CN105858730B - A kind of carbonitride/tungsten oxide compound hollow microballoon and preparation method thereof - Google Patents
A kind of carbonitride/tungsten oxide compound hollow microballoon and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of carbonitride/tungsten oxide compound hollow microballoon and preparation method thereof, the microballoon is the hollow ball shell collectively formed by carbonitride, tungsten oxide；The microballoon, as raw material, is sintered carbon ball as stay in place form using glucose, is prepared from by hydro-thermal method and high-temperature calcination using tungstates and carbon nitride precursor.Carbonitride/tungsten oxide compound hollow microballoon of the present invention has hollow lumen, shell is uniformly made up of carbonitride with tungsten oxide with certain proportion simultaneously, show good homogeneity, tiny balloon has bigger specific surface area, hollow lumen can provide more electromagnetic transmission reflection paths, and improving material, emittance absorbs ability to external world.
Description
Technical field
The invention belongs to semiconductor composite technical field, and in particular to a kind of carbonitride/tungsten oxide composite hollow is micro-
Ball and preparation method thereof.
Background technology
Tungsten oxide inorganic semiconductor material has obtained the extensive concern of people because of its unique physicochemical properties.Mesh
Before, tungsten oxide semiconductor has been obtained specifically in fields such as photocatalysis, photochromic, air-sensitive, electrochromism and Flied emissions
Using.Researcher can prepare the tungsten oxide micro Nano material of a variety of different sizes and pattern, such as nanometer by all means
Piece, nanometer rods and hollow ball etc..Wherein, hollow ball tungsten oxide is received much concern with its unique pattern, and it has higher ratio
The advantages of surface area, excellent weight capacity and low-density, this causes tungsten oxide to have more wide application space.It is used as one
Kind of n-type semiconductor, tungsten oxide has certain photocatalytic activity, and narrower energy gap can make it by excited by visible light, its
Valence band (VB) uppermost edge and TiO2It is close, exceed H2O/O2Oxidation potential, therefore, produced by tungsten oxide bandgap excitation
Photohole can aoxidize many organic matters.It is too low yet with the conduction band current potential of tungsten oxide, light induced electron be easy to in air
O2Reaction, causes the decline of its photocatalytic activity.In order to further improve the physics and chemical property of tungsten oxide, pass through pattern
Regulation and control, element doping and compound from different semi-conducting materials, the study hotspot as tungsten oxide material in recent years.
Patent CN102161510A discloses a kind of preparation method of hollow porous tungsten oxide sphere, and this method is by wolframic acid
Ammonium, ammonium metatungstate are configured to solution, and ammonium tungstate, ammonium metatungstate or its mixture are prepared using spray drying device spray drying
Hollow powder, this powder is put into electric furnace and heats obtained hollow POROUS TUNGSTEN ball.But tungsten oxide ball preparation technology is complicated, and need
Want special spray-drying installation.Patent CN102266783A discloses a kind of Fe2O3 doping tungsten trioxide photocatalyst and its preparation
Method, using the compound of tungstenic and iron content as precursor, by the way that both are mixed, the process such as grinding, high-temperature calcination makes raw material most
WO is converted into eventually3With the form of iron oxide, the tungstic acid of Fe2O3 doping is made, but the composite specific surface area of the method is smaller,
Pattern does not have outstanding feature, and visible light-responded indifferent.
The content of the invention
It is an object of the invention to provide one carbonitride/tungsten oxide compound hollow microballoon and preparation method thereof, prepared by the microballoon
Technique is simple, controllable, with higher specific surface area and good visible light-responded property, can be applied to photocatalytic degradation pollution
The multiple fields such as thing, photovoltaic cell, solar cell.
Realizing the technical solution of the object of the invention is：A kind of carbonitride/tungsten oxide compound hollow microballoon, the microballoon
It is the hollow ball shell Rotating fields collectively formed by carbonitride, tungsten oxide.
Wherein, the content of carbonitride is 5-10wt% in described microballoon.
The preparation method of above-mentioned compound hollow microballoon, using tungstates and carbon nitride precursor as raw material, with glucose
Sintering carbon ball is stay in place form, is prepared from by hydro-thermal method and high-temperature calcination, it is concretely comprised the following steps：
It is 20 that step a), which is added in 0.02~0.05mol/L wolframic acid saline solutions with tungstates mol ratio,:1~30:1
Glucose and with tungstates mol ratio be 2:1~8:1 carbon nitride precursor, stirs 0.5~1h, is uniformly mixed molten
Liquid；
Step b) is by the mixed solution of gained in step a) in 16~24h of hydro-thermal reaction, natural cooling at 180-200 DEG C
To room temperature, centrifuge, washing, and in being dried in vacuo 6~12h at 60 ± 10 DEG C, obtain carbonitride/tungsten oxide and be combined carbon ball；
Carbonitride/tungsten oxide of gained in step b) is combined carbon ball in 2~5h of calcining at 500~550 DEG C by step c),
Room temperature is naturally cooled to, carbonitride/tungsten oxide compound hollow microballoon material is obtained.
Step a）In, described tungstates is one kind in sodium tungstate, ammonium tungstate, and described carbon nitride precursor is trimerization
One kind in cyanamide, dicyanodiamine, cyanamide, urea.
Step b）In, heating rate is 2 DEG C/min.
Step c）In, heating rate is 2~6 DEG C/min.
Compared with prior art, the beneficial effects of the invention are as follows：
（1）The present invention is compound in carbon ball surface using the presoma of tungstates and carbonitride by hydro-thermal reaction, finally leads to
Cross calcining and remove carbon ball template acquisition hollow ball structure, preparation process is simple, controllable.
（2）Carbonitride/tungsten oxide compound hollow microballoon of the present invention has hollow lumen, and shell is simultaneously by carbonitride and oxygen
Change tungsten uniformly to be constituted with certain proportion, show good homogeneity, tiny balloon has bigger specific surface area, hollow lumen energy
Enough provide more electromagnetic transmission reflection paths, improving material, emittance absorbs ability to external world.
（3）Two kinds of semiconductors of carbonitride and tungsten oxide are uniformly contacted in shell, form typical heterojunction semiconductor knot
Structure, can improve material to the response range of light and the separative efficiency of photo-generated carrier, and then can significantly improve the photoelectricity of material
Performance.
The present invention is described in further detail below in conjunction with the accompanying drawings.
Brief description of the drawings
Fig. 1 is the preparation flow figure of carbonitride/tungsten oxide compound hollow microballoon.
Fig. 2 is the SEM photograph of the gained carbonitride of embodiment 5/tungsten oxide compound hollow microballoon different-shape（A is complete, b
Breach）.
Fig. 3 is the TEM photos under the gained carbonitride of embodiment 5/tungsten oxide compound hollow microballoon different multiples（a 40000
Times, 10 0000 times of b).
Fig. 4 is the XRD spectra of 5 carbonitrides of embodiment/tungsten oxide compound hollow microballoon.
Fig. 5 is the FTIR spectrograms of 5 carbonitrides of embodiment/tungsten oxide compound hollow microballoon.
Embodiment
The following examples can make those skilled in the art that the present invention is more fully understood.
Embodiment 1
By 0.330g (1.0mmol) Na2WO4·2H2O, 4.504g (25mmol) glucose and 0.336g (8mmol)
Cyanamide is dissolved in 50ml deionized waters, ultrasound, stirring 30min formation homogeneous solutions.Above-mentioned middle mixed solution is transferred to not
Become rusty in steel water heating kettle, 200 DEG C are warming up to 2 DEG C/min in Muffle furnace, be incubated 20 hours.After natural cooling, centrifugation, with steaming
It is dried in vacuo at distilled water and absolute ethyl alcohol cyclic washing 3 times, 60 DEG C, obtains WO3- CN is combined carbon ball.By obtained compound carbon ball
500 DEG C are heated to 2 DEG C/min in tube furnace, 2 hours are calcined, natural cooling finally gives carbonitride/tungsten oxide
Compound hollow microballoon.
Embodiment 2
By 0.330g (1.0mmol) Na2WO4·2H2O, 4.504g (25mmol) glucose and 0.252g (2mmol)
Melamine is dissolved in 50ml deionized waters, ultrasound, stirring 30min formation homogeneous solutions.Above-mentioned middle mixed solution is transferred to
In stainless steel water heating kettle, 200 DEG C are warming up to 2 DEG C/min in Muffle furnace, 20 hours are incubated.After natural cooling, centrifuge, use
It is dried in vacuo at distilled water and absolute ethyl alcohol cyclic washing 5 times, 60 DEG C, obtains WO3- CN is combined carbon ball.By obtained composite carbon
Ball is heated to 500 DEG C in tube furnace with 5 DEG C/min, calcines 2 hours, and natural cooling finally gives carbonitride/oxidation
Tungsten compound hollow microballoon.
Embodiment 3
By 0.330g (1.0mmol) Na2WO4·2H2O, 4.504g (25mmol) glucose and 0.481g (8mmol)
Urea is dissolved in 50ml deionized waters, ultrasound, stirring 30min formation homogeneous solutions.Above-mentioned middle mixed solution is transferred to stainless
In steel water heating kettle, 200 DEG C are warming up to 2 DEG C/min in Muffle furnace, 24 hours are incubated.After natural cooling, centrifugation, with distillation
It is dried in vacuo at water and absolute ethyl alcohol cyclic washing 4 times, 60 DEG C, obtains WO3- CN is combined carbon ball.Obtained compound carbon ball is existed
550 DEG C are heated to 5 DEG C/min in tube furnace, 5 hours are calcined, natural cooling finally gives carbonitride/tungsten oxide multiple
Close tiny balloon.
Embodiment 4
By 0.380g (0.125mmol) (NH4)10W12O41, 4.504g (25mmol) glucose and 0.481g
(8mmol) urea is dissolved in 50ml deionized waters, ultrasound, stirring 30min formation homogeneous solutions.Above-mentioned middle mixed solution is shifted
Into stainless steel water heating kettle, 200 DEG C are warming up to 2 DEG C/min in Muffle furnace, 18 hours are incubated.After natural cooling, centrifugation,
It is dried in vacuo with distilled water and absolute ethyl alcohol cyclic washing 5 times, 60 DEG C, obtains WO3- CN is combined carbon ball.It is compound by what is obtained
Carbon ball is heated to 500 DEG C in tube furnace with 2 DEG C/min, calcines 2 hours, and natural cooling finally gives carbonitride/oxygen
Change tungsten compound hollow microballoon.
Embodiment 5
By 0.330g (1.0mmol) Na2WO4·2H2O, 4.504g (25mmol) glucose and 0.336g (4mmol)
Dicyanodiamine is dissolved in 50ml deionized waters, ultrasound, stirring 30min formation homogeneous solutions.Above-mentioned middle mixed solution is transferred to
In stainless steel water heating kettle, 200 DEG C are warming up to 2 DEG C/min in Muffle furnace, 20 hours are incubated.After natural cooling, centrifuge, use
It is dried in vacuo at distilled water and absolute ethyl alcohol cyclic washing 3 times, 60 DEG C, obtains WO3- CN is combined carbon ball.By obtained composite carbon
Ball is heated to 550 DEG C in tube furnace with 2 DEG C/min, calcines 2 hours, and natural cooling finally gives carbonitride/oxidation
Tungsten compound hollow microballoon.
Fig. 2 is the SEM photograph of carbonitride/tungsten oxide compound hollow microballoon, can be seen that carbonitride/tungsten oxide is combined by Fig. 2 a
Tiny balloon rough surface, microsphere diameter is 3 μm of 1-, can be seen that microballoon has hollow structure by Fig. 2 b, shell is by largely receiving
Rice grain is constituted, wall thickness 300nm or so.Analyzed through EDS, microballoon top layer is made up of tetra- kinds of elements of C, N, O, W, and wherein carbonitride contains
Amount is in 5wt% or so.
Fig. 3 is the TEM photos of carbonitride/tungsten oxide compound hollow microballoon, it can be seen that micro-sphere structure is complete, diameter 1- 3
μm, and microballoon has obvious hollow-core construction, and wall thickness is 300nm or so.
Fig. 4 is WO in the XRD spectra of carbonitride/tungsten oxide compound hollow microballoon, figure3Each diffraction maximum and pure WO3Spread out
Penetrate peak almost completely the same, be g-C at 14.1 ° and 27.4 °3N4Two characteristic diffraction peaks, wherein at 14.1 ° diffraction maximum correspondence
In（100）Crystal face, is seven piperazine architectural feature peak in layer, 27.4 ° of correspondences（002）Crystal face, is interlayer stacking characteristic peak, is seen by spectrogram
Go out, characteristic peak is weaker less substantially at 14.1 °, has smaller spike to occur at 27.4 °.The XRD spectra show the composite by
WO3And g-C3N4Collectively constitute.
Fig. 5 is the FTIR spectrograms of carbonitride/tungsten oxide compound hollow microballoon, and figure is in 600-800cm-1、1000-1500cm-1With 2800-3400 cm -1Absorption band is occurred in that at three.Wherein in 600-800 cm-1Strong absworption peak be WO3Feature is inhaled
Receive peak and composition g-C3N4Unit triazine carbon azo-cycle flexural vibrations characteristic peak；1000-1500 cm-1's
Weak absorbing band, then be g-C3N4 Carbon azacyclo- on C=N, C- N and the outer C-N stretching vibration absworption peaks of ring；And
In 2800-3400 cm-1Absorption band be probably then g-C3N4NH and NH on edge breakage aromatic rings 2Base
Group stretching vibration, or the hydrone of its Adsorption on Surface stretching vibration.
Claims (5)
1. a kind of preparation method of carbonitride/tungsten oxide compound hollow microballoon, it is characterised in that its step is：
It is 20 that step a), which is added in 0.02~0.05mol/L wolframic acid saline solutions with tungstates mol ratio,:1~30:1 Portugal
Grape are sugared and are 2 with tungstates mol ratio:1~8:1 carbon nitride precursor, stirs 0.5~1h, obtains uniform mixed solution；
The mixed solution of gained in step a) in 16~24h of hydro-thermal reaction at 180-200 DEG C, is naturally cooled to room by step b)
Temperature, is centrifuged, washing, and in being dried in vacuo 6~12h at 60 ± 10 DEG C, is obtained carbonitride/tungsten oxide and be combined carbon ball；
Carbonitride/tungsten oxide of gained in step b) is combined carbon ball in calcining 2~5h at 500~550 DEG C by step c), natural
Room temperature is cooled to, carbonitride/tungsten oxide compound hollow microballoon material is obtained.
2. preparation method as claimed in claim 1, it is characterised in that step a）In, described tungstates is sodium tungstate, wolframic acid
One kind in ammonium.
3. preparation method as claimed in claim 1, it is characterised in that step a）In, described carbon nitride precursor is trimerization
One kind in cyanamide, dicyanodiamine, cyanamide, urea.
4. preparation method as claimed in claim 1, it is characterised in that step b）In, heating rate is 2 DEG C/min.
5. preparation method as claimed in claim 1, it is characterised in that step c）In, heating rate is 2~6 DEG C/min.
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| CN106311217B (en) * | 2016-08-19 | 2020-04-17 | 浙江师范大学 | Preparation method of activated carbon functionalized tungsten oxide |
| CN106602023B (en) * | 2016-12-26 | 2019-07-12 | 武汉理工大学 | A kind of method of fabricated in situ graphite phase carbon nitride-oxidation carbon/carbon-copper composite material |
| CN106975476A (en) * | 2017-04-24 | 2017-07-25 | 陕西科技大学 | A kind of efficient tungstic acid microsphere photocatalyst and preparation method thereof |
| CN107999110A (en) * | 2017-11-14 | 2018-05-08 | 肇庆市华师大光电产业研究院 | A kind of Lacking oxygen tungsten oxide/nitridation carbon composite photocatalyst and its preparation method and application |
| CN108313989B (en) * | 2018-02-11 | 2021-08-10 | 济南大学 | Preparation method of mushroom-like pleated carbon nitride microspheres and obtained product |
| CN111889122B (en) * | 2019-05-06 | 2021-07-27 | 天津大学 | Tungsten trioxide/graphite phase carbon nitride composite material and preparation method thereof |
| CN111889121B (en) * | 2019-05-06 | 2021-07-27 | 天津大学 | Application of tungsten trioxide/graphite phase carbon nitride composite material in degradation CIP |
| CN110545652B (en) * | 2019-07-26 | 2020-12-18 | 郑州航空工业管理学院 | Co/CoO-C composite material with porous structure and preparation method and application thereof |
| CN111068730B (en) * | 2019-11-29 | 2021-08-24 | 东南大学 | Graphite-like hollow microsphere photocatalyst and preparation method and application method thereof |
| CN111054421B (en) * | 2020-01-06 | 2021-08-24 | 东南大学 | Graphite-like carbon nitride doped modified microsphere catalyst and preparation method and application thereof |
| CN111408397A (en) * | 2020-03-30 | 2020-07-14 | 浙江工商大学 | Modified carbon nitride and tungsten oxide coupled p-n type heterojunction composite material and preparation method and application thereof |
| CN111977689A (en) * | 2020-07-09 | 2020-11-24 | 南阳师范学院 | Niobium pentoxide microsphere with hollow structure and preparation method and application thereof |
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