CN107055589A - The method that Microwave reduction method liquid phase prepares CdS nanometer material - Google Patents
The method that Microwave reduction method liquid phase prepares CdS nanometer material Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000000463 material Substances 0.000 title claims abstract description 24
- 239000007791 liquid phase Substances 0.000 title claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 60
- 239000007787 solid Substances 0.000 claims abstract description 50
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 39
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 39
- 239000007864 aqueous solution Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000008367 deionised water Substances 0.000 claims abstract description 28
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000005119 centrifugation Methods 0.000 claims abstract description 21
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 19
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 19
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000005642 Oleic acid Substances 0.000 claims abstract description 19
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 19
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 18
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims abstract description 11
- 238000013019 agitation Methods 0.000 claims abstract description 10
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 abstract description 8
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 235000019441 ethanol Nutrition 0.000 description 7
- 125000005909 ethyl alcohol group Chemical group 0.000 description 7
- 239000002071 nanotube Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
- C01G11/02—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of method that Microwave reduction method liquid phase prepares CdS nanometer material, this method comprises the following steps：(1) cadmium nitrate is added into stirring in deionized water to be completely dissolved, adds oleic acid, produce solution A；(2) sodium borohydride is added into stirring in deionized water to be completely dissolved, obtains sodium borohydride aqueous solution；(3) sodium borohydride aqueous solution is added in solution A, dark solution is changed into from colourless solution after microwave after being well mixed, room temperature is cooled to, absolute ethyl alcohol washing is then added into dark solution, through centrifugation, black solid is produced；(4) by black solid ultrasonic disperse in absolute ethyl alcohol, ammonium sulfide solution stirring is added after magnetic agitation, yellow or yellow-green soln is produced；(5) yellow or yellow-green soln are centrifuged with absolute ethyl alcohol, obtain yellow or greenish yellow solid；(6) yellow or greenish yellow solid are vacuum dried to constant weight, produce yellow or yellow green CdS solids.The inventive method is simple, cost is relatively low, environmental pollution is small.
Description
Technical field
CdS nanometers of materials are prepared the present invention relates to the preparing technical field of nano material, more particularly to Microwave reduction method liquid phase
The method of material.
Background technology
Photocatalysis nano material, such as CdS nanometer material, in the degrading of organic pollution, the synthesis of chemistry, photocatalytic water system
The fields such as hydrogen, carbon dioxide reduction methane, the recovery of heavy metal, the purified treatment of waste gas suffer from being widely applied prospect.
Hydro-thermal method is to prepare the conventional method of CdS nanometer material, and this method preparation condition requires very high, it is necessary in high temperature bar
Under part, and the reaction time is especially long, and workload is also very big, and preparation process is also special cumbersome.
The content of the invention
The technical problems to be solved by the invention are to provide the microwave that a kind of method is simple, cost is relatively low, environmental pollution is small
The method that reducing process liquid phase prepares CdS nanometer material.
To solve the above problems, the method that Microwave reduction method liquid phase of the present invention prepares CdS nanometer material, including with
Lower step：
(1) by cadmium nitrate（Cd(NO3)2·4H2O）By 0.5 ~ 5.0mmol：2.0 ~ 20.0mL ratio is added in deionized water,
It is completely dissolved in 18 ~ 25 DEG C of stirrings, obtains the cadmium nitrate aqueous solution；Oleic acid is added in the cadmium nitrate aqueous solution, solution A is produced；Institute
The volume ratio for stating oleic acid and the deionized water is 1：800~8000；
(2) by sodium borohydride (NaBH4) press 2.0 ~ 15.0mmol：0.4 ~ 3.0mL ratio is added in deionized water, in 18 ~
25 DEG C of stirrings are completely dissolved, and obtain sodium borohydride aqueous solution；
(3) the sodium borohydride aqueous solution is added in the solution A, obtains mixed liquor after being well mixed, the mixed liquor is through micro-
Dark solution is changed into from colourless solution after ripple, room temperature is cooled to, the nothing of 1 ~ 3 times of its volume is then added into the dark solution
Water-ethanol is washed, and through centrifugation 3 ~ 5 times, produces black solid；
(4) the black solid is pressed into 0.5 ~ 5.0mol：2 ~ 20mL ratio ultrasonic disperse is in absolute ethyl alcohol, through magnetic agitation
Ammonium sulfide solution is added after 10 ~ 15min, 0.5 ~ 3h is stirred in 18 ~ 25 DEG C, produces yellow or yellow-green soln；
(5) the yellow or yellow-green soln are centrifuged 3 ~ 5 times with absolute ethyl alcohol, obtain yellow or greenish yellow solid；
(6) the yellow or greenish yellow solid are vacuum dried to constant weight, produce yellow or yellow green CdS solids.
The condition of the step (3) middle microwave refers to high fire ~ high fire, and the time is 20 ~ 25s.
(3) the step each means that centrifugation rate is 4500 ~ 8000rpm with the condition of the step (5) middle centrifugation, often
The secondary time is 120 ~ 200 s.
(5) middle absolute ethyl alcohol and yellow or the volume ratio of yellow-green soln are 0.5 ~ 3.0 mL to the step：1 mL.
The step (6) in vacuum drying condition refer to temperature be 30 ~ 60 DEG C.
The present invention has advantages below compared with prior art：
1st, the present invention is, using cadmium nitrate, sodium borohydride, ammonium sulfide as raw material, CdS nanometer material to be synthesized through microwave, not only method
Simply, the defect of hydro-thermal method complex steps is efficiently solved, and environmental pollution is small.
2nd, the whole building-up process of the present invention is carried out at normal temperatures, and shortens whole generated time, is efficiently solved existing
Must be reacted under the high temperature conditions in technology, the defect of reaction time length.
3rd, x-ray diffraction experiment is carried out to nano-tube/CdS obtained by the present invention（Referring to Fig. 1）, from XRD spectra as can be seen that 2
θ is 24.8,26.5,28.2,36.6,43.6,47.8 and characteristic diffraction peak occurs in 51.8o position, with standard card JCPDS
NO. 41-1049 is corresponding, belongs to the CdS of hexagonal crystal system wurtzite structure, corresponds respectively to (100), (002), (101),
(102), (110), (103) and (112) crystal face；Substantially increase for 26.5,43.6 and 51.8o position feature diffraction maximum in 2 θ
By force, corresponding to the CdS of cubic system zincblende lattce structure, its standard card is JCPDS NO. 75-1546, is corresponded to respectively
(111), (220) and (311) crystal face.
4th, the CdS nanometer material size that prepared by the present invention is smaller, homogeneous（As shown in Figures 2 and 3）.
5th, the present invention uses Microwave reduction method, with regard to that can prepare the CdS nano-particles that crystallinity is high, purity is high, not only simple
Preparation technology is changed, has reduced production cost, and reduced operation difficulty, without special reactor.
Brief description of the drawings
The embodiment to the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is the X ray diffracting spectrum (XRD) of nano-tube/CdS material of the present invention.
Fig. 2（a）For nano-tube/CdS transmission electron microscope (TEM) photo of the present invention（50 nm）And Fig. 2（b）For nano-tube/CdS of the present invention
Transmission electron microscope (HTEM) photo.
Fig. 3 is nano-tube/CdS ESEM (SEM) photo of the present invention.
Embodiment
The method that the Microwave reduction method liquid phase of embodiment 1 prepares CdS nanometer material, comprises the following steps：
(1) by cadmium nitrate（Cd(NO3)2·4H2O）By 0.5mmol：2.0mL ratio is added in deionized water, in 18 DEG C of stirrings
It is completely dissolved, obtains the cadmium nitrate aqueous solution；Oleic acid is added in the cadmium nitrate aqueous solution, solution A is produced.
The volume ratio of oleic acid and deionized water is 1：800.
(2) by sodium borohydride (NaBH4) press 2.0mmol：0.4mL ratio is added in deionized water, in 18 DEG C of stirrings
It is completely dissolved, obtains sodium borohydride aqueous solution.
(3) sodium borohydride aqueous solution is added in solution A, it is well mixed after obtain mixed liquor, the mixed liquor high fire ~
Dark solution is changed into from colourless solution after 20 ~ 25s of microwave under conditions of high fire, room temperature is cooled to, then added into dark solution
Enter the absolute ethyl alcohol washing of 1 times of its volume, centrifuged 3 times under conditions of centrifugation rate is 4500rpm, 200 s, is produced black every time
Color solid.
(4) black solid is pressed into 0.5mol：2mL ratio ultrasonic disperse is in absolute ethyl alcohol, after magnetic agitation 10min
Ammonium sulfide solution is added, 0.5h is stirred in 18 DEG C, produces yellow or yellow-green soln.
(5) 1 mL yellow or yellow-green soln are centrifuged with 0.5 mL absolute ethyl alcohols under conditions of centrifugation rate is 4500rpm
3 times, 200 s, obtains yellow or greenish yellow solid every time.
(6) yellow or greenish yellow solid are vacuum dried to constant weight in 30 DEG C, produce yellow or yellow green CdS solids.
The method that the Microwave reduction method liquid phase of embodiment 2 prepares CdS nanometer material, comprises the following steps：
(1) by cadmium nitrate（Cd(NO3)2·4H2O）By 1.0mmol：4.0mL ratio is added in deionized water, in 20 DEG C of stirrings
It is completely dissolved, obtains the cadmium nitrate aqueous solution；Oleic acid is added in the cadmium nitrate aqueous solution, solution A is produced.
The volume ratio of oleic acid and deionized water is 1：1600.
(2) by sodium borohydride (NaBH4) press 4.0mmol：0.8mL ratio is added in deionized water, in 20 DEG C of stirrings
It is completely dissolved, obtains sodium borohydride aqueous solution.
(3) sodium borohydride aqueous solution is added in solution A, it is well mixed after obtain mixed liquor, the mixed liquor high fire ~
Dark solution is changed into from colourless solution after 20 ~ 25s of microwave under conditions of high fire, room temperature is cooled to, then added into dark solution
Enter the absolute ethyl alcohol washing of 3 times of its volume, centrifuged 5 times under conditions of centrifugation rate is 8000rpm, 120 s, is produced black every time
Color solid.
(4) black solid is pressed into 5.0mol：20mL ratio ultrasonic disperse is in absolute ethyl alcohol, after magnetic agitation 10min
Ammonium sulfide solution is added, 1h is stirred in 20 DEG C, produces yellow or yellow-green soln.
(5) 1 mL yellow or yellow-green soln are centrifuged with 1.0 mL absolute ethyl alcohols under conditions of centrifugation rate is 8000rpm
5 times, 120 s, obtains yellow or greenish yellow solid every time.
(6) yellow or greenish yellow solid are vacuum dried to constant weight in 60 DEG C, produce yellow or yellow green CdS solids.
The method that the Microwave reduction method liquid phase of embodiment 3 prepares CdS nanometer material, comprises the following steps：
(1) by cadmium nitrate（Cd(NO3)2·4H2O）By 1.5mmol：6.0mL ratio is added in deionized water, in 22 DEG C of stirrings
It is completely dissolved, obtains the cadmium nitrate aqueous solution；Oleic acid is added in the cadmium nitrate aqueous solution, solution A is produced.
The volume ratio of oleic acid and deionized water is 1：2400.
(2) by sodium borohydride (NaBH4) press 6.0mmol：1.2mL ratio is added in deionized water, in 22 DEG C of stirrings
It is completely dissolved, obtains sodium borohydride aqueous solution.
(3) sodium borohydride aqueous solution is added in solution A, it is well mixed after obtain mixed liquor, the mixed liquor high fire ~
Dark solution is changed into from colourless solution after 20 ~ 25s of microwave under conditions of high fire, room temperature is cooled to, then added into dark solution
Enter the absolute ethyl alcohol washing of 2 times of its volume, centrifuged 4 times under conditions of centrifugation rate is 5500rpm, 140 s, is produced black every time
Color solid.
(4) black solid is pressed into 1.0mol：5.0mL ratio ultrasonic disperse is in absolute ethyl alcohol, through magnetic agitation 12min
After add ammonium sulfide solution, in 22 DEG C stir 1h, produce yellow or yellow-green soln.
(5) 1 mL yellow or yellow-green soln are centrifuged with 2.0 mL absolute ethyl alcohols under conditions of centrifugation rate is 5500rpm
4 times, 140 s, obtains yellow or greenish yellow solid every time.
(6) yellow or greenish yellow solid are vacuum dried to constant weight in 40 DEG C, produce yellow or yellow green CdS solids.
The method that the Microwave reduction method liquid phase of embodiment 4 prepares CdS nanometer material, comprises the following steps：
(1) by cadmium nitrate（Cd(NO3)2·4H2O）By 2.0mmol：8.0mL ratio is added in deionized water, in 24 DEG C of stirrings
It is completely dissolved, obtains the cadmium nitrate aqueous solution；Oleic acid is added in the cadmium nitrate aqueous solution, solution A is produced.
The volume ratio of oleic acid and deionized water is 1：3200.
(2) by sodium borohydride (NaBH4) press 8.0mmol：1.6mL ratio is added in deionized water, in 24 DEG C of stirrings
It is completely dissolved, obtains sodium borohydride aqueous solution.
(3) sodium borohydride aqueous solution is added in solution A, it is well mixed after obtain mixed liquor, the mixed liquor high fire ~
Dark solution is changed into from colourless solution after 20 ~ 25s of microwave under conditions of high fire, room temperature is cooled to, then added into dark solution
Enter the absolute ethyl alcohol washing of 1.5 times of its volume, centrifuged 4 times under conditions of centrifugation rate is 6500rpm, 180 s, is produced every time
Black solid.
(4) black solid is pressed into 2.0mol：10mL ratio ultrasonic disperse is in absolute ethyl alcohol, after magnetic agitation 12min
Ammonium sulfide solution is added, 1.5h is stirred in 24 DEG C, produces yellow or yellow-green soln.
(5) 1 mL yellow or yellow-green soln are centrifuged with 3.0 mL absolute ethyl alcohols under conditions of centrifugation rate is 6500rpm
4 times, 180 s, obtains yellow or greenish yellow solid every time.
(6) yellow or greenish yellow solid are vacuum dried to constant weight in 50 DEG C, produce yellow or yellow green CdS solids.
The method that the Microwave reduction method liquid phase of embodiment 5 prepares CdS nanometer material, comprises the following steps：
(1) by cadmium nitrate（Cd(NO3)2·4H2O）By 2.5mmol：10.0mL ratio is added in deionized water, is stirred in 25 DEG C
Mix and be completely dissolved, obtain the cadmium nitrate aqueous solution；Oleic acid is added in the cadmium nitrate aqueous solution, solution A is produced.
The volume ratio of oleic acid and deionized water is 1：4000.
(2) by sodium borohydride (NaBH4) press 10.0mmol：2.0mL ratio is added in deionized water, in 25 DEG C of stirrings
It is completely dissolved, obtains sodium borohydride aqueous solution.
(3) sodium borohydride aqueous solution is added in solution A, it is well mixed after obtain mixed liquor, the mixed liquor high fire ~
Dark solution is changed into from colourless solution after 20 ~ 25s of microwave under conditions of high fire, room temperature is cooled to, then added into dark solution
Enter the absolute ethyl alcohol washing of 2.5 times of its volume, centrifuged 5 times under conditions of centrifugation rate is 7500rpm, 180 s, is produced every time
Black solid.
(4) black solid is pressed into 3.0mol：15mL ratio ultrasonic disperse is in absolute ethyl alcohol, after magnetic agitation 15min
Ammonium sulfide solution is added, 1.5h is stirred in 25 DEG C, produces yellow or yellow-green soln.
(5) 1 mL yellow or yellow-green soln are centrifuged with 3.0 mL absolute ethyl alcohols under conditions of centrifugation rate is 7500rpm
4 times, 180 s, obtains yellow or greenish yellow solid every time.
(6) yellow or greenish yellow solid are vacuum dried to constant weight in 55 DEG C, produce yellow or yellow green CdS solids.
The method that the Microwave reduction method liquid phase of embodiment 6 prepares CdS nanometer material, comprises the following steps：
(1) by cadmium nitrate（Cd(NO3)2·4H2O）By 3.0mmol：12.0mL ratio is added in deionized water, is stirred in 25 DEG C
Mix and be completely dissolved, obtain the cadmium nitrate aqueous solution；Oleic acid is added in the cadmium nitrate aqueous solution, solution A is produced.
The volume ratio of oleic acid and deionized water is 1：4800.
(2) by sodium borohydride (NaBH4) press 12.0mmol：2.4mL ratio is added in deionized water, in 25 DEG C of stirrings
It is completely dissolved, obtains sodium borohydride aqueous solution.
(3) sodium borohydride aqueous solution is added in solution A, it is well mixed after obtain mixed liquor, the mixed liquor high fire ~
Dark solution is changed into from colourless solution after 20 ~ 25s of microwave under conditions of high fire, room temperature is cooled to, then added into dark solution
Enter the absolute ethyl alcohol washing of 2.5 times of its volume, centrifuged 5 times under conditions of centrifugation rate is 8000rpm, 200 s, is produced every time
Black solid.
(4) black solid is pressed into 4.0mol：15mL ratio ultrasonic disperse is in absolute ethyl alcohol, after magnetic agitation 15min
Ammonium sulfide solution is added, 2h is stirred in 25 DEG C, produces yellow or yellow-green soln.
(5) 1 mL yellow or yellow-green soln are centrifuged with 3.0 mL absolute ethyl alcohols under conditions of centrifugation rate is 8000rpm
5 times, 200 s, obtains yellow or greenish yellow solid every time.
(6) yellow or greenish yellow solid are vacuum dried to constant weight in 60 DEG C, produce yellow or yellow green CdS solids.
The method that the Microwave reduction method liquid phase of embodiment 7 prepares CdS nanometer material, comprises the following steps：
(1) by cadmium nitrate（Cd(NO3)2·4H2O）By 5.0mmol：20.0mL ratio is added in deionized water, is stirred in 25 DEG C
Mix and be completely dissolved, obtain the cadmium nitrate aqueous solution；Oleic acid is added in the cadmium nitrate aqueous solution, solution A is produced.
The volume ratio of oleic acid and deionized water is 1：8000.
(2) by sodium borohydride (NaBH4) press 15.0mmol：3.0mL ratio is added in deionized water, in 25 DEG C of stirrings
It is completely dissolved, obtains sodium borohydride aqueous solution.
(3) sodium borohydride aqueous solution is added in solution A, it is well mixed after obtain mixed liquor, the mixed liquor high fire ~
Dark solution is changed into from colourless solution after 20 ~ 25s of microwave under conditions of high fire, room temperature is cooled to, then added into dark solution
Enter the absolute ethyl alcohol washing of 2.5 times of its volume, centrifuged 5 times under conditions of centrifugation rate is 8000rpm, 200 s, is produced every time
Black solid.
(4) black solid is pressed into 4.0mol：15mL ratio ultrasonic disperse is in absolute ethyl alcohol, after magnetic agitation 15min
Ammonium sulfide solution is added, 3h is stirred in 25 DEG C, produces yellow or yellow-green soln.
(5) 1 mL yellow or yellow-green soln are centrifuged with 3.0 mL absolute ethyl alcohols under conditions of centrifugation rate is 8000rpm
5 times, 200 s, obtains yellow or greenish yellow solid every time.
(6) yellow or greenish yellow solid are vacuum dried to constant weight in 60 DEG C, produce yellow or yellow green CdS solids.
Claims (5)
1. the method that Microwave reduction method liquid phase prepares CdS nanometer material, comprises the following steps：
(1) cadmium nitrate is pressed into 0.5 ~ 5.0mmol：2.0 ~ 20.0mL ratio is added in deionized water, has been stirred in 18 ~ 25 DEG C
Fully dissolved, obtains the cadmium nitrate aqueous solution；Oleic acid is added in the cadmium nitrate aqueous solution, solution A is produced；The oleic acid with it is described go from
The volume ratio of sub- water is 1：800~8000；
(2) sodium borohydride is pressed into 2.0 ~ 15.0mmol：0.4 ~ 3.0mL ratio is added in deionized water, in 18 ~ 25 DEG C of stirrings
It is completely dissolved, obtains sodium borohydride aqueous solution；
(3) the sodium borohydride aqueous solution is added in the solution A, obtains mixed liquor after being well mixed, the mixed liquor is through micro-
Dark solution is changed into from colourless solution after ripple, room temperature is cooled to, the nothing of 1 ~ 3 times of its volume is then added into the dark solution
Water-ethanol is washed, and through centrifugation 3 ~ 5 times, produces black solid；
(4) the black solid is pressed into 0.5 ~ 5.0mol：2 ~ 20mL ratio ultrasonic disperse is in absolute ethyl alcohol, through magnetic agitation
Ammonium sulfide solution is added after 10 ~ 15min, 0.5 ~ 3h is stirred in 18 ~ 25 DEG C, produces yellow or yellow-green soln；
(5) the yellow or yellow-green soln are centrifuged 3 ~ 5 times with absolute ethyl alcohol, obtain yellow or greenish yellow solid；
(6) the yellow or greenish yellow solid are vacuum dried to constant weight, produce yellow or yellow green CdS solids.
2. the method that Microwave reduction method liquid phase as claimed in claim 1 prepares CdS nanometer material, it is characterised in that：The step
The condition of rapid (3) middle microwave refers to high fire ~ high fire, and the time is 20 ~ 25s.
3. the method that Microwave reduction method liquid phase as claimed in claim 1 prepares CdS nanometer material, it is characterised in that：The step
Suddenly (3) each meaning with the condition of the step (5) middle centrifugation that centrifugation rate is 4500 ~ 8000rpm, each time is 120 ~
200 s。
4. the method that Microwave reduction method liquid phase as claimed in claim 1 prepares CdS nanometer material, it is characterised in that：The step
Rapid (5) middle absolute ethyl alcohol is 0.5 ~ 3.0 mL with yellow or the volume ratio of yellow-green soln：1 mL.
5. the method that Microwave reduction method liquid phase as claimed in claim 1 prepares CdS nanometer material, it is characterised in that：The step
Suddenly (6) in vacuum drying condition refer to temperature be 30 ~ 60 DEG C.
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| CN102125858A (en) * | 2010-12-28 | 2011-07-20 | 南京林业大学 | Preparation method of p-CuO/n-CdS/ZnS composite semiconductor photochemical catalyst |
| CN102942210A (en) * | 2012-11-14 | 2013-02-27 | 陕西科技大学 | Preparation method of red-shift cadmium sulfide ball cluster microcrystalline |
| CN103332724A (en) * | 2013-05-22 | 2013-10-02 | 温州大学 | Preparation method of sea urchin-shaped cadmium sulfide nanospheres |
| CN103771487A (en) * | 2013-12-26 | 2014-05-07 | 江苏大学 | Method for synthetizing Ag2S-CdS hetero-nanostructure employing microwave |
| CN105016313A (en) * | 2015-06-12 | 2015-11-04 | 温州大学 | Gourd string structure cadmium sulfide-tellurium heterojunction photoelectrolysis composite material, preparation method and use |
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| CN102125858A (en) * | 2010-12-28 | 2011-07-20 | 南京林业大学 | Preparation method of p-CuO/n-CdS/ZnS composite semiconductor photochemical catalyst |
| CN102942210A (en) * | 2012-11-14 | 2013-02-27 | 陕西科技大学 | Preparation method of red-shift cadmium sulfide ball cluster microcrystalline |
| CN103332724A (en) * | 2013-05-22 | 2013-10-02 | 温州大学 | Preparation method of sea urchin-shaped cadmium sulfide nanospheres |
| CN103771487A (en) * | 2013-12-26 | 2014-05-07 | 江苏大学 | Method for synthetizing Ag2S-CdS hetero-nanostructure employing microwave |
| CN105016313A (en) * | 2015-06-12 | 2015-11-04 | 温州大学 | Gourd string structure cadmium sulfide-tellurium heterojunction photoelectrolysis composite material, preparation method and use |
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