CN104857980A - Preparation method of hexagonal boron nitride ceramic material stable silver carbonate semiconductor - Google Patents
Preparation method of hexagonal boron nitride ceramic material stable silver carbonate semiconductor Download PDFInfo
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Abstract
The invention relates to the field of material preparation, and specifically discloses a preparation method of a hexagonal boron nitride ceramic material stable silver carbonate semiconductor. The method comprises the following steps: (1) graphite-phase hexagonal boron nitride nano-sheets are prepared; (2) a boron nitride/silver carbonate composition is prepared with a precipitation method, wherein the prepared hexagonal boron nitride nano-sheets are subjected to ultrasonic dispersion in deionized water; silver nitrate is added; a sodium bicarbonate solution is added drop by drop under a magnetic stirring condition; deionized water and anhydrous ethanol are used in centrifugation and washing; and drying is carried out, such that a target product is obtained. According to the invention, the graphite-phase hexagonal boron nitride is prepared with a high-temperature calcination method, and is used as a carrier for preparing the boron nitride/silver carbonate composite material with a simple precipitation method, such that the obtained composite material has substantially improved activity and stability. The material has an important significance in synergetic catalysis and stable semiconductor.
Description
Technical field
The invention belongs to technical field of material, be specifically related to the preparation method that silver carbonate semiconductor stablized by a kind of hexagonal boron nitride ceramic material.
Technical background
Boron nitride is a kind of important ceramic compound, there is the process based prediction model of many excellences, as low in high heat conductance, non-oxidizability that chemical stability is high, excellent, density etc., therefore have broad application prospects in high temperature, high frequency, photoelectron and radioresistance etc.Boron nitride has various structures, mainly contain six sides, cube, tripartite etc.Wherein six side's phase boron nitrides (
h-BN) in B-N key be with
sp 2 hydridization bonding, very similar with the layer structure of graphite, be commonly called " white graphite ".In recent years, Graphene is widely used at catalytic field due to character such as its high-ratio surfaces, similar with graphite-structure
h-BN has high-ratio surface characteristic equally, is conducive to the dispersion of active component, therefore hexagonal boron nitride (
h-BN) also receive the concern of researcher gradually.With
h-BN carries out compound as catalyst carrier and other nano materials, is expected to prepare the higher nano composite material of catalytic activity, thus improves its application in photocatalysis field.
At present, the preparation method of boron nitride mainly contains: (1) water/solvent-thermal method; (2) template; (3) organic precursor method method.But these preparation methods exist some shortcomings, the character of such as precursors is unstable, poisonous and explosive, forms serious threat to environment and safety, and the productive rate of product and specific surface are not very high simultaneously.And boric acid-urea method technique is simple, it is preparation
hthe important method of-BN.The application is by boric acid-urea technique preparation
h-BN, and using it as catalyst carrier, the simple precipitation method of compound prepare the boron nitride/silver carbonate nano material of stable in properties, has great importance in the resistance to photoetch of silver carbonate and photocatalytic pollutant degradation.
Summary of the invention
A kind of simple method is the object of the present invention is to provide to prepare the preparation method that silver carbonate semiconductor stablized by hexagonal boron nitride ceramic material.With urea and boric acid for raw material, prepared by conventional high temperature synthesis
h-BN nanometer sheet, simultaneously using it as the carrier of catalyst, adopts the simple precipitation method to prepare hexagonal boron nitride/silver carbonate nano composite material.Stratiform
h-BN effectively can not only improve the performance of silver carbonate photocatalytic pollutant degradation, inhibits the photoetch of silver carbonate simultaneously.Preparation method of the present invention is simple, and environmental pollution is little, has great importance in photocatalysis field application.
The invention provides kind of a simple method and prepare preparation method and the application thereof that silver carbonate semiconductor stablized by hexagonal boron nitride ceramic material, this preparation method is realized by following steps:
(1) graphite-phase hexagonal boron nitride nanosheet is prepared:
Weigh CO (NH
2)
2and H
3bO
4in beaker, under ultrasonication, make it be dissolved in completely in deionized water, then water bath method solution under magnetic stirring, be placed in alumina crucible by sample after evaporate to dryness, and be placed in tube furnace, atmosphere of inert gases Program is warming up to calcining heat, after calcining terminates, after Temperature fall to room temperature, grinding, obtains graphite-phase boron nitride;
(2) graphite-phase boron nitride step (1) prepared is ultrasonic to be dispersed in ionized water, then adds silver nitrate, under ultrasonication, obtain homodisperse solution A;
(3) in solution A, dropwise add the ammonia spirit of 0.5mol/L, stir 20min obtained solution B under magnetic stirring simultaneously;
(4) sodium bicarbonate solution being dissolved in deionized water is dropwise joined in solution B, produce yellow mercury oxide, and Keep agitation under magnetic stirring, then centrifugal, obtain boron nitride/silver carbonate composite precipitation, with deionized water and absolute ethanol washing, centrifugal, vacuum drying, then grinding obtains boron nitride/silver carbonate nano-complex.
In step (1), described CO (NH
2)
2and H
3bO
4the ratio of amount of substance be 24:1.
In step (1), described bath temperature is 65 DEG C.
In step (1), described inert gas is nitrogen or argon gas, and the speed of described temperature programming is 3 ~ 8 DEG C/min, and described calcining heat is 700 ~ 1100 DEG C, and calcination time is 3 ~ 7h.
In step (1), described inert gas is nitrogen or argon gas, and the speed of described temperature programming is 4 ~ 7 DEG C/min, and calcining heat is 700 ~ 1000 DEG C, and the time of maintenance is 3 ~ 6h.
In step (1), described inert gas is nitrogen or argon gas, and the speed of described temperature programming is 4 ~ 6 DEG C/min, and calcining heat is 800 ~ 1000 DEG C, and the time of maintenance is 4 ~ 6h.
In step (2), the mass ratio of described boron nitride and silver nitrate is 1:20 ~ 1:70, and in step (3), the volume of described ammonia spirit is 0.5 ~ 3mL.
In step (2), the mass ratio of described boron nitride and silver nitrate is 1:30 ~ 1:60, and in step (3), the volume of ammonia spirit is 0.5 ~ 2mL.
In step (2), the mass ratio of described boron nitride and silver nitrate is 1:40 ~ 1:50, and in step (3), the volume of ammonia spirit is 0.5 ~ 1.5mL.
In step (4), the mass ratio of described silver nitrate and sodium acid carbonate is 2:1 ~ 6:1.
In step (4), the mass ratio of described silver nitrate and sodium acid carbonate is 3:1 ~ 6:1,
In step (4), the mass ratio of described silver nitrate and sodium acid carbonate is 3:1 ~ 5:1.
In step (4), the time of described magnetic agitation is 0.5 ~ 2h.
In step (4), described vacuum drying temperature is 40 ~ 60 DEG C, and drying time is 11 ~ 13h.
Product utilization transmission electron microscope (TEM) prepared by the present invention, SEM (SEM), Fourier infrared spectrograph (FT-IR) X-ray diffractometer (XRD) are analyzed the structure of product and pattern, be that dyestuff contaminant carries out photocatalytic degradation experiment with rhodamine B (RhB) solution, absorbance is measured, to probe into its photocatalytic activity by ultraviolet-visible spectrophotometer.
The photocatalytic activity experiment of pure silver carbonate and boron nitride/silver carbonate nano composite material:
(1) configuration concentration is rhodamine B (RhB) solution of 10mg/L, and the solution prepared is placed in dark place;
(2) silver carbonate and each 50mg of boron nitride/silver carbonate is taken, be placed in photo catalysis reactor respectively, then the rhodamine B solution of 50mL is added, dark place magnetic agitation 30min makes catalyst reach adsorption equilibrium (utilizing recirculated water to make the temperature of reaction remain on room temperature), open light source, carry out photocatalytic degradation;
(3) get the photocatalytic degradation liquid in 5mL reactor every 10min, centrifugal rear ultraviolet-visible spectrophotometer measures the absorbance of solution.
Method preparation technology of the present invention is simple, environmental pollution is little, safety coefficient is high, and the reaction time is short.The hexagonal boron nitride nanosheet of preparation as good catalyst carrier, can have great importance in concerted catalysis and stabilization of semiconductor.
Beneficial effect of the present invention is: the graphite-phase boron nitride of high-ratio surface effectively can improve the activity of silver carbonate photocatalytic pollutant degradation as carrier, the activity of its photocatalytic degradation rhodamine B is 1.24 times of simple silver carbonate, and the photoetch of silver carbonate photocatalytic semiconductor material can be reduced, improve its stability, have broad application prospects in photocatalysis field.
Method of the present invention is with urea and boric acid for raw material, and high-temperature calcination in vacuum tube furnace, obtains the hexagonal boron nitride nanosheet of graphite-phase.Then take hexagonal boron nitride as carrier, with silver nitrate, ammoniacal liquor and sodium acid carbonate for raw material, by the precipitation method, prepare hexagonal boron nitride/silver carbonate nano-particle compound.
Accompanying drawing explanation
The transmission electron microscope picture of the hexagonal boron nitride of Fig. 1 prepared by case study on implementation 1 and scanning electron microscope (SEM) photograph.
The infrared spectrogram of the hexagonal boron nitride of Fig. 2 prepared by case study on implementation 1.
The silver carbonate of Fig. 3 prepared by case study on implementation 1 and the scanning electron microscope (SEM) photograph of boron nitride/silver carbonate composite.
The EDS analysis result of Fig. 4 hexagonal boron nitride prepared by case study on implementation 1/silver carbonate composite.
The hexagonal boron nitride of Fig. 5 prepared by case study on implementation 1 and the XRD figure of boron nitride/silver carbonate composite.
Fig. 6 is the time m-degradation rate graph of a relation of pure silver carbonate and boron nitride/silver carbonate nano-complex photocatalytic degradation rhodamine B (RhB) solution.
Fig. 7 is that boron nitride/silver carbonate nano-complex photocatalytic degradation circulates the figure of the XRD after four times.
Detailed description of the invention
the preparation of case study on implementation 1 hexagonal boron nitride and boron nitride/silver carbonate nano composite material
Be the CO (NH of 24:1 by mol ratio
2)
2and H
3bO
4put into beaker, under ultrasonication, make it be dissolved in completely in deionized water, then 65 DEG C of water bath method solution under magnetic stirring, then the sample after evaporate to dryness is placed in alumina crucible, be placed in tube furnace, in the atmosphere of nitrogen, be warmed up to 900 DEG C with the speed of 5 DEG C/min, and keep 5h, after the temperature of tube furnace drops to room temperature, take out sample carry out grinding and obtain white boron nitride powder.
The graphite-phase boron nitride getting 0.015g is dispersed in deionized water under ultrasonication, then the silver nitrate of 0.6163g is added, homodisperse solution is obtained under ultrasonication, dropwise add the 0.5mol/L ammonia spirit of 1mL under magnetic stirring, after stirring 20min, the dropwise of the sodium acid carbonate being dissolved in the 0.1524g of deionized water is joined in above-mentioned solution, and Keep agitation 1 h, after having reacted, solution is carried out centrifugal, then after using deionized water and absolute ethanol washing repeatedly, dry 12h in 50 DEG C of vacuum drying chambers, then grinding obtains boron nitride/silver carbonate nano composite material.
the preparation of case study on implementation 2 hexagonal boron nitride and boron nitride/silver carbonate nano composite material
Be the CO (NH of 24:1 by mol ratio
2)
2and H
3bO
4put into beaker, under ultrasonication, make it be dissolved in completely in deionized water, then 65 DEG C of water bath method solution under magnetic stirring, then the sample after evaporate to dryness is placed in alumina crucible, be placed in tube furnace, in the atmosphere of nitrogen, be warmed up to 700 DEG C with the speed of 3 DEG C/min, and keep 3h, after the temperature of tube furnace drops to room temperature, take out sample carry out grinding and obtain white boron nitride powder.
The graphite-phase boron nitride getting 0.03g is dispersed in deionized water under ultrasonication, then the silver nitrate of 0.6163g is added, homodisperse solution is obtained under ultrasonication, dropwise add the 0.5mol/L ammonia spirit of 0.5mL under magnetic stirring, after stirring 20min, the dropwise of the sodium acid carbonate being dissolved in the 0.3081g of deionized water is joined in above-mentioned solution, and Keep agitation 1h, after having reacted, solution is carried out centrifugal, then after using deionized water and absolute ethanol washing repeatedly, dry 11h in 40 DEG C of vacuum drying chambers, then grinding obtains boron nitride/silver carbonate nano composite material.
the preparation of case study on implementation 3 hexagonal boron nitride and boron nitride/silver carbonate nano composite material
Be the CO (NH of 24:1 by mol ratio
2)
2and H
3bO
4put into beaker, under ultrasonication, make it be dissolved in completely in deionized water, then 65 DEG C of water bath method solution under magnetic stirring, then the sample after evaporate to dryness is placed in alumina crucible, be placed in tube furnace, in the atmosphere of nitrogen, be warmed up to 1100 DEG C with the speed of 8 DEG C/min, and keep 7h, after the temperature of tube furnace drops to room temperature, take out sample carry out grinding and obtain white boron nitride powder.
The graphite-phase boron nitride getting 0.0088g is dispersed in deionized water under ultrasonication, then the silver nitrate of 0.6163g is added, homodisperse solution is obtained under ultrasonication, dropwise add the 0.5mol/L ammonia spirit of 1.5mL under magnetic stirring, after stirring 20min, the dropwise of the sodium acid carbonate being dissolved in the 0.1027g of deionized water is joined in above-mentioned solution, and Keep agitation 0.5h, after having reacted, solution is carried out centrifugal, then after using deionized water and absolute ethanol washing repeatedly, dry 13h in 60 DEG C of vacuum drying chambers, then grinding obtains boron nitride/silver carbonate nano composite material.
the preparation of case study on implementation 4 hexagonal boron nitride and boron nitride/silver carbonate nano composite material
Be the CO (NH of 24:1 by mol ratio
2)
2and H
3bO
4put into beaker, under ultrasonication, make it be dissolved in completely in deionized water, then 65 DEG C of water bath method solution under magnetic stirring, then the sample after evaporate to dryness is placed in alumina crucible, be placed in tube furnace, in the atmosphere of nitrogen, be warmed up to 8000 DEG C with the speed of 4 DEG C/min, and keep 4h, after the temperature of tube furnace drops to room temperature, take out sample carry out grinding and obtain white boron nitride powder.
The graphite-phase boron nitride getting 0.0123g is dispersed in deionized water under ultrasonication, then the silver nitrate of 0.6163g is added, homodisperse solution is obtained under ultrasonication, dropwise add the 0.5mol/L ammonia spirit of 2.5mL under magnetic stirring, after stirring 20min, the dropwise of the sodium acid carbonate being dissolved in the 0.2054g of deionized water is joined in above-mentioned solution, and Keep agitation 1h, after having reacted, solution is carried out centrifugal, then after using deionized water and absolute ethanol washing repeatedly, dry 13h in 40 DEG C of vacuum drying chambers, then grinding obtains boron nitride/silver carbonate nano composite material.
the preparation of case study on implementation 5 hexagonal boron nitride and boron nitride/silver carbonate nano composite material
Be the CO (NH of 24:1 by mol ratio
2)
2and H
3bO
4put into beaker, under ultrasonication, make it be dissolved in completely in deionized water, then 65 DEG C of water bath method solution under magnetic stirring, then the sample after evaporate to dryness is placed in alumina crucible, be placed in tube furnace, in the atmosphere of nitrogen, be warmed up to 1000 DEG C with the speed of 6 DEG C/min, and keep 6h, after the temperature of tube furnace drops to room temperature, take out sample carry out grinding and obtain white boron nitride powder.
The graphite-phase boron nitride getting 0.0103g is dispersed in deionized water under ultrasonication, then the silver nitrate of 0.6163g is added, homodisperse solution is obtained under ultrasonication, dropwise add the 0.5mol/L ammonia spirit of 3mL under magnetic stirring, after stirring 20min, the dropwise of the sodium acid carbonate being dissolved in the 0.1233g of deionized water is joined in above-mentioned solution, and Keep agitation 2h, after having reacted, solution is carried out centrifugal, then after using deionized water and absolute ethanol washing repeatedly, dry 11h in 60 DEG C of vacuum drying chambers, then grinding obtains boron nitride/silver carbonate nano composite material.
Fig. 1 is transmission and the scanning electron microscope (SEM) photograph of hexagonal boron nitride carrier, and as can be seen from the figure, hexagonal boron nitride is a kind of nanometer sheet of similar Graphene layer structure;
Fig. 2 is the infrared spectrogram of hexagonal boron nitride, the 1387cm in figure
-1, 801cm
-1the absworption peak at place is the characteristic peak belonging to boron nitride;
Fig. 3 is the scanning electron microscope (SEM) photograph of silver carbonate and hexagonal boron nitride/silver carbonate, and as can be seen from the figure silver carbonate particle dispersion is better, and the size of particle is between 0.5 ~ 1 μm, hexagonal boron nitride and silver carbonate compound fine;
Fig. 4 is the analysis result of the EDS of the nano composite material of hexagonal boron nitride/silver carbonate, and this composite of surface is made up of boron, nitrogen, silver, carbon, oxygen element;
Fig. 5 is XRD figure, (100), (110), (-101) in figure, (130), (202), (031) crystal face belong to the characteristic diffraction peak of silver carbonate, the characteristic diffraction peak belonging to hexagonal boron nitride of (002) crystal face;
As can be seen from Fig. 6, the catalytic activity of the hexagonal boron nitride prepared using the graphite-phase hexagonal boron nitride of high-ratio surface as carrier/silver carbonate nano composite material photocatalytic degradation rhodamine B is 1.24 times of pure silver carbonate nano material;
Can find out after recycling hexagonal boron nitride/silver carbonate nano composite material in Fig. 7, there is not obvious change in the peak of its XRD, illustrate that graphite-phase hexagonal boron nitride is as carrier, namely the recombination rate of photo-generate electron-hole can be reduced, the photoetch of silver carbonate can be suppressed again, thus the ability that raising silver carbonate pollutes at photocatalytic degradation.
Described embodiment is preferred embodiment of the present invention; but the present invention is not limited to above-mentioned embodiment; when not deviating from flesh and blood of the present invention, any apparent improvement that those skilled in the art can make, replacement or modification all belong to protection scope of the present invention.
Claims (10)
1. a preparation method for silver carbonate semiconductor stablized by hexagonal boron nitride ceramic material, it is characterized in that, comprises the steps:
(1) graphite-phase hexagonal boron nitride nanosheet is prepared:
Weigh CO (NH
2)
2and H
3bO
4in beaker, under ultrasonication, make it be dissolved in completely in deionized water, then water bath method solution under magnetic stirring, be placed in alumina crucible by sample after evaporate to dryness, and be placed in tube furnace, atmosphere of inert gases Program is warming up to calcining heat, after calcining terminates, after Temperature fall to room temperature, grinding, obtains graphite-phase boron nitride;
(2) graphite-phase boron nitride step (1) prepared is ultrasonic to be dispersed in ionized water, then adds silver nitrate, under ultrasonication, obtain homodisperse solution A;
(3) in solution A, dropwise add the ammonia spirit of 0.5mol/L, stir 20min obtained solution B under magnetic stirring simultaneously;
(4) sodium bicarbonate solution being dissolved in deionized water is dropwise joined in solution B, produce yellow mercury oxide, and Keep agitation under magnetic stirring, then centrifugal, obtain boron nitride/silver carbonate composite precipitation, with deionized water and absolute ethanol washing, centrifugal, vacuum drying, then grinding obtains boron nitride/silver carbonate nano-complex.
2. preparation method according to claim 1, is characterized in that, in step (1), and described CO (NH
2)
2and H
3bO
4the ratio of amount of substance be 24:1, described bath temperature is 65 DEG C.
3. preparation method according to claim 1, is characterized in that, in step (1), described inert gas is nitrogen or argon gas, and the speed of described temperature programming is 3 ~ 8 DEG C/min, and described calcining heat is 700 ~ 1100 DEG C, and calcination time is 3 ~ 7h.
4. preparation method according to claim 1, is characterized in that, in step (1), described inert gas is nitrogen or argon gas, and the speed of described temperature programming is 4 ~ 7 DEG C/min, and calcining heat is 700 ~ 1000 DEG C, and the time of maintenance is 3 ~ 6h.
5. preparation method according to claim 1, is characterized in that, in step (1), described inert gas is nitrogen or argon gas, and the speed of described temperature programming is 4 ~ 6 DEG C/min, and calcining heat is 800 ~ 1000 DEG C, and the time of maintenance is 4 ~ 6h.
6. preparation method according to claim 1, it is characterized in that, in step (2), the mass ratio of described boron nitride and silver nitrate is 1:20 ~ 1:70, in step (3), the volume of described ammonia spirit is 0.5 ~ 3mL, and in step (4), the mass ratio of described silver nitrate and sodium acid carbonate is 2:1 ~ 6:1.
7. preparation method according to claim 1, is characterized in that, in step (2), the mass ratio of described boron nitride and silver nitrate is 1:30 ~ 1:60, and in step (3), the volume of ammonia spirit is 0.5 ~ 2mL, in step (4), the mass ratio of described silver nitrate and sodium acid carbonate is 3:1 ~ 6:1.
8. preparation method according to claim 1, it is characterized in that, in step (2), the mass ratio of described boron nitride and silver nitrate is 1:40 ~ 1:50, in step (3), the volume of ammonia spirit is 0.5 ~ 1.5mL, and in step (4), the mass ratio of described silver nitrate and sodium acid carbonate is 3:1 ~ 5:1.
9. preparation method according to claim 1, is characterized in that, in step (4), the time of described magnetic agitation is 0.5 ~ 2h.
10. preparation method according to claim 1, is characterized in that, in step (4), described vacuum drying temperature is 40 ~ 60 DEG C, and drying time is 11 ~ 13h.
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| CN106674603A (en) * | 2016-12-29 | 2017-05-17 | 中国科学院深圳先进技术研究院 | Heat-conducting hexagonal boron nitride hybrid material as well as preparation method and application thereof |
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| CN110302817A (en) * | 2019-06-06 | 2019-10-08 | 广东工业大学 | A kind of foamed nickel supported silver carbonate composite photocatalyst material and its preparation method and application |
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| CN106732727A (en) * | 2016-12-26 | 2017-05-31 | 湖南大学 | Hexagonal boron nitride modification graphitization nitridation carbon composite photocatalyst and its preparation method and application |
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| CN107934930A (en) * | 2017-12-15 | 2018-04-20 | 中霖中科环境科技（安徽）股份有限公司 | A kind of low-temperature synthetic method for efficiently removing the boron nitride nanosheet of lead ion in water removal |
| CN110302817A (en) * | 2019-06-06 | 2019-10-08 | 广东工业大学 | A kind of foamed nickel supported silver carbonate composite photocatalyst material and its preparation method and application |
| CN110721658A (en) * | 2019-10-15 | 2020-01-24 | 江苏索普（集团）有限公司 | Preparation method and application of hexagonal boron nitride-graphite phase carbon nitride intercalation composite material |
| CN110721658B (en) * | 2019-10-15 | 2022-06-10 | 江苏索普（集团）有限公司 | Preparation method and application of hexagonal boron nitride-graphite phase carbon nitride intercalation composite material |
| CN112551964A (en) * | 2021-01-15 | 2021-03-26 | 福州大学 | Antibacterial cement mortar and preparation and application methods thereof |
| CN112551964B (en) * | 2021-01-15 | 2021-11-30 | 福州大学 | Antibacterial cement mortar and preparation and application methods thereof |
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Application publication date: 20150826 |