CN104108682A - Visible-light responsive germanium hydride and preparation method and application thereof - Google Patents
Visible-light responsive germanium hydride and preparation method and application thereof Download PDFInfo
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- CN104108682A CN104108682A CN201410356275.9A CN201410356275A CN104108682A CN 104108682 A CN104108682 A CN 104108682A CN 201410356275 A CN201410356275 A CN 201410356275A CN 104108682 A CN104108682 A CN 104108682A
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Abstract
The invention relates to visible-light responsive germanium hydride and a preparation method and an application thereof. The preparation method comprises the following steps of: firstly, synthesizing calcium germanide crystals by utilizing a molten cosolvent method; then, performing ion exchange to obtain a final product, namely germanium hydride. The synthesized germanium hydride has a nanoscale laminated structure, and the formed germanium hydride photocatalyst is high in absorptive capacity in a visible light area and high in photocatalytic activity in hydrogen production and degradation of organic pollutants utilizing photocatalysis.
Description
Technical field
The present invention relates to a kind of novel photocatalysis material, particularly a kind of have visible light-responded germanium hydride and its preparation method and application.
Background technology
In recent years, along with the aggravation of global energy crisis and environmental pollution, Hydrogen Energy, as the effective carrier of sun power, can effectively solve the problems such as sun power storage and transport.Since 1972, Fijishima and Honda reported at N-shaped semi-conductor TiO
2on Single Crystalline Electrodes, photic water of decomposition produces H
2and O
2, utilize sun power to carry out the research that photochemical catalyzing produces clean, efficient and reproducible hydrogen and be more and more subject to global extensive concern.Utilize semiconductor light-catalyst to become electric energy and chemical energy to become in recent years one of most active research field in the world light energy conversion.Wherein photocatalytic hydrogen production by water decomposition causes countries in the world scientist's extensive concern with its unique advantage, and it is carried out widely to theory and experimental study will have very important strategy and realistic meaning.
But, visible ray accounts for 43% left and right in solar spectrum, much larger than UV-light (3～4%) proportion, therefore, research and develop visible light-responded photocatalyst and fully efficiently utilize solar hydrogen making to become the emphasis that current researchers study, having more practical significance.
The research of germanium hydride is applied in becomes a study hotspot in recent years." american chemical association " (ACS Nano, 2013,4414-4421), (ACS Nano, 2013,2898-2926) and " chemical physics magazine " (THE JOURNAL OF CHEMICAL PHYSICS, 2013,124709-5) report that germanium hydride is that a kind of hydrogen is the Multi-layer graphite alkane analogue of the germanium of terminal, and there is the direct band gap of 1.53eV.Therefore, germanium hydride is applied to photocatalysis field and there is important practical application meaning.
Summary of the invention
The object of this invention is to provide a kind of visible light-responded germanium hydride and its preparation method and application that has, this material has very strong absorption in visible region, and there is stronger photocatalytic activity, comprise photocatalysis Decomposition aquatic products hydrogen and photocatalytically degradating organic dye rhodamine B.
The technical scheme that the present invention takes is as follows:
There is a preparation method for visible light-responded germanium hydride, comprise that step is as follows:
1) utilize melting solubility promoter growing crystal method to synthesize presoma germanium calcium: in the glove box that is full of argon gas, be that Ca:Ge:Pb=0.7～1.5:2:20～25 weigh above-mentioned three kinds of simple substance according to the mol ratio of Ca, Ge, Pb, after mixing, put into alumina crucible, and alumina crucible is sealed in quartz glass tube by high vacuum line operative technique (vacuum-line), process furnace was warming up to system 1000 DEG C and be incubated 18-22 hour in 4 hours, be cooled to 600 DEG C with the speed of 3-7 per hour DEG C again, insulation 10-15 hour; Subsequently Glass tubing is taken out, be inverted into and centrifugal in whizzer melting solubility promoter lead is separated and collected, under the microscope in glove box, pick out tabular crystal presoma germanium calcium;
2) described presoma germanium calcium is reacted to 24-48h with concentrated hydrochloric acid in the cryogenic thermostat ethanol bath of-30 DEG C, naturally return to room temperature, centrifugation, washing, dry and obtain.
Preferably, described molar ratio pass is Ca:Ge=1:2.
The described centrifugal speed of step (1) is turn/min of 3000-3500.
In step (2), the ratio of presoma germanium calcium and concentrated hydrochloric acid is 0.2:100, g/ml; The mass concentration of concentrated hydrochloric acid is 37%.What aforesaid method made has visible light-responded germanium hydride, has laminate structure.Under visible ray, hydrogen-producing speed is 22 μ molh
-1g
-1.
The described visible light-responded germanium hydride that has produces the application in hydrogen as catalyzer at visible light catalytic water of decomposition.
A kind of germanium hydride photocatalyst, contains the above-mentioned visible light-responded germanium hydride that has, and makes under illumination.
The preparation method of described a kind of germanium hydride photocatalyst: described germanium hydride sample is joined in the mixing solutions of deionized water and methyl alcohol, and the noble metal platinum of load germanium hydride quality 1.0 wt%, under constantly stirring, irradiate 0.5-1 hour with 300W xenon lamp and obtain.
Described deionized water, methanol usage is every 50mg germanium hydride sample, uses 20-30 ml deionized water, 20-25 ml methanol.
The application of visible light responsible photocatalytic material germanium hydride of the present invention, the removal of application photocatalysis Decomposition aquatic products hydrogen and air, waste water, surface water or Organic Pollutants of Drinking Water.
Excellent results of the present invention is as follows:
1. photocatalyst material germanium hydride of the present invention has laminate structure, and this photocatalyst material is visible light-responded.
2. the present invention, by ion-exchange techniques, is exchanged into hydrogen by the calcium in germanium calcium, and reaction forms germanium hydride.
3. the germanium hydride photocatalyst material that obtained, demonstrates good photocatalytic activity, can decompose aquatic products hydrogen 135umol at 6 hours, 82% the rhodamine B organic dye of degrading in 4 minutes.
4. it is controlled that photocatalyst material of the present invention is prepared synthetic method condition, has higher commercial applications prospect.
Through experimental studies have found that germanium hydride demonstrates good photocatalysis performance, the photocatalyst making for photocatalysis Decomposition aquatic products hydrogen decomposes aquatic products hydrogen 135 umol for 6 hours at radiation of visible light.Can degrade in 4 minutes 82% rhodamine B organic dye.Comparatively speaking photocatalyst rhodamine B degradation 70% in 30 minutes that, nitrogen doping P25 forms.Therefore compared with the P25 adulterating with N in photocatalytic applications with the synthetic germanium hydride of ion-exchange, there is higher activity.
Brief description of the drawings
Fig. 1 is the X ray picture of the embodiment of the present invention 1 presoma;
Fig. 2 is the X ray picture of the embodiment of the present invention 1 product;
Fig. 3 is the SEM figure of the embodiment of the present invention 1 product;
Fig. 4 is photocatalyst and nitrogen that the embodiment of the present invention 1 product the forms comparison diagram of P25 for photocatalytically degradating organic dye rhodamine B that adulterate;
Fig. 5 be the embodiment of the present invention 1 product form photocatalyst for photocatalysis Decomposition aquatic products hydrogen output figure;
Fig. 6 is the X ray picture of the embodiment of the present invention 2 products;
Fig. 7 is the SEM figure of the embodiment of the present invention 2 products.
Embodiment
To being described further in the present invention, but be not limited to this below in conjunction with accompanying drawing.
In embodiment, prepared material is carried out to the method for photocatalytic activity test as follows:
The test of photocatalysis Decomposition aquatic products hydrogen is carried out and is carried out in the Glass Containers system that is connected with recirculated cooling water (5 DEG C) sealing, and vacuum condition is-97 KPa.The light source irradiating at top is selected the 300 W xenon lamps that spectral filter is housed, and makes optical source wavelength be greater than 420nm.First sample is carried out to carried noble metal platinum (1.0 wt%).Take 50 mg sample dispersion in 30 ml water and 20 ml methyl alcohol, measure 33 ul platinum acid chloride solutions (0.0772 mM), under constantly stirring, irradiate and make for 30 minutes with 300W xenon lamp.Before the test of photocatalysis Decomposition aquatic products hydrogen, lucifuge magnetic agitation 1 h, gets rid of the interference of residual gas.Subsequently, add that spectral filter (λ >=420 nm) carries out illumination.After logical light, test every 1h, the peak area value being recorded by gas chromatograph is converted into the output of hydrogen.
Photocatalytically degradating organic dye test (transverse section 30 cm in glass beaker
2, high 5 cm) carry out under normal temperature and pressure.Light source is selected the 300 W xenon lamps that spectral filter is housed, and makes optical source wavelength be greater than 420nm.Carry out the photocatalytic activity of assess sample with rhodamine B.Take 50 mg germanium hydride sample dispersion in 50 ml rhodamine B solution (20 mg/L).Before light-catalyzed reaction test, lucifuge magnetic agitation 30 min make rhodamine B reach adsorption equilibrium at catalyst surface, after logical light, sample 5 ml every 2 min, and centrifugation, gets supernatant liquor measurement of ultraviolet-visible spectrophotometer absorbancy.
Embodiment 1
Take Ca:0.0401g, Ge:01452g, Pb:5.1807g puts into approximately 2 cm
3alumina crucible in, and alumina crucible is sealed in quartz glass tube by high vacuum line operative technique (vacuum-line), system is warming up to 1000 DEG C and be incubated 20 hours in 4 hours with experiment box-type furnace, to ensure that raw material fully reacts; Be cooled to 600 DEG C with 3 DEG C per hour again, be incubated 10 hours; Subsequently Glass tubing is taken out, be inverted in whizzer, the rotating speed turning with per minute 3,500 is separated melting solubility promoter lead collect.Under microscope in glove box, pick out the sheet germanium calcium crystal 0.2 of crystal type high-quality, react ethanol bath with cryogenic thermostat and reacting 48 hours (temperature of reaction is subzero 30 DEG C) with 100 ml concentrated hydrochloric acids under constantly stirring, treat that nature is warming up to room temperature and carries out suction filtration, wash with methyl alcohol and deionized water, and within 8 hours, obtain final product germanium hydride at vacuum drying oven inner drying under room temperature.
Accompanying drawing 1 is the X-ray diffractogram of the present embodiment gained presoma germanium calcium, as seen from the figure, except existing the assorted peak of metal promoted solvent lead, the each diffraction peak of this presoma germanium calcium is all corresponding with the peak position on the standard card (JCPDS file no.13-299) of trigonal system germanium calcium, and diffraction peak is stronger, illustrate that product is the germanium calcium crystal that contains impurity lead.Accompanying drawing 2 is the X-ray diffractogram of the present embodiment gained final product germanium hydride, as seen from the figure, the each diffraction peak of this product germanium hydride all with document (ACSNano, 2013,4414-4421) peak position on report is corresponding, and diffraction peak is stronger, illustrates that product is pure germanium hydride.Accompanying drawing 3 is the SEM figure of the present embodiment products therefrom germanium hydride, and germanium hydride is nanometer laminated structure as seen from the figure.The photocatalyst that accompanying drawing 4 is the formation of the present embodiment products therefrom is for photocatalytically degradating organic dye rhodamine B, as seen from the figure, test through photocatalytically degradating organic dye rhodamine B, the photocatalyst that germanium hydride forms can be at 4 min by rhodamine B degraded 82%, and the photocatalyst that nitrogen doping P25 forms degrades 70% at 30 min by rhodamine B.Compared with the visible P25 adulterating with N with the synthetic germanium hydride of ion-exchange, there is higher activity in photocatalytic applications.The photocatalyst that accompanying drawing 5 is the formation of the present embodiment products therefrom is for photocatalysis Decomposition aquatic products hydrogen.Through the test of photocatalysis Decomposition aquatic products hydrogen, it is 135 umol that the photocatalyst that germanium hydride forms can produce hydrogen at 6h water of decomposition.
The proof that above determination and analysis is comprehensive the product that obtains of the present embodiment be to there is the visible light-responded photocatalyst for Photocatalyzed Hydrogen Production.Adopt the germanium hydride prepared of the inventive method after photocatalyst, to have stronger visible light-respondedly being converted into, and there is high light catalytic activity, obtained effective application in fields such as photocatalysis Decomposition aquatic products hydrogen and degradable organic pollutants.
Embodiment 2
Take Ca:0.0407g, Ge:01448g, Pb:5.1795g puts into 2 cm
3alumina crucible in, and alumina crucible is sealed in quartz glass tube by high vacuum line operative technique (vacuum-line), system is warming up to 1000 DEG C and be incubated 20 hours in 4 hours with experiment box-type furnace, to ensure that raw material fully reacts; Be cooled to 600 DEG C with 5 DEG C per hour again, be incubated 8 hours; Subsequently Glass tubing is taken out, be inverted in whizzer, the rotating speed turning with per minute 3,500 is separated melting solubility promoter lead collect.Under microscope in glove box, pick out the sheet germanium calcium crystal 0.2g of crystal type high-quality, react ethanol bath with cryogenic thermostat and reacting 48 hours (temperature of reaction is subzero 30 DEG C) with 100ml concentrated hydrochloric acid under constantly stirring, treat that nature is warming up to room temperature and carries out suction filtration, wash with methyl alcohol and deionized water, and within 6 hours, obtain final product germanium hydride at vacuum drying oven inner drying under room temperature.
Accompanying drawing 6 is the X-ray diffractogram of the present embodiment gained final product germanium hydride, and as seen from the figure, this product is pure germanium hydride.Accompanying drawing 7 is the SEM figure of the present embodiment products therefrom germanium hydride, and germanium hydride is nanometer laminated structure as seen from the figure.
Embodiment 3
Take Ca:0.0411g, Ge:01445g, Pb:5.1802g puts into 2 cm
3alumina crucible in, and alumina crucible is sealed in quartz glass tube by high vacuum line operative technique (vacuum-line), system is warming up to 1000 DEG C and be incubated 20 hours in 4 hours with experiment box-type furnace, to ensure that raw material fully reacts; Be cooled to 600 DEG C with 5 DEG C per hour again, be incubated 10 hours; Subsequently Glass tubing is taken out, be inverted in whizzer, the rotating speed turning with per minute 3,500 is separated melting solubility promoter lead collect.Under microscope in glove box, pick out the sheet germanium calcium crystal 0.2g of crystal type high-quality, react ethanol bath with cryogenic thermostat and reacting 24 hours (temperature of reaction is subzero 30 DEG C) with 100ml concentrated hydrochloric acid under constantly stirring, treat that nature is warming up to room temperature and carries out suction filtration, wash with methyl alcohol and deionized water, and within 6 hours, obtain final product germanium hydride at vacuum drying oven inner drying under room temperature.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendments that creative work can make or distortion still in protection scope of the present invention.
Claims (9)
1. a preparation method with visible light-responded germanium hydride, is characterized in that, comprises that step is as follows:
1) utilize melting solubility promoter growing crystal method to synthesize presoma germanium calcium: in the glove box that is full of argon gas, be that Ca:Ge:Pb=0.7～1.5:2:20～25 weigh above-mentioned three kinds of simple substance according to the mol ratio of Ca, Ge, Pb, after mixing, put into alumina crucible, alumina crucible is sealed in quartz glass tube, process furnace was warming up to system 1000 DEG C and be incubated 18-22 hour in 4 hours, be cooled to 600 DEG C with the speed of 3-7 per hour DEG C again, insulation 10-15 hour; Subsequently Glass tubing is taken out, be inverted into and centrifugal in whizzer melting solubility promoter lead is separated and collected, under the microscope in glove box, pick out tabular crystal presoma germanium calcium;
2) described presoma germanium calcium is reacted to 24-48h with concentrated hydrochloric acid in the cryogenic thermostat ethanol bath of-30 DEG C, naturally return to room temperature, centrifugation, washing, dry and obtain.
2. a kind of preparation method with visible light-responded germanium hydride according to claim 1, is characterized in that, it is Ca:Ge=1:2 that described molar ratio closes.
3. a kind of preparation method with visible light-responded germanium hydride according to claim 1, is characterized in that, the described centrifugal speed of step (1) is turn/min of 3000-3500.
4. a kind of preparation method with visible light-responded germanium hydride according to claim 1, is characterized in that, in step (2), the ratio of presoma germanium calcium and concentrated hydrochloric acid is 0.2:100, g/ml; The mass concentration of concentrated hydrochloric acid is 37%.
5. the germanium hydride that the method described in claim 1-4 any one makes, is characterized in that, it has laminate structure.
6. germanium hydride claimed in claim 5 produces the application in hydrogen as catalyzer at visible light catalytic water of decomposition.
7. a germanium hydride photocatalyst, contains germanium hydride claimed in claim 5, and makes under illumination.
8. the preparation method of a kind of germanium hydride photocatalyst claimed in claim 7: it is characterized in that,
Described germanium hydride sample is joined in the mixing solutions of deionized water and methyl alcohol, and the noble metal platinum of load germanium hydride quality 1.0 wt%, under constantly stirring, irradiate 0.5-1 hour with 300W xenon lamp and obtain.
9. the preparation method of a kind of germanium hydride photocatalyst according to claim 8: it is characterized in that, described deionized water, methanol usage is every 50mg germanium hydride sample, uses 20-30 ml deionized water, 20-25 ml methanol.
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| CN108793230A (en) * | 2018-04-03 | 2018-11-13 | 广东工业大学 | A kind of stratiform germanium disulfide nanometer sheet of high power capacity and its preparation method and application |
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| CN110612365A (en) * | 2017-05-19 | 2019-12-24 | 昭和电工株式会社 | Method for electrochemically producing germane |
| CN110612365B (en) * | 2017-05-19 | 2022-04-05 | 昭和电工株式会社 | Method for electrochemically producing germane |
| CN109592641B (en) * | 2017-09-30 | 2021-12-07 | 天津大学 | Vinyl-modified hydrogen germanium two-dimensional material and preparation method thereof |
| CN109592641A (en) * | 2017-09-30 | 2019-04-09 | 天津大学 | Germanium hydrogen two-dimensional material of modified by vinyl and preparation method thereof |
| CN108172680A (en) * | 2018-01-24 | 2018-06-15 | 福州大学 | A kind of cubic phase Ca2Ge thermoelectric materials and preparation method thereof |
| CN110117744A (en) * | 2018-02-05 | 2019-08-13 | 天津大学 | A kind of hydroxylated two-dimensional semiconductor germanium-silicon alloy of hydrogenation-with gap tunable and preparation method |
| CN110117744B (en) * | 2018-02-05 | 2021-04-09 | 天津大学 | Hydrogenated-hydroxylated two-dimensional semiconductor germanium-silicon alloy with adjustable band gap and preparation method |
| CN108793230A (en) * | 2018-04-03 | 2018-11-13 | 广东工业大学 | A kind of stratiform germanium disulfide nanometer sheet of high power capacity and its preparation method and application |
| CN110745859A (en) * | 2018-07-24 | 2020-02-04 | 天津大学 | Method for preparing high-performance material by two-dimensional material CaGeTe functionalization |
| CN114890385A (en) * | 2021-07-01 | 2022-08-12 | 中国科学院上海硅酸盐研究所 | Efficient antioxidant two-dimensional hydrogermanium alkene nanosheet and preparation method and application thereof |
| CN114890385B (en) * | 2021-07-01 | 2023-09-08 | 中国科学院上海硅酸盐研究所 | Efficient antioxidant two-dimensional hydrogen germanium alkene nano-sheet and preparation method and application thereof |
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