CN113135588A - Carbon-coated SnO2Preparation method of hollow nanosphere - Google Patents

Carbon-coated SnO2Preparation method of hollow nanosphere Download PDF

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CN113135588A
CN113135588A CN202110420054.3A CN202110420054A CN113135588A CN 113135588 A CN113135588 A CN 113135588A CN 202110420054 A CN202110420054 A CN 202110420054A CN 113135588 A CN113135588 A CN 113135588A
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hollow
hollow nanosphere
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carbon
sno
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杨友文
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Hefei University of Technology
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    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C01G19/02—Oxides
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
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    • C01B32/15—Nano-sized carbon materials
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    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C01P2004/34—Spheres hollow
    • 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
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases

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Abstract

The invention discloses a carbon-coated Sn02The preparation method of the hollow nanosphere comprises the following steps: preparation of Sn02Hollow nanosphere carbonized precursor, and prepared Sn02Screening the hollow nanosphere carbonized precursor; for the screened Sn02Grinding the hollow nanosphere carbonized precursor, and then grinding the Sn02The hollow nanosphere carbonized powder is calcined. The invention relates to carbon-coated Sn02The preparation method of the hollow nanosphere has the advantages that the raw materials are simple and cheap, no additive is required to be added in the calcining process, the calcining time is short, the production cost can be reduced, and the carbon-coated Sn0 is coated with carbon2The preparation method of the hollow nanosphere is simple and can be used for large-scale production, and D-glucose and Sn0 can be adjusted2Proportional adjustment of hollow nanospheres to generate carbon-coated Sn02The thickness of the carbon layer of the hollow nanosphere can be increased, so that the carbon-coated Sn0 can be improved2The hollow nanospheres have better stability and quality.

Description

Carbon-coated SnO2Preparation method of hollow nanosphere
Technical Field
The invention relates to the field of hollow nanospheres, in particular to carbon-coated Sn02A preparation method of hollow nanospheres.
Background
As a nano material with high specific surface area and low density, the hollow nano carbon sphere not only has the characteristics of good permeability, higher chemical and thermal stability, adsorption property, nontoxicity, biocompatibility and the like, but also has a regular spherical structure, so that the hollow nano carbon sphere has great potential application value in a plurality of new technical fields such as gas storage, catalyst carriers, biological controllable drug delivery, biological capsules, light structure materials, micro-nano containers, super capacitor electrode materials and the like.
The existing hollow nano carbon spheres have expensive raw materials, various additives need to be added in the reaction process, the production and calcination time is long, and the production cost is high, so that a carbon-coated Sn0 is provided2A preparation method of hollow nanospheres.
Disclosure of Invention
The invention mainly aims to provide carbon-coated Sn02The preparation method of the hollow nanosphere can effectively solve the problems in the background technology.
In order to achieve the purpose, the invention adopts the technical scheme that:
carbon-coated Sn02The preparation method of the hollow nanosphere comprises the following steps:
(1) preparation of Sn02Hollow nanosphere carbonized precursor, and prepared Sn02Screening the hollow nanosphere carbonized precursor;
(2) and the screened Sn02Grinding the hollow nanosphere carbonized precursor, and then grinding the Sn02Calcining the hollow nanosphere carbonized powder;
(3) the calcined Sn02Taking out the hollow nanospheres, and screening the products to obtain the carbon-coated Sn02Hollow nanospheres.
Preferably, Sn0 is prepared in step (1)2The preparation method of the hollow nanosphere carbonized precursor comprises the following steps:
(i) arrangement of Sn02Mixed liquid required by the hollow nanosphere carbonized precursor;
② treating the mixed solution to obtain Sn02A hollow nanosphere precursor;
③ to Sn02Treating the hollow nanosphere precursor to obtain a second mixed solution;
fourthly, processing the second mixed solution to obtain Sn02And (3) carbonizing a precursor of the hollow nanosphere.
Preferably, the preparing the mixed solution in the step (i) comprises the following steps:
i, adding absolute ethyl alcohol, distilled water and concentrated hydrochloric acid into a reaction container;
II, stirring the raw materials by adopting a stirrer to fully mix the absolute ethyl alcohol, the distilled water and the concentrated hydrochloric acid;
III, adding the uniformly mixed raw materials into ultrasonic equipment for ultrasonic treatment;
and IV, stirring the ultrasonically treated raw materials again to obtain a mixed solution.
Preferably, the ratio of the absolute ethyl alcohol, the distilled water and the concentrated hydrochloric acid in the step I is 160:13-17:3-5, the stirring machine in the step II adopts a magnetic stirrer, the stirring time is 2-4min, stannous oxide is added into the reaction container before ultrasonic treatment in the step III, the ultrasonic time is 6-10min, and the stirring time in the step IV is 55-65min again.
Preferably, the optimal ratio of the absolute ethyl alcohol to the distilled water to the concentrated hydrochloric acid is 150:15:4, the stirrer in the step II adopts a magnetic stirrer, the stirring time is 3min, stannous oxide is added into the reaction container before the ultrasonic treatment in the step III, the ultrasonic time is 9min, and the stirring time in the step IV is 58min again.
Preferably, the treatment of the mixed solution in the second step includes the following steps:
A. adding the mixed solution into a reaction kettle for reaction;
B. sequentially carrying out centrifugal treatment, washing and drying treatment on the reaction product to obtain Sn02A hollow nanosphere precursor.
Preferably, the reaction temperature in the step A is 180-210 ℃, the reaction time is 10-12h, and the reaction product is cooled to room temperature before the treatment in the step B.
Preferably, the reaction temperature in the step A is 190 ℃, the reaction time is 11h, and the reaction product is cooled to room temperature before the treatment in the step B.
Preferably, Sn0 in step (c)2The hollow nanosphere precursor treatment comprises the following steps:
a. dissolving D-glucose in water, and then carrying out ultrasonic treatment;
b. addition of Sn0 to sonicated D-glucose water2And (5) carrying out hollow nanosphere precursor, and continuing ultrasonic treatment.
Preferably, the ultrasonic treatment time in step a is 8-12min, the D-glucose water in step b is 2.5% -7.5% of D-glucose water, and the added Sn02The weight ratio of the hollow nanosphere precursor to the D-glucose is 1:10-30, and the ultrasonic time is 25-30 min.
Preferably, the ultrasonic treatment time in step a is 10min, the D-glucose water in step b is 2.5% -7.5% of D-glucose water, and the added Sn02The weight ratio of the hollow nanosphere precursor to the D-glucose is 1:10-30, and the ultrasonic time is 28 min.
The proportion of the hollow nanosphere precursor to the D-glucose is different, and the obtained carbon-coated Sn02The wall thickness of the hollow nanospheres is different, and the carbon coating of Sn0 can be realized by controlling the proportion of the hollow nanosphere precursor to D-glucose2Control of wall thickness of hollow nanospheres.
Preferably, the processing of the second mixed solution in the step (iv) includes the steps of:
adding the second mixed solution into a reaction kettle to react for 2-7h at the temperature of 180-190 ℃;
(II) sequentially carrying out centrifugal treatment, washing and drying treatment on the reaction product to obtain Sn02And (3) carbonizing a precursor of the hollow nanosphere.
Preferably, Sn0 in step (2)2The particle size of the carbonized precursor of the hollow nanosphere is 200-500nm after grinding, and the ground Sn0 is used during calcination2And (3) flattening the hollow nanosphere carbonized precursor powder, wherein the heating rate in the calcining process is 4-7 ℃/min, the temperature is increased to 500-550 ℃, and the constant temperature is kept for calcining for 2-4 h.
Compared with the prior art, the carbon-coated Sn0 is prepared by the method2The preparation method of the hollow nanosphere has the following beneficial effects:
1. the raw materials in the invention are simple and cheap, no additive is needed in the calcining process, the calcining time is short, the production cost can be reduced, and the carbon-coated Sn02The preparation method of the hollow nanosphere is simple and can be produced on a large scale;
2. in the invention, D-glucose and Sn0 can be adjusted2Proportional adjustment of hollow nanospheres to generate carbon-coated Sn02The thickness of the carbon layer of the hollow nanosphere can be increased, so that the carbon-coated Sn0 can be improved2The hollow nanospheres have better stability and quality.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
Carbon-coated Sn02The preparation method of the hollow nanosphere comprises the following steps:
(1) preparation of Sn02Hollow nanosphere carbonized precursor, and prepared Sn02Screening the hollow nanosphere carbonized precursor;
preparation of Sn0 in step (1)2The preparation method of the hollow nanosphere carbonized precursor comprises the following steps:
(i) arrangement of Sn02Mixed liquid required by the hollow nanosphere carbonized precursor;
i, adding absolute ethyl alcohol, distilled water and concentrated hydrochloric acid into a reaction container, wherein the ratio of the absolute ethyl alcohol to the distilled water to the concentrated hydrochloric acid is 150:15: 4;
II, stirring the raw materials by adopting a stirrer, so that the absolute ethyl alcohol, the distilled water and the concentrated hydrochloric acid are fully mixed, wherein the stirrer adopts a magnetic stirrer, and the stirring time is 3 min;
III, adding the uniformly mixed raw materials into ultrasonic equipment for ultrasonic treatment, wherein stannous oxide is added into a reaction container before the ultrasonic treatment, and the ultrasonic time is 9 min;
and IV, re-stirring the ultrasonically treated raw materials for 58min to obtain a mixed solution.
② treating the mixed solution to obtain Sn02A hollow nanosphere precursor;
A. adding the mixed solution into a reaction kettle for reaction, wherein the reaction temperature is 190 ℃, and the reaction time is 11 hours;
B. cooling a reaction product to room temperature, sequentially performing centrifugal treatment, washing and drying on the reaction product, washing the product obtained by centrifuging for 3-4 times by using distilled water and ethanol, and drying by using a dryer at the drying temperature of 65 ℃ to obtain Sn02A hollow nanosphere precursor.
③ to Sn02Treating the hollow nanosphere precursor to obtain a second mixed solution;
a. dissolving D-glucose in water, and performing ultrasonic treatment for 10 min;
b. addition of Sn0 to sonicated D-glucose water2Continuing ultrasonic treatment of the hollow nanosphere precursor, wherein the D-glucose water is 2.5% of D-glucose water, and adding Sn02The weight ratio of the hollow nanosphere precursor to the D-glucose is 1:10, and the ultrasonic time is 26 min.
Fourthly, processing the second mixed solution to obtain Sn02A hollow nanosphere carbonized precursor;
adding the second mixed solution into a reaction kettle to react for 5 hours at 185 ℃;
(II) sequentially carrying out centrifugal treatment, washing and drying treatment on the reaction product, centrifuging for 4 times by using a centrifuge to obtain a black product, cleaning for 5 feet by using deionized water and ethanol, and drying for 5 hours at 65 ℃ by using a dryer to obtain Sn02And (3) carbonizing a precursor of the hollow nanosphere.
(2) And the screened Sn02Grinding the hollow nanosphere carbonized precursor, and then grinding the Sn02Calcining the hollow nanosphere carbonized powder;
Sn02the particle size of the carbonized precursor of the hollow nanosphere is 200nm after grinding, and the grinded Sn0 is calcined2And (3) flattening the hollow nanosphere carbonized precursor powder, heating to 550 ℃ at the heating rate of 6 ℃/min during calcination, and calcining for 3h at constant temperature.
(3) The calcined Sn02Taking out the hollow nanospheres, screening the products with the particle size of 200-400nm,obtaining carbon coated Sn02Hollow nanospheres.
Example 2
Carbon-coated Sn02The preparation method of the hollow nanosphere comprises the following steps:
(2) preparation of Sn02Hollow nanosphere carbonized precursor, and prepared Sn02Screening the hollow nanosphere carbonized precursor;
preparation of Sn0 in step (1)2The preparation method of the hollow nanosphere carbonized precursor comprises the following steps:
(i) arrangement of Sn02Mixed liquid required by the hollow nanosphere carbonized precursor;
i, adding absolute ethyl alcohol, distilled water and concentrated hydrochloric acid into a reaction container, wherein the ratio of the absolute ethyl alcohol to the distilled water to the concentrated hydrochloric acid is 150:15: 4;
II, stirring the raw materials by adopting a stirrer, so that the absolute ethyl alcohol, the distilled water and the concentrated hydrochloric acid are fully mixed, wherein the stirrer adopts a magnetic stirrer, and the stirring time is 3 min;
III, adding the uniformly mixed raw materials into ultrasonic equipment for ultrasonic treatment, wherein stannous oxide is added into a reaction container before the ultrasonic treatment, and the ultrasonic time is 9 min;
and IV, re-stirring the ultrasonically treated raw materials for 58min to obtain a mixed solution.
② treating the mixed solution to obtain Sn02A hollow nanosphere precursor;
A. adding the mixed solution into a reaction kettle for reaction, wherein the reaction temperature is 190 ℃, and the reaction time is 11 hours;
B. cooling a reaction product to room temperature, sequentially performing centrifugal treatment, washing and drying on the reaction product, washing the product obtained by centrifuging for 3-4 times by using distilled water and ethanol, and drying by using a dryer at the drying temperature of 65 ℃ to obtain Sn02A hollow nanosphere precursor.
③ to Sn02Treating the hollow nanosphere precursor to obtain a second mixed solution;
a. dissolving D-glucose in water, and performing ultrasonic treatment for 10 min;
b. addition of Sn0 to sonicated D-glucose water2Continuing ultrasonic treatment of the hollow nanosphere precursor, wherein the D-glucose water is 5% of D-glucose water, and added Sn02The weight ratio of the hollow nanosphere precursor to the D-glucose is 1:20, and the ultrasonic time is 26 min.
Fourthly, processing the second mixed solution to obtain Sn02A hollow nanosphere carbonized precursor;
adding the second mixed solution into a reaction kettle to react for 5 hours at 185 ℃;
(II) sequentially carrying out centrifugal treatment, washing and drying treatment on the reaction product, centrifuging for 4 times by using a centrifuge to obtain a black product, cleaning for 5 feet by using deionized water and ethanol, and drying for 5 hours at 65 ℃ by using a dryer to obtain Sn02And (3) carbonizing a precursor of the hollow nanosphere.
(2) And the screened Sn02Grinding the hollow nanosphere carbonized precursor, and then grinding the Sn02Calcining the hollow nanosphere carbonized powder;
Sn02the particle size of the carbonized precursor of the hollow nanosphere is 200nm after grinding, and the grinded Sn0 is calcined2And (3) flattening the hollow nanosphere carbonized precursor powder, heating to 550 ℃ at the heating rate of 6 ℃/min during calcination, and calcining for 3h at constant temperature.
(3) The calcined Sn02Taking out the hollow nanospheres, screening the products, and screening the products with the particle size of 200-400nm to obtain the carbon-coated Sn02Hollow nanospheres.
Example 3
Carbon-coated Sn02The preparation method of the hollow nanosphere comprises the following steps:
(1) preparation of Sn02Hollow nanosphere carbonized precursor, and prepared Sn02Screening the hollow nanosphere carbonized precursor;
preparation of Sn0 in step (1)2The preparation method of the hollow nanosphere carbonized precursor comprises the following steps:
(i) arrangement of Sn02Mixed liquid required by the hollow nanosphere carbonized precursor;
i, adding absolute ethyl alcohol, distilled water and concentrated hydrochloric acid into a reaction container, wherein the ratio of the absolute ethyl alcohol to the distilled water to the concentrated hydrochloric acid is 150:15: 4;
II, stirring the raw materials by adopting a stirrer, so that the absolute ethyl alcohol, the distilled water and the concentrated hydrochloric acid are fully mixed, wherein the stirrer adopts a magnetic stirrer, and the stirring time is 3 min;
III, adding the uniformly mixed raw materials into ultrasonic equipment for ultrasonic treatment, wherein stannous oxide is added into a reaction container before the ultrasonic treatment, and the ultrasonic time is 9 min;
and IV, re-stirring the ultrasonically treated raw materials for 58min to obtain a mixed solution.
② treating the mixed solution to obtain Sn02A hollow nanosphere precursor;
A. adding the mixed solution into a reaction kettle for reaction, wherein the reaction temperature is 190 ℃, and the reaction time is 11 hours;
B. cooling a reaction product to room temperature, sequentially performing centrifugal treatment, washing and drying on the reaction product, washing the product obtained by centrifuging for 3-4 times by using distilled water and ethanol, and drying by using a dryer at the drying temperature of 65 ℃ to obtain Sn02A hollow nanosphere precursor.
③ to Sn02Treating the hollow nanosphere precursor to obtain a second mixed solution;
a. dissolving D-glucose in water, and performing ultrasonic treatment for 10 min;
b. addition of Sn0 to sonicated D-glucose water2Continuing ultrasonic treatment of the hollow nanosphere precursor, wherein the D-glucose water is 7.5% of D-glucose water, and adding Sn02The weight ratio of the hollow nanosphere precursor to the D-glucose is 1:30, and the ultrasonic time is 26 min.
Fourthly, processing the second mixed solution to obtain Sn02A hollow nanosphere carbonized precursor;
adding the second mixed solution into a reaction kettle to react for 5 hours at 185 ℃;
(II) sequentially carrying out centrifugal treatment, washing and drying treatment on the reaction product, centrifuging for 4 times by using a centrifuge to obtain a black product, cleaning for 5 feet by using deionized water and ethanol, and drying for 5 hours at 65 ℃ by using a dryer to obtain Sn02And (3) carbonizing a precursor of the hollow nanosphere.
(2) And the screened Sn02Grinding the hollow nanosphere carbonized precursor, and then grinding the Sn02Calcining the hollow nanosphere carbonized powder;
Sn02the particle size of the carbonized precursor of the hollow nanosphere is 200nm after grinding, and the grinded Sn0 is calcined2And (3) flattening the hollow nanosphere carbonized precursor powder, heating to 550 ℃ at the heating rate of 6 ℃/min during calcination, and calcining for 3h at constant temperature.
(3) The calcined Sn02Taking out the hollow nanospheres, screening the products, and screening the products with the particle size of 200-400nm to obtain the carbon-coated Sn02Hollow nanospheres.
Sn0 in examples 1 to 32The weight ratio of the hollow nanosphere precursor to the D-glucose is different, and the obtained carbon-coated Sn02The thicknesses of the carbon layers on the outer surface of the hollow nanosphere are different, and the thicknesses of the carbon layers are 16nm, 18nm and 20nm in sequence.
In addition, the carbon-coated Sn0 of the invention2The preparation method of the hollow nanosphere has the advantages that the raw materials are simple and cheap, no additive is required to be added in the calcining process, the calcining time is short, the production cost can be reduced, and the carbon-coated Sn0 is coated with carbon2The preparation method of the hollow nanosphere is simple and can be produced on a large scale;
in the invention, D-glucose and Sn0 can be adjusted2Proportional adjustment of hollow nanospheres to generate carbon-coated Sn02The thickness of the carbon layer of the hollow nanosphere can be increased, so that the carbon-coated Sn0 can be improved2The hollow nanospheres have better stability and quality.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1.一种碳包覆Sn02中空纳米球的制备方法，其特征在于，包括以下步骤：1. a preparation method of carbon-coated SnO 2 hollow nanospheres, is characterized in that, comprises the following steps: (1)、制备Sn02中空纳米球碳化前驱体，并且对制备的Sn02中空纳米球碳化前驱体进行筛选；(1), prepare SnO 2 hollow nanosphere carbonization precursor, and screen the prepared SnO 2 hollow nanosphere carbonization precursor; (2)、对筛选后的Sn02中空纳米球碳化前驱体进行研磨，然后对研磨后的Sn02中空纳米球碳化粉末进行煅烧；(2), grinding the Sn0 2 hollow nanosphere carbonized precursor after screening, and then calcining the ground Sn0 2 hollow nanosphere carbonized powder; (3)、将煅烧后的Sn02中空纳米球取出，对产物进行筛选，得到碳包覆Sn02中空纳米球。(3), taking out the calcined Sn0 2 hollow nanospheres, and screening the product to obtain carbon-coated Sn0 2 hollow nanospheres. 2.根据权利要求1所述的一种碳包覆Sn02中空纳米球的制备方法，其特征在于：步骤(1)中制备Sn02中空纳米球碳化前驱体的制备方法包括以下步骤：2. the preparation method of a kind of carbon-coated SnO hollow nanosphere according to claim 1, is characterized in that: the preparation method of preparing SnO hollow nanosphere carbonization precursor in step (1) comprises the following steps: ①、配置Sn02中空纳米球碳化前驱体所需要的混合液；①, configure the mixed solution required for Sn0 2 hollow nanosphere carbonization precursor; ②、对混合液进行处理，得到Sn02中空纳米球前驱体；2. Process the mixed solution to obtain SnO 2 hollow nanosphere precursor; ③、对Sn02中空纳米球前驱体进行处理，得到第二种混合液；3. Process the Sn0 2 hollow nanosphere precursor to obtain the second mixed solution; ④、对第二种混合液进行加工，得到Sn02中空纳米球碳化前驱体。④. Process the second mixed solution to obtain Sn0 2 hollow nanosphere carbonized precursor. 3.根据权利要求2所述的一种碳包覆Sn02中空纳米球的制备方法，其特征在于：步骤①中的配置混合液包括以下步骤：3. the preparation method of a kind of carbon-coated SnO hollow nanosphere according to claim 2, is characterized in that: the configuration mixed solution in step 1. comprises the following steps: Ⅰ、将无水乙醇、蒸馏水和浓盐酸添加到反应容器中；1. Add dehydrated alcohol, distilled water and concentrated hydrochloric acid into the reaction vessel; Ⅱ、采用搅拌机搅拌原料，使得无水乙醇、蒸馏水和浓盐酸充分混合；Ⅱ. Use a mixer to stir the raw materials, so that absolute ethanol, distilled water and concentrated hydrochloric acid are fully mixed; Ⅲ、将混合均匀的原料添加到超声设备中进行超声处理；Ⅲ. Add the evenly mixed raw materials to the ultrasonic equipment for ultrasonic treatment; Ⅳ、对超声处理的原料进行再次搅拌，得到混合液。Ⅳ. Stirring the raw material of ultrasonic treatment again to obtain a mixed solution. 4.根据权利要求3所述的一种碳包覆Sn02中空纳米球的制备方法，其特征在于：步骤Ⅰ中无水乙醇、蒸馏水和浓盐酸的比例为140-160:13-17:3-5，步骤Ⅱ中的搅拌机采用磁力搅拌器，搅拌时间为2-4min，步骤Ⅲ中超声处理前向反应容器中添加氧化亚锡，超声时间为6-10min，步骤Ⅳ中再次搅拌的时间为55-65min。4. the preparation method of a kind of carbon-coated SnO hollow nanosphere according to claim 3, is characterized in that: in step 1, the ratio of absolute ethanol, distilled water and concentrated hydrochloric acid is 140-160:13-17:3 -5, the stirrer in step II adopts a magnetic stirrer, and the stirring time is 2-4min. In step III, stannous oxide is added to the reaction vessel before ultrasonic treatment, and the ultrasonic time is 6-10min. The time of stirring again in step IV is 55-65min. 5.根据权利要求2所述的一种碳包覆Sn02中空纳米球的制备方法，其特征在于：步骤②中混合液处理包括以下步骤：5. the preparation method of a kind of carbon-coated SnO hollow nanospheres according to claim 2, is characterized in that: in step 2., the mixed solution treatment comprises the following steps: A、将混合液添加到反应釜中进行反应；A, the mixed solution is added in the reactor to react; B、对反应的产物依次进行离心处理、冲洗和烘干处理，得到Sn02中空纳米球前驱体。B. Perform centrifugal treatment, washing and drying treatment on the reaction product in turn to obtain Sn0 2 hollow nanosphere precursor. 6.根据权利要求5所述的一种碳包覆Sn02中空纳米球的制备方法，其特征在于：步骤A中的反应温度为180-210℃，反应时间为10-12h，步骤B中处理前先将反应的产物冷却至室温。6 . The preparation method of carbon-coated SnO hollow nanospheres according to claim 5 , wherein the reaction temperature in step A is 180-210° C., the reaction time is 10-12 h, and the treatment in step B is 10-12 h. 7 . The reaction product was previously cooled to room temperature. 7.根据权利要求2所述的一种碳包覆Sn02中空纳米球的制备方法，其特征在于：步骤③中Sn02中空纳米球前驱体处理包括以下步骤：7. the preparation method of a kind of carbon-coated SnO hollow nanospheres according to claim 2, is characterized in that: in step 3., SnO hollow nanosphere precursor processing comprises the following steps: a、D-葡萄糖溶解到水中，然后进行超声处理；a, D-glucose is dissolved in water, and then ultrasonically treated; b、向超声处理的D-葡萄糖水中添加Sn02中空纳米球前驱体，继续超声。b. Add Sn0 2 hollow nanosphere precursor to the sonicated D-glucose water, and continue to sonicate. 8.根据权利要求7所述的一种碳包覆Sn02中空纳米球的制备方法，其特征在于：步骤a中超声时间为8-12min，步骤b中的D-葡萄糖水为2.5％-7.5％的D-葡萄糖水，添加的Sn02中空纳米球前驱体与D-葡萄糖的重量比为1:10-30，超声时间为25-30min。8. The preparation method of a carbon-coated SnO hollow nanosphere according to claim 7, wherein the ultrasonic time in step a is 8-12min, and the D-glucose water in step b is 2.5%-7.5 % D-glucose water, the weight ratio of the added SnO 2 hollow nanosphere precursor and D-glucose is 1:10-30, and the ultrasonic time is 25-30min. 9.根据权利要求2所述的一种碳包覆Sn02中空纳米球的制备方法，其特征在于：步骤④中第二种混合液加工包括以下步骤：9. the preparation method of a kind of carbon-coated SnO hollow nanosphere according to claim 2, is characterized in that: in step 4., the second mixed solution processing comprises the following steps: (一)、将第二种混合液添加到反应釜中在180-190℃下进行反应2-7h；(1), the second kind of mixed solution is added in the reaction kettle and reacts at 180-190 ℃ for 2-7h; (二)、对反应的产物依次进行离心处理、冲洗和烘干处理，得到Sn02中空纳米球碳化前驱体。(2), performing centrifugal treatment, washing and drying treatment on the reaction product successively to obtain SnO 2 hollow nanosphere carbonized precursor. 10.根据权利要求1所述的一种碳包覆Sn02中空纳米球的制备方法，其特征在于：步骤(2)中Sn02中空纳米球碳化前驱体研磨后粒径为200-500nm，煅烧时将研磨后的Sn02中空纳米球碳化前驱体粉末摊平，煅烧时的升温速度为4-7℃/min，升温至500-550℃，并保持恒温煅烧2-4h。10. The preparation method of a carbon-coated SnO hollow nanosphere according to claim 1, characterized in that: in step (2), the particle size of the SnO hollow nanosphere carbonized precursor after grinding is 200-500 nm, and the calcination The ground SnO 2 hollow nanosphere carbonized precursor powder is flattened, the heating rate during calcination is 4-7 °C/min, the temperature is raised to 500-550 °C, and the calcination is maintained at a constant temperature for 2-4 hours.
CN202110420054.3A 2021-04-19 2021-04-19 Carbon-coated SnO2Preparation method of hollow nanosphere Pending CN113135588A (en)

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