CN102351513A - Preparation method for bismuth silicate powder for utilization of optical performance - Google Patents

Preparation method for bismuth silicate powder for utilization of optical performance Download PDF

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CN102351513A
CN102351513A CN2011101870906A CN201110187090A CN102351513A CN 102351513 A CN102351513 A CN 102351513A CN 2011101870906 A CN2011101870906 A CN 2011101870906A CN 201110187090 A CN201110187090 A CN 201110187090A CN 102351513 A CN102351513 A CN 102351513A
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bismuth
powder
containing solution
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sintering
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CN102351513B (en
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王秀峰
许亚琴
江红涛
鲁俊雀
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Shaanxi University of Science and Technology
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Abstract

The invention relates to preparation of optical crystals and discloses a preparation method for bismuth silicate powder for utilization of optical performance. The method comprises the following steps: dissolving Bi(NO)3.5H2O in glacial acetic acid to prepare a bismuth-containing solution; adding ethyl orthosilicate drop by drop into the bismuth-containing solution according to a mol ratio of Bi to Si of 12:1, carrying out ultrasonic rinsing at low temperature, and adjusting viscosity by utilizing analytically pure ethylene glycol methyl ether to form a uniform sol; drying the sol to obtain dried precursor powder; sintering the precursor powder to obtain bismuth silicate Bi12SiO20 powder. The invention enables Bi12SiO20 powder with good purity and crystallinity to be prepared at low temperature within a short period of time, and the preparation method has the advantages of a simple preparation process, a short period and low cost.

Description

A kind of optical property is with the preparation method of bismuth silicate powder
Technical field
The present invention relates to the preparation of optical crystal material, be specifically related to the preparation method of a kind of optical property with bismuth silicate powder.
Background technology
Bismuth silicate (Bi 12SiO 20, be called for short BSO) and be non-ferroelectric cube of semi-insulator of a kind of broad-band gap, high resistivity.Effects such as it has simultaneously that electric light, photoconduction, light are sold off, piezoelectricity, acousto-optic, optically-active and faraday rotation; Take a picture in Hologram Storage, interferometry speckle, the application of phase place coupling and aspect such as in real time relevant, having demonstrated it is a kind of up-and-coming multifunctional material.Utilize electric light and the photoconductive property of BSO, at room temperature just can realize many kinds of nonlinear optics conversion with low power laser.As real-time body hologram recording material, BSO is one of a few photorefractive material that sensitivity is the highest, response speed is the fastest that is obtained at present, thereby in technology such as optical information processing in real time and photometry calculation, is widely used.Many fields such as incoherent/coherent light picture inversion that these application comprise (PROM, PRIZ etc.), optical storage, real-time interferometry, image multiplication and phase conjugate.In addition, the detection that photo-sensor is used for electric substation's internal fault is also processed with this material by Japan, has also developed the transmitter that can measure current/voltage simultaneously.Can expect that along with light being sold off the further understanding of microprocess and going deep into of applied research, the BSO optical dioptric device will get into the practical stage and become commercialized device, thereby in the message area in future, plays a significant role.
Wang Yan etc. are with Bi 2O 3With SiO 2Mix than 1: 1 with amount of substance, solid state reaction generates Bi at a certain temperature 2SiO 5, Bi 12SiO 20And Bi 4Si 3O 12Etc. multiple crystalline phase.It is more to show that this component produces the crystalline kind in temperature-rise period, prepares single crystal preparation technology and is difficult to control.Zhang Zhengguang etc. are with Bi 2O 3And SiO 2Be raw material, the bismuth silicate (Bi that adopted prepared by mechanical alloy 12SiO 20) powder.This method utilizes the mechanical alloying that takes place in collision and crushing process repeatedly of two kinds of powders to react to synthesize target product, has saved high-temperature heat treatment process.But the mechanical alloying method required time is long, and production efficiency is low, is inappropriate for the batch process bismuth silicate powder.
Document " Journal of Materials Science Letters 1999,18:1871-1874 " and document " silicate circular, 2007,26 (6): 1236-1239 " are to adopt mechanical alloying to prepare bismuth silicate powder.This method is to be raw material with bismuth oxide and silicon oxide powder; Directly prepare bismuth silicate powder through high-energy ball milling; This method has utilized the mechanical alloying that two kinds of powders take place in collision and crushing process times without number to react to synthesize target product, has saved high-temperature heat treatment process.But the mechanical alloying method required time is long, and production efficiency is low, is inappropriate for the batch process bismuth silicate powder.
CN10038071C provides a kind of preparation high purity silicic acid bismuth nano-powder; At first bismuth salt is dissolved in the organic solvent; Forming the bismuth salt concn is the bismuth-containing solution of 0.5~5M; At Bi: Si=12 in molar ratio: 1 joins silicoorganic compound in the bismuth-containing solution; Fully stir; Form uniform solution; Colloidal sol is adopted atmospheric evaporation or negative pressure evaporation; Obtain exsiccant precursor powder; At last in the environment of aerobic, the precursor powder is carried out sintering, prepare purity and the good bismuth silicate nano powder of degree of crystallinity in lower temperature with in than the short time.Its common whole sol-gel process required time is longer, often needs several days or several weeks of youngster: there are a large amount of micropores in the gel, and in drying process, will overflow again many gases and organism, and produce contraction.
Document " preparation method of CN1821088A bismuth silicate nano powder and application " adopts solvent evaporation method to prepare nano level bismuth silicate powder; And Congo red performance in its photocatalytic degradation water estimated, think that bismuth silicate has bigger potentiality to be exploited as photocatalyst.
CN101157026A provides a kind of preparation method of bismuth silicate powder photocatalyst.At first with five water Bismuth trinitrates and block interpolymers surfactant dissolves in acetate, form even clear soln, again bismuth in molar ratio: silicon=12: 1 joins silicon ester in the bismuth-containing solution, fully stirs, and forms uniform sol.After the ageing; It is moved into airtight crystallization in the autoclave, obtain the composite oxides gel of bismuth silicon, after filtration, washing, drying; In air ambient, this precursor powder is carried out roasting at last, stable and uniform ground obtains the good bismuth silicate powder of degree of crystallinity under lower temperature.And this catalyst particles granularity is bigger, is convenient to from water body, separate be beneficial to reclaim use, and has photocatalytic activity efficiently, can be used for photocatalysis degradation organic contaminant.Its shortcoming is to be reflected in the airtight container to carry out, and can't observe process of growth, and is not directly perceived; And equipment requirements high (steel of high temperature high voltage resistant, corrosion resistant liner), technical difficulty big (temperature and pressure control is strict), cost height; Poor safety performance; Be unfavorable for suitability for industrialized production.
Summary of the invention
In order to overcome the deficiency of above-mentioned prior art, the object of the present invention is to provide the preparation method of a kind of optical property with bismuth silicate powder, can prepare purity and the good Bi of degree of crystallinity in lower temperature with in than the short time 12SiO 20Powder, and preparation technology is simple, and the cycle is short, and cost is low.
To achieve these goals, the technical scheme of the present invention's employing is:
A kind of optical property may further comprise the steps with the preparation method of bismuth silicate powder:
The first step is with the Bi (NO) of 0.01~0.04mol 35H 2O is dissolved in the glacial acetic acid of 15~60ml and makes bismuth-containing solution;
Second step; Bi: Si=12 in molar ratio: 1 is added drop-wise to tetraethoxy in the above-mentioned bismuth-containing solution; After put into ultrasonic instrument in 10~40 ℃ of following ultrasonic cleaning 1~6h, utilize the analytical pure ethylene glycol monomethyl ether of 0.01~10ml to regulate viscosity, form uniform sol;
In the 3rd step, the colloidal sol that obtains carries out drying, and drying temperature is controlled at 90~150 ℃, and be 9~15h time of drying, obtains the dry precursor powder;
The 4th step, said precursor powder is carried out sintering, sintering temperature is 700~900 ℃, sintering time is 1~12h, promptly gets bismuth silicate Bi 12SiO 20Powder.
More excellent scheme, the dropping time of tetraethoxy is 1~30min in second step.
Compared with prior art, advantage of the present invention is:
(1) method is easy, easy handling, and reaction conditions is gentle;
(2) preparation cycle is short, is generally 2~3 days;
(3) the preparation impurity in products is few, and purity is higher, and degree of crystallinity is good, and calculating can get thing phase Bi 12SiO 20Massfraction be 89%, degree of crystallinity is 75%.
Description of drawings
Accompanying drawing is the bismuth silicate Bi of the embodiment of the invention three preparations 12SiO 20The XRD figure of powder, sintering condition is 800 ℃ of insulation 1.5h in the preparation process.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is explained further details.
Embodiment one
A kind of optical property may further comprise the steps with the preparation method of bismuth silicate powder:
The first step is with the Bi (NO) of 0.01mol 35H 2O is dissolved in the glacial acetic acid of 15ml and makes bismuth-containing solution;
In second step, Bi: Si=12 in molar ratio: 1 is added drop-wise to tetraethoxy in the said bismuth-containing solution, after put into ultrasonic instrument in 40 ℃ of following ultrasonic cleaning 1h, utilize the analytical pure ethylene glycol monomethyl ether of 0.01ml to regulate viscosity, form uniform sol;
In the 3rd step, 90 ℃ of dry 15h of the colloidal sol that obtains obtain the dry precursor powder;
The 4th step, said precursor powder to be put into put into retort furnace together with alumina crucible behind the alumina crucible and carry out sintering, sintering temperature is 700 ℃, sintering time 12h promptly gets bismuth silicate Bi 12SiO 20Powder.
Embodiment two
A kind of optical property may further comprise the steps with the preparation method of bismuth silicate powder:
The first step is with the Bi (NO) of 0.04mol 35H 2O is dissolved in the glacial acetic acid of 60ml and makes bismuth-containing solution;
In second step, Bi: Si=12 in molar ratio: 1 is added drop-wise to tetraethoxy in the said bismuth-containing solution, after put into ultrasonic instrument in 10 ℃ of following ultrasonic cleaning 1h, utilize the analytical pure ethylene glycol monomethyl ether of 10ml to regulate viscosity, form uniform sol;
In the 3rd step, 150 ℃ of dry 9h of the colloidal sol that obtains obtain the dry precursor powder;
The 4th step, said precursor powder to be put into put into retort furnace together with alumina crucible behind the alumina crucible and carry out sintering, sintering temperature is 900 ℃, sintering time is 1h, promptly gets bismuth silicate Bi 12SiO 20Powder.
Embodiment three
A kind of optical property may further comprise the steps with the preparation method of bismuth silicate powder:
The first step is with the Bi (NO) of 0.02mol 35H 2O is dissolved in the glacial acetic acid of 20ml and makes bismuth-containing solution;
In second step, Bi: Si=12 in molar ratio: 1 is added drop-wise to tetraethoxy in the said bismuth-containing solution, after put into ultrasonic instrument in 30 ℃ of following ultrasonic cleaning 2h, utilize the analytical pure ethylene glycol monomethyl ether of 0.1ml to regulate viscosity, form uniform sol;
In the 3rd step, 100 ℃ of dry 11h of the colloidal sol that obtains obtain the dry precursor powder;
The 4th step, said precursor powder to be put into put into retort furnace together with alumina crucible behind the alumina crucible and carry out sintering, sintering temperature is 800 ℃, sintering time is 1.5h, promptly gets bismuth silicate Bi 12SiO 20Powder.
The bismuth silicate Bi that present embodiment is made 12SiO 20Powder is analyzed, and its XRD figure can be found out the bismuth silicate Bi that present embodiment makes shown in accompanying drawing 12SiO 20Powder purity is higher.
Embodiment four
A kind of optical property may further comprise the steps with the preparation method of bismuth silicate powder:
The first step is with the Bi (NO) of 0.03mol 35H 2O is dissolved in the glacial acetic acid of 50ml and makes bismuth-containing solution;
In second step, Bi: Si=12 in molar ratio: 1 is added drop-wise to tetraethoxy in the said bismuth-containing solution, after put into ultrasonic instrument in 20 ℃ of following ultrasonic cleaning 4h, utilize the analytical pure ethylene glycol monomethyl ether of 6ml to regulate viscosity, form uniform sol;
In the 3rd step, 120 ℃ of dry 10h of the colloidal sol that obtains obtain the dry precursor powder;
The 4th step, said precursor powder to be put into put into retort furnace together with alumina crucible behind the alumina crucible and carry out sintering, sintering temperature is 850 ℃, sintering time is 4h, promptly gets bismuth silicate Bi 12SiO 20Powder.
Embodiment five
A kind of optical property may further comprise the steps with the preparation method of bismuth silicate powder:
The first step is with the Bi (NO) of 0.03mol 35H 2O is dissolved in the glacial acetic acid of 22ml and makes bismuth-containing solution;
In second step, Bi: Si=12 in molar ratio: 1 is added drop-wise to tetraethoxy in the said bismuth-containing solution, after put into ultrasonic instrument in 10~40 ℃ of following ultrasonic cleaning 2h, utilize the analytical pure ethylene glycol monomethyl ether of 5.5ml to regulate viscosity, form uniform sol;
In the 3rd step, 100 ℃ of dry 10h of the colloidal sol that obtains obtain the dry precursor powder;
The 4th step, said precursor powder to be put into put into retort furnace together with alumina crucible behind the alumina crucible and carry out sintering, sintering temperature is 750 ℃, sintering time is 8h, promptly gets bismuth silicate Bi 12SiO 20Powder.
The bismuth silicate Bi that above each embodiment is made 12SiO 20The powder experiment Analysis, its thing phase Bi 12SiO 20Massfraction for can reach 89%, degree of crystallinity reaches 75%.

Claims (8)

1. an optical property is characterized in that with the preparation method of bismuth silicate powder, may further comprise the steps:
The first step is with the Bi (NO) of 0.01~0.04mol 35H 2O is dissolved in the glacial acetic acid of 15~60mL and makes bismuth-containing solution;
Second step; Bi: Si=12 in molar ratio: 1 is added drop-wise to tetraethoxy in the said bismuth-containing solution; After put into ultrasonic instrument in 10~40 ℃ of following ultrasonic cleaning 1~6h, utilize the analytical pure ethylene glycol monomethyl ether of 0.01~10mL to regulate viscosity, form uniform sol;
In the 3rd step, the colloidal sol that obtains carries out drying, and drying temperature is controlled at 90~150 ℃, and be 9~15h time of drying, obtains the dry precursor powder;
The 4th step, said precursor powder is carried out sintering, sintering temperature is 700~900 ℃, sintering time is 1~12h, promptly gets bismuth silicate Bi 12SiO 20Powder.
2. an optical property is characterized in that with the preparation method of bismuth silicate powder, may further comprise the steps:
The first step is with the Bi (NO) of 0.01mol 35H 2O is dissolved in the glacial acetic acid of 15mL and makes bismuth-containing solution;
In second step, Bi: Si=12 in molar ratio: 1 is added drop-wise to tetraethoxy in the said bismuth-containing solution, after put into ultrasonic instrument in 40 ℃ of following ultrasonic cleaning 1h, utilize the analytical pure ethylene glycol monomethyl ether of 0.01mL to regulate viscosity, form uniform sol;
In the 3rd step, 90 ℃ of dry 15h of the colloidal sol that obtains obtain the dry precursor powder;
The 4th step, said precursor powder is carried out sintering, sintering temperature is 700 ℃, sintering time 12h promptly gets bismuth silicate Bi 12SiO 20Powder.
3. an optical property is characterized in that with the preparation method of bismuth silicate powder, may further comprise the steps:
The first step is with the Bi (NO) of 0.04mol 35H 2O is dissolved in the glacial acetic acid of 60mL and makes bismuth-containing solution;
In second step, Bi: Si=12 in molar ratio: 1 is added drop-wise to tetraethoxy in the said bismuth-containing solution, after put into ultrasonic instrument in 10 ℃ of following ultrasonic cleaning 1h, utilize the analytical pure ethylene glycol monomethyl ether of 10mL to regulate viscosity, form uniform sol;
In the 3rd step, 150 ℃ of dry 9h of the colloidal sol that obtains obtain the dry precursor powder;
The 4th step, said precursor powder is carried out sintering, sintering temperature is 900 ℃, sintering time is 1h, promptly gets bismuth silicate Bi 12SiO 20Powder.
4. an optical property is characterized in that with the preparation method of bismuth silicate powder, may further comprise the steps:
The first step is with the Bi (NO) of 0.02mol 35H 2O is dissolved in the glacial acetic acid of 20mL and makes bismuth-containing solution;
In second step, Bi: Si=12 in molar ratio: 1 is added drop-wise to tetraethoxy in the said bismuth-containing solution, after put into ultrasonic instrument in 30 ℃ of following ultrasonic cleaning 2h, utilize the analytical pure ethylene glycol monomethyl ether of 0.1mL to regulate viscosity, form uniform sol;
In the 3rd step, 100 ℃ of dry 11h of the colloidal sol that obtains obtain the dry precursor powder;
The 4th step, said precursor powder is carried out sintering, sintering temperature is 800 ℃, sintering time is 1.5h, promptly gets bismuth silicate Bi 12SiO 20Powder.
5. an optical property is characterized in that with the preparation method of bismuth silicate powder, may further comprise the steps:
The first step is with the Bi (NO) of 0.03mol 35H 2O is dissolved in the glacial acetic acid of 50mL and makes bismuth-containing solution;
In second step, Bi: Si=12 in molar ratio: 1 is added drop-wise to tetraethoxy in the said bismuth-containing solution, after put into ultrasonic instrument in 20 ℃ of following ultrasonic cleaning 4h, utilize the analytical pure ethylene glycol monomethyl ether of 6mL to regulate viscosity, form uniform sol;
In the 3rd step, 120 ℃ of dry 10h of the colloidal sol that obtains obtain the dry precursor powder;
The 4th step, said precursor powder is carried out sintering, sintering temperature is 850 ℃, sintering time is 4h, promptly gets bismuth silicate Bi 12SiO 20Powder.
6. an optical property is characterized in that with the preparation method of bismuth silicate powder, may further comprise the steps:
The first step is with the Bi (NO) of 0.03mol 35H 2O is dissolved in the glacial acetic acid of 22mL and makes bismuth-containing solution;
In second step, Bi: Si=12 in molar ratio: 1 is added drop-wise to tetraethoxy in the said bismuth-containing solution, after put into ultrasonic instrument in 10~40 ℃ of following ultrasonic cleaning 2h, utilize the analytical pure ethylene glycol monomethyl ether of 5.5mL to regulate viscosity, form uniform sol;
In the 3rd step, 100 ℃ of dry 10h of the colloidal sol that obtains obtain the dry precursor powder;
The 4th step, said precursor powder is carried out sintering, sintering temperature is 750 ℃, sintering time is 8h, promptly gets bismuth silicate Bi 12SiO 20Powder.
7. according to the preparation method of the described optical property of the arbitrary claim of claim 1 to 6, it is characterized in that the dropping time of tetraethoxy is 1~30min in said second step with bismuth silicate powder.
8. according to the preparation method of the described optical property of the arbitrary claim of claim 1 to 6, it is characterized in that said precursor powder is to put into to put into retort furnace together with alumina crucible behind the alumina crucible and carry out agglomerating with bismuth silicate powder.
CN 201110187090 2011-07-06 2011-07-06 Preparation method for bismuth silicate powder for utilization of optical performance Expired - Fee Related CN102351513B (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN105924145A (en) * 2016-05-05 2016-09-07 陕西科技大学 Preparation method of Bi12SiO20 porous material
CN105948807A (en) * 2016-05-05 2016-09-21 陕西科技大学 Preparation method of porous Bi12SiO20 bulk
CN105948808A (en) * 2016-05-05 2016-09-21 陕西科技大学 Preparation method of stable Bi12SiO20 nano-porous material
CN105967745A (en) * 2016-05-05 2016-09-28 陕西科技大学 Preparation method of porous stable state Bi12SiO20 block
RU2643563C1 (en) * 2017-06-13 2018-02-02 федеральное государственное бюджетное образовательное учреждение высшего образования "Белгородский государственный технологический университет им. В.Г. Шухова" METHOD FOR PRODUCTION OF BISMUTH SILICATE Bi12SiO20 CRYSTALLINE COMPOUND POWDER

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RU2669677C1 (en) * 2018-03-22 2018-10-12 Федеральное государственное автономное образовательное учреждение высшего образования "Сибирский федеральный университет" METHOD FOR PRODUCING Bi12SiO20 BISMUTH SILICATE BY CASTING METHOD

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105924145A (en) * 2016-05-05 2016-09-07 陕西科技大学 Preparation method of Bi12SiO20 porous material
CN105948807A (en) * 2016-05-05 2016-09-21 陕西科技大学 Preparation method of porous Bi12SiO20 bulk
CN105948808A (en) * 2016-05-05 2016-09-21 陕西科技大学 Preparation method of stable Bi12SiO20 nano-porous material
CN105967745A (en) * 2016-05-05 2016-09-28 陕西科技大学 Preparation method of porous stable state Bi12SiO20 block
RU2643563C1 (en) * 2017-06-13 2018-02-02 федеральное государственное бюджетное образовательное учреждение высшего образования "Белгородский государственный технологический университет им. В.Г. Шухова" METHOD FOR PRODUCTION OF BISMUTH SILICATE Bi12SiO20 CRYSTALLINE COMPOUND POWDER

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