopting claim 1 or 6 is characterized in that using photocatalyst.
CN 200610023639 2006-01-26 2006-01-26 Bismuth germanate nanometer powder preparation method Pending CN1807261A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103526294A (en) * 2013-10-16 2014-01-22 中国科学院上海硅酸盐研究所 Crystalline material with intermediate infrared broadband luminescence property and preparation method thereof
CN103586015A (en) * 2013-11-22 2014-02-19 武汉理工大学 Method for preparing regular-triangular-pyramid-shaped bismuth germinate visible-light catalyst
CN105727937A (en) * 2016-02-17 2016-07-06 桂林理工大学 Visible-light response photocatalyst Mn3Bi2Ge3O12 and preparation method thereof
CN106082330A (en) * 2016-07-29 2016-11-09 安徽理工大学 The Bi that a kind of size is controlled12geO20mesomorphic and synthetic method thereof
CN109078645A (en) * 2018-09-04 2018-12-25 辽宁大学 A kind of photochemical catalyst and its preparation method and application of novel cladding Z-type structure
CN109289873A (en) * 2018-10-29 2019-02-01 江苏大学 A kind of heterojunction material and preparation method and purposes
CN109553132A (en) * 2018-11-22 2019-04-02 商丘师范学院 A kind of bismuth germanium oxide two-dimensional nano piece and preparation method thereof

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103526294A (en) * 2013-10-16 2014-01-22 中国科学院上海硅酸盐研究所 Crystalline material with intermediate infrared broadband luminescence property and preparation method thereof
CN103586015A (en) * 2013-11-22 2014-02-19 武汉理工大学 Method for preparing regular-triangular-pyramid-shaped bismuth germinate visible-light catalyst
CN103586015B (en) * 2013-11-22 2015-07-22 武汉理工大学 Method for preparing regular-triangular-pyramid-shaped bismuth germinate visible-light catalyst
CN105727937A (en) * 2016-02-17 2016-07-06 桂林理工大学 Visible-light response photocatalyst Mn3Bi2Ge3O12 and preparation method thereof
CN106082330A (en) * 2016-07-29 2016-11-09 安徽理工大学 The Bi that a kind of size is controlled12geO20mesomorphic and synthetic method thereof
CN106082330B (en) * 2016-07-29 2017-06-16 安徽理工大学 A kind of controllable Bi of size12GeO20Mesomorphic and its synthetic method
CN109078645A (en) * 2018-09-04 2018-12-25 辽宁大学 A kind of photochemical catalyst and its preparation method and application of novel cladding Z-type structure
CN109078645B (en) * 2018-09-04 2021-04-30 辽宁大学 Photocatalyst coated with Z-shaped structure and preparation method and application thereof
CN109289873A (en) * 2018-10-29 2019-02-01 江苏大学 A kind of heterojunction material and preparation method and purposes
CN109289873B (en) * 2018-10-29 2021-09-10 江苏大学 Heterojunction material, preparation method and application
CN109553132A (en) * 2018-11-22 2019-04-02 商丘师范学院 A kind of bismuth germanium oxide two-dimensional nano piece and preparation method thereof
CN109553132B (en) * 2018-11-22 2021-03-30 商丘师范学院 Bismuth germanate two-dimensional nanosheet and preparation method thereof

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