CN104275196A - Ferroferric oxide/carbon/cadmium sulfide composite nano material and preparation method thereof - Google Patents

Ferroferric oxide/carbon/cadmium sulfide composite nano material and preparation method thereof Download PDF

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CN104275196A
CN104275196A CN201410574434.2A CN201410574434A CN104275196A CN 104275196 A CN104275196 A CN 104275196A CN 201410574434 A CN201410574434 A CN 201410574434A CN 104275196 A CN104275196 A CN 104275196A
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nano particle
carbon
cadmium sulfide
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谢坚坚
李正全
李丹
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Zhejiang Normal University CJNU
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Zhejiang Normal University CJNU
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Abstract

The invention provides a ferroferric oxide/carbon/cadmium sulfide composite nano material and a preparation method thereof. The preparation method comprises the following steps: firstly, synthesizing one-pack-one Fe3O4@C nano particles with good monodispersity by using a hydrothermal process, wherein the 'one-pack-one' means that one Fe3O4@C nano particle is only wrapped in one carbon layer; then obtaining Fe3O4@C@Cd<2+> by means of simple adsorption; and finally forming Fe3O4@C@CdS nano particles by adopting a microwave method. Compared with the prior art, the preparation method provided by the invention is simple in process and easy to operate; the prepared material has the characteristics of proper size, uniform structure, relatively strong magnetism and good photocatalysis effect; the material has a uniform spherical core-shell structure, is relatively good in dispersity in a solution, can perform a photocatalysis action under the irradiation of visible light; and because the composite nano material has magnetism, the composite nano material can be recycled for multiple times by using a magnet.

Description

Ferroferric oxide/carbon/cadmium sulfide composition nano material and preparation method thereof
Technical field
The present invention relates to technical field of inorganic nano-material preparation, particularly relate to a kind of ferroferric oxide/carbon/cadmium sulfide composition nano material and preparation method thereof.
Background technology
Cadmium sulfide (CdS) is a kind of very important II-VI group compound semiconductor light catalyst, and energy gap is 2.41eV, and electron mobility is , its relative dielectric constant is 11.6, has good visible absorption response and the redox ability of photohole electronics, can be used for degraded organic molecule group.CdS owing to having the characteristics such as excellent photoelectromagnetic, thus is widely used in the fields such as solar cell, light sensor material, nonlinear optical material and photochemical catalysis material.Wherein, CdS, as a kind of photochemical catalyst, has been widely used in life and the field of Environment Protections such as coating, antiseptic, water treatment, contaminant degradation.Under the irradiation of visible ray, CdS is excited, and the electron transition in valence band, to conduction band, produces electron-hole pair.The electron-hole pair on CdS surface can with the water of surrounding and oxygen effect and produce oxygen radical, this free radical has superpower oxidability, can the organic matter of oxidize majority, is degraded into carbon dioxide and water.
Although cadmium sulfide has the advantages such as cheap, stable, efficient, how reclaiming used catalyst efficiently, realize recycling of catalyst, is a problem needing to solve.Magneto separate is a kind of effective ways being separated magnetizable material, is therefore current common method by catalyst and magnetic material compound.Nano ferriferrous oxide (Fe 3o 4) owing to having the features such as superparamagnetism, high magnetic susceptibility, high-biocompatibility, adsorptivity, be widely used in fields such as bio-molecular separation, Magnetic resonance imagings (MRI), not only can pollutant in adsorbed water as phosphate, and easily to be separated from water rapidly by the effect of externally-applied magnetic field.In view of this, cadmium sulfide and tri-iron tetroxide compound are prepared efficient photochemical catalyst, the recycling rate of waterused of catalyst can be improved and industrially easily operate.
Early stage, more existing scholars carried out this type of trial work, and such as, Shim etc. have used high temperature process successfully to synthesize the cadmium sulfide heterojunction structure of tri-iron tetroxide; JoshyJoseph etc. have synthesized tri-iron tetroxide/cadmium sulfide nucleocapsid structure, but particle is easily reunited, and dispersiveness is not good, and pattern size is uneven, limit its application in a lot of field; Wanquan Jiang has synthesized the hollow ball of the tri-iron tetroxide of doped cadmium sulfide, but photocatalysis effect is not good; Some scholars also uses cladding process layer by layer to synthesize ferroferric oxide/carbon/cadmium sulfide, but complex steps.In sum, although these materials of scholar's synthesis of above-mentioned citing have photocatalysis performance at visible light wave range and recoverable, but there is following shortcoming: the pattern size of composite is uneven, dispersiveness is not good, and the ferroferric oxide/carbon material of inside adopts multistep synthesis, and process is loaded down with trivial details.
Summary of the invention
Ferroferric oxide/carbon/cadmium sulfide nano composite material that the object of the present invention is to provide a kind of nucleocapsid structure and preparation method thereof, this preparation method's technique is simple, easy to operate, ferroferric oxide/carbon/cadmium sulfide nano composite material the size of preparation is applicable to, and even structure, catalytic efficiency is higher.
The invention provides a kind of ferroferric oxide/carbon/cadmium sulfide composition nano material, chemical formula is: Fe 3o 4@C@CdS; Wherein, "@" represents coated.
Accordingly, the present invention also provides a kind of preparation method of ferroferric oxide/carbon/cadmium sulfide composition nano material, comprises the following steps:
Steps A: be added to by ferrocene in acetone, ultrasonic agitation forms mixed liquor, is then dropwise added by hydrogen peroxide in described mixed liquor, to move in autoclave and to heat, eccentric cleaning, be dispersed in ethanol, form Fe after stirring 3o 4@C nano particle ,@represents coated;
Step B: cadmium nitrate is added second alcohol and water and form clear solution, by described Fe 3o 4@C nano particle adds in described clear solution, ultrasonic disperse, eccentric cleaning after heating water bath, forms Fe 3o 4@C@Cd 2+nano particle ,@represents coated;
Step C: by described Fe 3o 4@C@Cd 2+nano particle, thioacetamide and water mix, microwave treatment after stirring, and eccentric cleaning dries formation ferroferric oxide/carbon/cadmium sulfide composition nano material of milling.
Preferably, in steps A, the ratio of described ferrocene, acetone and hydrogen peroxide is 0.4-0.8 gram: 30-50 milliliter: 0.5-3 milliliter.
Preferably, in steps A, the time of ultrasonic agitation is 20-50 minute.
Preferably, the temperature heated in steps A is 160-210 degree Celsius, and the time of heating is 24 hours.
Preferably, described Fe 3o 4the particle diameter of@C nano particle is 90-100 nanometer.
Preferably, in step B, the ratio of cadmium nitrate, ethanol and water is 0.01 mole: 10 milliliters: 10 milliliters.
Preferably, in step B, Fe 3o 4the mol ratio of@C nano particle and cadmium nitrate is 1:50-100.
Preferably, in step B, the temperature of heating water bath is 60-90 degree Celsius.
Preferably, the mol ratio of described thioacetamide and cadmium nitrate is 1:1.
Preferably, in step C, the microwave power of microwave treatment is 280 watts, and the microwave time is 15-30 minute.
First the present invention uses water heat transfer one to wrap one and the good Fe of monodispersity 3o 4@C nano particle, described " one bag one " to refer in a carbon-coating an only coated Fe 3o 4nano particle.Then Fe is obtained by simple absorption 3o 4@C@Cd 2+, finally adopt microwave method to form Fe 3o 4@C@CdS nano particle.Compared with prior art, preparation method's technique provided by the invention is simple, easy to operate; The material prepared has the advantages that size is applicable to, even structure, magnetic are comparatively strong and photocatalysis effect is good; Material has uniform spherical nucleocapsid, better dispersed in the solution, under visible light illumination, can carry out photocatalysis, because composite has magnetic, repeatedly can recycle and reuse with magnet.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of embodiment 1, and wherein A represents Fe 3o 4the X-ray diffractogram of@C nano particle, B represents Fe 3o 4x-ray diffractogram after the process of@C@CdS anneal nanoparticles, Fe 3o 4the standard card that@C is corresponding is 19-0629(JCPDS:19-0629), the standard card that CdS is corresponding is 89-0440(JCPDS:89-0440);
Fig. 2 is the transmission electron microscopy figure of embodiment 1, and wherein A represents Fe 3o 4the transmission electron microscopy figure of@C nano particle; B and C represents Fe 3o 4the transmission electron microscopy figure of@C@CdS nano particle; D represents Fe 3o 4the full resolution pricture of@C@CdS nano particle;
Fig. 3 is Fe prepared by embodiment 3o 4the transmission electron microscopy figure of@C nano particle, wherein, A is the Fe of the 2-in-1 one-tenth of embodiment 3o 4the transmission electron microscopy figure of@C nano particle, B are the Fe that embodiment 3 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle, C are the Fe that embodiment 4 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle, D are the Fe that embodiment 1 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle;
Fig. 4 is Fe prepared by embodiment 3o 4the transmission electron microscopy figure of@C nano particle, wherein, A is the Fe that embodiment 5 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle, B are the Fe that embodiment 6 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle, C are the Fe that embodiment 7 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle, D are the Fe that embodiment 1 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle;
Fig. 5 is Fe prepared by embodiment 1 3o 4the hysteresis curve figure of@C@CdS nano particle and six photocatalysis cycles of carrying out rhodamine B solution, A represents Fe 3o 4@C nano particle and Fe 3o 4the hysteresis curve figure of@C@CdS nano particle, list of illustrations is wherein shown in or without the Fe under magnetic fields 3o 4@C@CdS suspension; B represents Fe 3o 4six photocatalysis cycles that@C@CdS sample carries out rhodamine B solution;
Fig. 6 is the visible light photocatalytic degradation figure of sample prepared by embodiment 1, and wherein, A represents rhodamine B respectively at the Fe without any catalyst (blank), the sample (a) not carrying out microwave irradiation synthesis, above-mentioned synthesis (carrying out microwave 30min) 3o 4visible light photocatalytic degradation under@C@CdS sample (b); B represents rhodamine B respectively without any catalyst (blank), 10 milligrams of Fe 3o 4@C@CdS(a), 15 milligrams of Fe 3o 4@C@CdS(b), 20 milligrams of Fe 3o 4@C@CdS(c) under visible light photocatalytic degradation.
Detailed description of the invention
Below in conjunction with embodiment, concrete scheme of the present invention is further described.But the concrete scheme used, formula and explanation are not limitation of the present invention.
The invention provides a kind of preparation method of ferroferric oxide/carbon/cadmium sulfide composition nano material, comprise the following steps:
Steps A: be added to by ferrocene in acetone, ultrasonic agitation forms mixed liquor, is then dropwise added by hydrogen peroxide in described mixed liquor, to move in autoclave and to heat, eccentric cleaning, be dispersed in ethanol, form Fe after stirring 3o 4@C nano particle ,@represents coated;
Step B: cadmium nitrate is added second alcohol and water and form clear solution, by described Fe 3o 4@C nano particle adds in described clear solution, ultrasonic disperse, eccentric cleaning after heating water bath, forms Fe 3o 4@C@Cd 2+nano particle ,@represents coated;
Step C: by described Fe 3o 4@C@Cd 2+nano particle, thioacetamide and water mix, microwave treatment after stirring, and eccentric cleaning dries formation ferroferric oxide/carbon/cadmium sulfide composition nano material of milling.
The chemical formula of ferroferric oxide/carbon/cadmium sulfide composition nano material prepared by the present invention is: Fe 3o 4@C@CdS; Wherein, "@" represents coated.
One-step synthesis of the present invention take tri-iron tetroxide as the carbon ball of core, porous carbon layer wherein has very high specific area, be widely regarded as the potential adsorbent of tool and desirable carrier material, to adsorb multiple organic or inorganic pollutant and metal ion, good dispersiveness can be had in aqueous; Then ferroferric oxide/carbon is dispersed in the larger cadmium nitrate solution of concentration, utilizes heating water bath simply to adsorb, form ferroferric oxide/carbon/cadmium ion; Finally, the quick laminated one-tenth cadmium sulfide nanoparticles outside of microwave is utilized.Simple and the easy control of reaction conditions of preparation method's step provided by the invention, avoids high-temperature heating, utilizes microwave can the coated cadmium sulfide nanoparticles of Quick uniform.
In preparation process, in steps A, described Fe 3o 4@C nano particle adopts the synthesis of hydro-thermal method method, and it is brilliant in core with ferriferrous oxide nano, at its Surface coating one deck carbon shell, and the Fe prepared 3o 4the particle diameter of@C nano particle is preferably 90-100 nanometer.The ratio of described ferrocene, acetone and hydrogen peroxide is preferably 0.4-0.8 gram: 30-50 milliliter: 0.5-3 milliliter, is more preferably 0.5-0.6 gram: 30-40 milliliter: 1-3 milliliter, is more preferably 0.6 gram: 30 milliliters: 3 milliliters; The time of ultrasonic agitation is preferably 20-50 minute, is more preferably 30-40 minute, is more preferably 30 minutes; The temperature of heating is preferably 160-210 degree Celsius, and be more preferably 180-210 degree Celsius, be more preferably 210 degrees Celsius, the time of heating is preferably 24 hours.Preferably, in steps A, the Fe preferably eccentric cleaning obtained 3o 4@C is dispersed in ethanol, preferably obtains the mixed solution that concentration is 0.5 mM often liter.The present invention regulates Fe by adopting appropriate hydrogen peroxide 3o 4the size of nano particle, hydrogen peroxide is too much or very fewly all can cause Fe 3o 4nano particle is excessive or too small.
In step B, the ratio of cadmium nitrate, ethanol, water is preferably 0.01 mole: 10 milliliters: 10 milliliters; Fe 3o 4the mol ratio of@C nano particle and cadmium nitrate is preferably 1:50-100, is more preferably 1:50-80; The temperature of heating water bath is preferably 60-90 degree Celsius, is more preferably 60-80 degree Celsius, is more preferably 60-70 degree Celsius.
In step C, the mol ratio of described thioacetamide and cadmium nitrate is preferably 1:1; In step C, the microwave power of microwave treatment is preferably 280 watts, and the microwave time is preferably 15-30 minute, is more preferably 20-30 minute.In preparation process, when the reaction time is less than 15 minutes, cadmium sulfide growing amount is less, and the reaction time is greater than 30 minutes then without practical significance, and cadmium sulfide growing amount about 30 minutes is close to saturated.
In the preparation process of ferroferric oxide/carbon/cadmium sulfide composition nano material, the present invention is by changing concentration and the reaction condition of reaction raw materials, prepare ferroferric oxide/carbon/cadmium sulfide magnetic composite nano photochemical catalyst that particle diameter is 130-140 ran, even structure, favorable dispersibility, thus effectively reclaim cadmium sulfide, improve and utilize number of times not affect its catalytic effect.
In order to understand the present invention further, be described in detail to technical scheme provided by the invention below in conjunction with embodiment, protection scope of the present invention is not limited by the following examples.
The raw material that the embodiment of the present invention adopts and chemical reagent are commercial.
Embodiment 1
The preparation method of ferroferric oxide/carbon/cadmium sulfide composition nano material, comprises the following steps:
A. brilliant in core with ferriferrous oxide nano, at its Surface coating one deck carbon shell:
A. 0.6 gram of ferrocene is joined in 30 milliliters of acetone, ultrasonic disperse 10 minutes, form Homogeneous phase mixing liquid;
B. 3mL hydrogen peroxide is dropwise added in the mixed liquor of previous step formation, stir;
C. the mixed liquor that previous step is formed to be moved in 50 milliliters of autoclaves and puts into baking oven and keep 210 degrees Centigrade one day;
D. by the mixed liquor eccentric cleaning that previous step is formed, then be distributed in 6 milliliters of ethanol, namely form Fe 3o 4@C nano particle ,@represents coated;
B. at carbon-coating surface uniform parcel cadmium sulfide nanoparticles:
E. 0.01 mM of (3.0847 grams) cadmium nitrate is added 9 milliliters of ethanol and 10 ml waters formation clear solution;
F. 1 milliliter that step A is synthesized containing Fe 3o 4the alcohol mixed solution of@C nano particle adds in the solution of previous step formation, and ultrasonic disperse is even;
G. solution heating water bath previous step formed 24 hours;
H. by the mixed liquor eccentric cleaning that previous step is formed, namely Fe is formed 3o 4@C@Cd 2+nano particle ,@represents coated;
I. by Fe 3o 4@C@Cd 2+nano particle, 0.01 mM of (0.75 gram) thioacetamide and water mix, microwave 30 minutes after stirring;
J. by the mixed liquor eccentric cleaning that previous step is formed, namely drying mills forms Fe 3o 4@C@CdS nano particle ,@represents coated;
embodiment 2
On the basis of embodiment 1, change the hydrogen peroxide of b step in A into 0.5 milliliter.
embodiment 3
On the basis of embodiment 1, change the hydrogen peroxide of b step in A into 1 milliliter.
embodiment 4
On the basis of embodiment 1, change the hydrogen peroxide of b step in A into 2 milliliters.
embodiment 5
On the basis of embodiment 1, change the oven temperature of step c in A into 160 degrees Celsius.
embodiment 6
On the basis of embodiment 1, change the oven temperature of step c in A into 180 degrees Celsius.
embodiment 7
On the basis of embodiment 1, change the oven temperature of step c in A into 200 degrees Celsius.
The data recorded under x-ray powder diffraction instrument of composite prepared by above embodiment 1 as shown in Figure 1.In Fig. 1, A represents Fe 3o 4the X-ray diffractogram of@C nano particle, B represents Fe 3o 4x-ray diffractogram after the process of@C@CdS anneal nanoparticles, Fe 3o 4the standard card that@C is corresponding is 19-0629(JCPDS:19-0629), the standard card that CdS is corresponding is 89-0440(JCPDS:89-0440).The X ray diffracting data of Fig. 1 shows that the degree of crystallinity of ferroferric oxide/carbon is higher, and the peak of X-ray powder diffraction Standards Coordinating Committee powder diffraction card JCPDS:19-0629 coincide.The annealed process of product after coated cadmium sulfide its record X-ray powder diffraction data and show, in product except having tri-iron tetroxide crystal, to also have cadmium sulfide (JCPDS:89-0440).
Fig. 2 is that composite prepared by embodiment 1 characterizes the data obtained under transmission electron microscope (being called for short TEM).Figure A is that the TEM of ferroferric oxide/carbon characterizes picture, show that ferroferric oxide/carbon particle used has good monodispersity, and diameter is at 90-100 ran.Figure B and figure C represents that the TEM of ferroferric oxide/carbon/cadmium sulfide composite nanometer particle characterizes picture, and data show that cadmium sulfide is coated very even, and sample particle size is homogeneous, and single dispersing performance is good, and diameter is in 130-140 nanometer.
Fig. 3 is Fe prepared by embodiment 3o 4the transmission electron microscopy figure of@C nano particle, wherein, A is the Fe of the 2-in-1 one-tenth of embodiment 3o 4the transmission electron microscopy figure of@C nano particle, B are the Fe that embodiment 3 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle, C are the Fe that embodiment 4 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle, D are the Fe that embodiment 1 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle.As can be seen from the figure, oven temperature is improved within the specific limits, Fe 3o 4@C nano grain crystalline Du Gengjia.
Fig. 4 is Fe prepared by embodiment 3o 4the transmission electron microscopy figure of@C nano particle, wherein, A is the Fe that embodiment 5 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle, B are the Fe that embodiment 6 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle, C are the Fe that embodiment 7 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle, D are the Fe that embodiment 1 is synthesized 3o 4the transmission electron microscopy figure of@C nano particle.As can be seen from the figure, the amount of hydrogen peroxide is increased within the specific limits, Fe 3o 4@C nano particle diameter becomes large.
Fig. 5 is Fe prepared by embodiment 1 3o 4the hysteresis curve figure of@C@CdS nano particle and six photocatalysis cycles of carrying out rhodamine B solution, A represents Fe 3o 4@C nano particle and Fe 3o 4the hysteresis curve figure of@C@CdS nano particle, list of illustrations is wherein shown in or without the Fe under magnetic fields 3o 4@C@CdS suspension, as seen from the figure, the Fe of synthesis 3o 4@C CdS composite nanometer particle has stronger magnetic, under the effect of external magnetic force, is separated by catalyst easily from solution.B represents Fe 3o 4six photocatalysis cycles that@C@CdS sample carries out rhodamine B solution, as the recyclable catalyst of reality, are required at each cycle high catalytic activity used.As can be seen from the figure, slightly decline after each circulation of the photocatalytic activity of nano composite material.But in the end one-period, still has the rhodamine B of 64% to be decomposed.Known from the research of photocatalytic activity, 6 cycles that the rhodamine B degradation water solution that prepared nano composite material has a high photocatalytic activity just uses after neutralizing this activity slightly decline.Therefore, prepared Fe 3o 4@C@CdS nano composite material can be used as photochemical catalyst desirable in actual applications.
Fig. 6 is the visible light photocatalytic degradation figure of sample prepared by embodiment 1, and wherein, A represents rhodamine B respectively at the Fe not carrying out the sample (a) of microwave irradiation synthesis, above-mentioned synthesis (carrying out microwave 30min) without any catalyst (blank), i step 3o 4visible light photocatalytic degradation under@C@CdS sample (b), final rhodamine B is respectively 92%, 50%, 16%; B represents rhodamine B respectively without any catalyst (blank), 10 milligrams of Fe 3o 4@C@CdS(a), 15 milligrams of Fe 3o 4@C@CdS(b), 20 milligrams of Fe 3o 4@C@CdS(c) under visible light photocatalytic degradation, final rhodamine B is respectively 92%, 20%, 13%, 4%.In sum, microwave is conducive to CdS nano particle and is coated to Fe better 3o 4@C thus bear the good Fe of photocatalysis performance 3o 4@C@CdS nano particle, in addition, suitably increases Fe 3o 4@C@CdS quality can carry out photocatalysis experiment better to improve catalytic efficiency.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.

Claims (11)

1. ferroferric oxide/carbon/cadmium sulfide composition nano material, is characterized in that, chemical formula is: Fe 3o 4@C@CdS; Wherein, "@" represents coated.
2. a preparation method for ferroferric oxide/carbon/cadmium sulfide composition nano material, is characterized in that, comprises the following steps:
Steps A: be added to by ferrocene in acetone, ultrasonic agitation forms mixed liquor, is then dropwise added by hydrogen peroxide in described mixed liquor, to move in autoclave and to heat, eccentric cleaning, be dispersed in ethanol, form Fe after stirring 3o 4@C nano particle ,@represents coated;
Step B: cadmium nitrate is added second alcohol and water and form clear solution, by described Fe 3o 4@C nano particle adds in described clear solution, ultrasonic disperse, eccentric cleaning after heating water bath, forms Fe 3o 4@C@Cd 2+nano particle ,@represents coated;
Step C: by described Fe 3o 4@C@Cd 2+nano particle, thioacetamide and water mix, microwave treatment after stirring, and eccentric cleaning dries formation ferroferric oxide/carbon/cadmium sulfide composition nano material of milling.
3. preparation method according to claim 2, is characterized in that, in steps A, the ratio of described ferrocene, acetone and hydrogen peroxide is 0.4-0.8 gram: 30-50 milliliter: 0.5-3 milliliter.
4. preparation method according to claim 2, is characterized in that, in steps A, the time of ultrasonic agitation is 20-50 minute.
5. preparation method according to claim 2, is characterized in that, the temperature heated in steps A is 160-210 degree Celsius, and the time of heating is 24 hours.
6. preparation method according to claim 2, is characterized in that, described Fe 3o 4the particle diameter of@C nano particle is 90-100 nanometer.
7. the preparation method according to claim 2 ~ 6 any one, is characterized in that, in step B, the ratio of cadmium nitrate, ethanol and water is 0.01 mole: 10 milliliters: 10 milliliters.
8. the preparation method according to claim 2 ~ 6 any one, is characterized in that, in step B, and Fe 3o 4the mol ratio of@C nano particle and cadmium nitrate is 1:50-100.
9. the preparation method according to claim 2 ~ 6 any one, is characterized in that, in step B, the temperature of heating water bath is 60-90 degree Celsius.
10. the preparation method according to claim 2 ~ 6 any one, is characterized in that, the mol ratio of described thioacetamide and cadmium nitrate is 1:1.
11. preparation methods according to claim 2 ~ 6 any one, it is characterized in that, in step C, the microwave power of microwave treatment is 280 watts, and the microwave time is 15-30 minute.
CN201410574434.2A 2014-10-24 2014-10-24 Ferroferric oxide/carbon/cadmium sulfide composite nano material and preparation method thereof Pending CN104275196A (en)

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CN110255617B (en) * 2019-06-28 2022-06-21 东莞深圳清华大学研究院创新中心 Preparation method of vanadium dioxide nano powder
CN110560090A (en) * 2019-08-19 2019-12-13 江苏大学 Preparation method and application of superparamagnetic ferroferric oxide @ silicon dioxide @ cadmium sulfide nano core-shell structure material
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CN111774072B (en) * 2020-07-10 2022-02-01 重庆工程职业技术学院 Method for preparing carbon-coated magnetic cadmium sulfide composite photocatalyst
CN111774072A (en) * 2020-07-10 2020-10-16 重庆工程职业技术学院 Method for preparing carbon-coated magnetic cadmium sulfide composite photocatalyst
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CN113003603A (en) * 2021-03-09 2021-06-22 中国石油大学(华东) CdS/Co3O4Composite material, preparation method and application thereof in acetone gas detection under light excitation
CN113003603B (en) * 2021-03-09 2022-05-31 中国石油大学(华东) CdS/Co3O4Composite material, preparation method and application thereof in acetone gas detection under light excitation
CN114471617A (en) * 2022-03-23 2022-05-13 浙江理工大学 Magnetic photocatalyst, preparation method and application thereof
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