CN114132955A - Preparation method of hexagonal system alpha-ZnS nano material - Google Patents

Preparation method of hexagonal system alpha-ZnS nano material Download PDF

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CN114132955A
CN114132955A CN202111427183.1A CN202111427183A CN114132955A CN 114132955 A CN114132955 A CN 114132955A CN 202111427183 A CN202111427183 A CN 202111427183A CN 114132955 A CN114132955 A CN 114132955A
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zns
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urea
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宋明
季生福
闫东鹏
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Shandong Pengfu New Material Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00Compounds of zinc
    • C01G9/08Sulfides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
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    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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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Abstract

The invention discloses a preparation method of a hexagonal system alpha-ZnS nano material. Firstly, preparing high-dispersion beta-ZnS nano-particles by taking an inorganic zinc source and a sulfur source as raw materials and taking alkali metal chloride as a nano-particle control and dispersing agent at room temperature by adopting an ultrasonic method; then reacting the beta-ZnS nano particles with a urea solution under the action of ultrasonic waves, carrying out centrifugal separation, and roasting at high temperature under a vacuum condition to prepare the alpha-ZnS nano powder material. The invention adopts inorganic zinc source, sulfur source, alkali metal chloride, urea and the like as raw materials, so that only inorganic salt-containing wastewater is generated in the production process, no organic matter-containing wastewater is generated, and the wastewater is easier to treat. The invention adopts the coordination complexing and crystal transformation of the urea to the beta-ZnS, so that the temperature for converting the beta-ZnS into the alpha-ZnS is greatly reduced, and the reaction process flow is simple and convenient to operate, thereby having important industrial application value.

Description

Preparation method of hexagonal system alpha-ZnS nano material
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a preparation method of a hexagonal system alpha-ZnS nano material.
Background
ZnS is an important semiconductor material and has wide application in the fields of luminescent devices, sensors, biological detection, fluorescent labeling, photocatalysis, plastic additives and the like. ZnS is also a white pigment with excellent coverage and good dispersibility in plastics. The structure and the morphology of the ZnS material are closely related to the performance of the ZnS material, and the ZnS materials prepared by different methods also have different structural characteristics and performance. ZnS has two crystal structures, one is beta-ZnS of face-centered cubic system, also called sphalerite; the other is hexagonal alpha-ZnS, also called wurtzite.
alpha-ZnS is a high temperature variant of zinc sulfide, and beta-ZnS can be converted into alpha-ZnS under the condition of 1020 ℃; different zinc sources and sulfur sources can be adopted to prepare the alpha-ZnS, but the existing reaction process flow is more complicated, and the requirement on reaction conditions is higher; in some reaction processes, waste liquid containing organic matters is generated, and the environmental pressure is higher.
Disclosure of Invention
The invention aims to provide a preparation method of a hexagonal system alpha-ZnS nano material. Firstly, preparing high-dispersion beta-ZnS nano-particles by taking an inorganic zinc source and a sulfur source as raw materials and taking alkali metal chloride as a nano-particle control and dispersing agent at room temperature by adopting an ultrasonic method; then reacting the beta-ZnS nano particles with a urea solution under the action of ultrasonic waves, carrying out centrifugal separation, and roasting at high temperature under a vacuum condition to prepare the alpha-ZnS nano powder material.
The preparation method of the hexagonal system alpha-ZnS nano material comprises the following steps:
(1) respectively preparing soluble zinc salt solution, sulfide salt solution and alkali metal chloride solution;
(2) at room temperature, dropwise adding an alkali metal chloride solution into a soluble zinc salt solution, fully stirring, dropwise adding a sulfide salt solution, performing ultrasonic treatment at the power of 100-150W for 40-60min, and finally aging at room temperature for 8-20 h;
(3) centrifugally separating the reaction liquid aged in the step (2), centrifugally washing the precipitate with deionized water, and finally drying in vacuum at 60-100 ℃ for 5-10 hours to obtain the beta-ZnS nano material;
(4) adding the beta-ZnS nano material into a urea solution, uniformly stirring, carrying out ultrasonic treatment for 60-80min under the power of 60-100W, and finally standing for 5-12 h at room temperature;
(5) and (4) centrifugally separating the reaction liquid obtained in the step (4), and roasting the solid under the vacuum condition to obtain the hexagonal system alpha-ZnS nano material.
The soluble zinc salt is one or more of zinc chloride, zinc nitrate and zinc sulfate.
The sulfide salt is sodium sulfide and/or ammonium sulfide.
The alkali metal chloride is one or more of sodium chloride, potassium chloride and cesium chloride.
The mass ratio of the soluble zinc salt solution to the sulfide salt solution to the alkali metal chloride solution is 1-4:1-4: 1.
The mass concentration of the soluble zinc salt solution is 1-5%.
The mass concentration of the sulfide salt solution is 0.3-3%.
The mass concentration of the alkali metal chloride solution is 0.3-3%.
The mass concentration of the urea solution is 0.2-3%.
The adding amount of the beta-ZnS nano material added into the urea solution is 1-5 wt%.
The roasting temperature in the step (5) is 500-600 ℃, and the roasting time is 1-2 hours.
The method for preparing the alpha-ZnS nano material has the following remarkable advantages:
(1) in the preparation of alpha-ZnS, because inorganic zinc source, sulfur source, alkali metal chloride, urea and the like are adopted as raw materials, only inorganic salt-containing wastewater is generated in the production process, and organic matter-containing wastewater is not generated, so that the wastewater is easier to treat.
(2) The coordination complexing and the crystal transformation of the urea to the beta-ZnS are adopted, so that the Zn of the beta-ZnS and the N of the urea form a coordination bond, the temperature for converting the beta-ZnS into the alpha-ZnS is greatly reduced, and the reaction process flow is simple and convenient to operate, so that the method has important industrial application value.
Drawings
Fig. 1 is an X-ray diffraction (XRD) pattern of the α -ZnS nanomaterial prepared in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited thereto.
Example 1
(1) Weighing 4.09g ZnCl2Dissolving in 95.91g deionized water to obtain ZnCl2The solution with a mass content of 4.09 wt.%, referred to as A1 solution. Weighing 7.21g of Na2S·6H2O was dissolved in 92.79g of deionized water to prepare Na2The solution with an S content of 2.34 wt.% was designated as B1 solution. 0.88g of NaCl was weighed out and dissolved in 49.12g of deionized water to prepare a solution with a NaCl mass content of 1.76 wt%, which was designated as C1 solution.
(2) C1 is dripped into A1 liquid under the condition of room temperature, the B1 liquid is slowly dripped after the full stirring, the ultrasonic treatment is carried out for 60min under the ultrasonic power of 130W after the dripping is finished, and the reaction liquid is aged for 12 hours under the room temperature.
(3) The aged reaction solution was subjected to centrifugal separation, and then the solid was washed with 100g of deionized water, subjected to centrifugal separation, and repeated 3 times. And finally, drying the solid for 8 hours in vacuum at the temperature of 80 ℃ to obtain the prepared beta-ZnS nano-particle material which is marked as beta-ZnS-1.
(4) 1.80g of urea ((NH) was weighed out2)2CO) was dissolved in 98.20g of deionized water to make a solution with a urea mass content of 1.80 wt%, which was designated as D1 solution.
(5) 2.92g of prepared beta-ZnS-1 is weighed and added into the D1 solution, after being stirred uniformly, the solution is subjected to ultrasonic treatment for 80min under the ultrasonic power of 60W, and the reaction solution is kept stand at the room temperature for 8 hours.
(6) And (3) carrying out centrifugal separation on the reaction liquid after standing, and roasting the solid for 2 hours at 500 ℃ under a vacuum condition to obtain the prepared alpha-ZnS nano-particle material. The label is alpha-ZnS-1.
FIG. 1 is an X-ray diffraction (XRD) pattern of the α -ZnS-1 nanoparticle material obtained in this example 1, which is in full agreement with the standard pattern (JCPDS NO.36-1450) of hexagonal α -ZnS (wurtzite) and shows a pure hexagonal α -ZnS (wurtzite) nanoparticle material.
Example 2
(1) 2.73g of ZnCl are weighed out2Dissolved in 97.27gIn deionized water to prepare ZnCl2The solution with a mass content of 2.73 wt.% is designated as A2 solution. 5.23g (NH) are weighed4)2S was dissolved in 94.77g of deionized water to prepare (NH)4)2The solution containing 1.36 wt% of S was designated as B2 solution. 0.75g of KCl is weighed and dissolved in 49.25g of deionized water to prepare a solution with the KCl mass content of 1.50wt percent, which is marked as C2 solution.
(2) C2 is dripped into A2 liquid under the condition of room temperature, the B2 liquid is slowly dripped after the full stirring, the ultrasonic treatment is carried out for 40min under the ultrasonic power of 150W after the dripping is finished, and the reaction liquid is aged for 12 hours under the room temperature.
(3) The aged reaction solution was subjected to centrifugal separation, and then the solid was washed with 100g of deionized water, subjected to centrifugal separation, and repeated 3 times. And finally, drying the solid for 8 hours in vacuum at the temperature of 80 ℃ to obtain the prepared beta-ZnS nano-particle material which is marked as beta-ZnS-2.
(4) 1.20g of urea ((NH) was weighed out2)2CO) was dissolved in 98.80g of deionized water to make a solution with a urea mass content of 1.20 wt%, which was designated as D2 solution.
(5) 1.95g of prepared beta-ZnS-2 is weighed and added into the D2 solution, after being stirred uniformly, the solution is subjected to ultrasonic treatment for 75min under the ultrasonic power of 70W, and the reaction solution is kept stand at room temperature for 8 hours.
(6) And (3) carrying out centrifugal separation on the reaction liquid after standing, and roasting the solid for 1.5 hours at 560 ℃ under the vacuum condition to obtain the prepared alpha-ZnS nano-particle material. The label is alpha-ZnS-2.
Example 3
(1) Weighing 7.14g Zn (NO)3)2·6H2O was dissolved in 92.86g of deionized water to make Zn (NO)3)2The solution with a mass content of 4.54 wt.% is designated as A3 solution. 5.76g of Na were weighed2S·6H2O was dissolved in 94.24g of deionized water to prepare Na2The solution with an S content of 1.87 wt.% was designated as B3 solution. 2.02g CsCl was weighed out and dissolved in 47.98g deionized water to prepare a solution with CsCl mass content of 4.04 wt%, which was denoted as C3 solution.
(2) C3 is dripped into A3 liquid under the condition of room temperature, the B3 liquid is slowly dripped after the full stirring, the ultrasonic treatment is carried out for 60min under the ultrasonic power of 120W after the dripping, and the reaction liquid is aged for 12 hours under the room temperature.
(3) The aged reaction solution was subjected to centrifugal separation, and then the solid was washed with 100g of deionized water, subjected to centrifugal separation, and repeated 3 times. And finally, drying the solid for 8 hours in vacuum at the temperature of 80 ℃ to obtain the prepared beta-ZnS nano-particle material which is marked as beta-ZnS-3.
(4) 1.44g of urea ((NH) was weighed out2)2CO) was dissolved in 98.56g of deionized water to make a solution with a urea mass content of 1.44 wt%, which was designated as D3 solution.
(5) 2.34g of prepared beta-ZnS-1 is weighed and added into the D3 solution, after being stirred uniformly, the solution is subjected to ultrasonic treatment for 65min under the ultrasonic power of 80W, and the reaction solution is kept stand at room temperature for 8 hours.
(6) And (3) carrying out centrifugal separation on the reaction liquid after standing, and roasting the solid for 1 hour at 600 ℃ under a vacuum condition to obtain the prepared alpha-ZnS nano-particle material. The label is alpha-ZnS-3.
Example 4
(1) 3.57g Zn (NO) are weighed out3)2·6H2O was dissolved in 96.43g of deionized water to prepare Zn (NO)3)2The solution having a mass content of 2.27% by weight is designated as A4 solution. 3.15g (NH) are weighed4)2S was dissolved in 96.85g of deionized water to prepare (NH)4)2The solution with an S content of 0.82 wt% was designated as B4 solution. 0.35g of NaCl was weighed out and dissolved in 49.65g of deionized water to prepare a solution with a NaCl mass content of 0.70 wt%, which was denoted as C4 solution.
(2) C4 is dripped into A4 liquid under the condition of room temperature, the B4 liquid is slowly dripped after the full stirring, the ultrasonic treatment is carried out for 40min under the ultrasonic power of 150W after the dripping is finished, and the reaction liquid is aged for 12 hours under the room temperature.
(3) The aged reaction solution was subjected to centrifugal separation, and then the solid was washed with 100g of deionized water, subjected to centrifugal separation, and repeated 3 times. And finally, drying the solid for 8 hours in vacuum at the temperature of 80 ℃ to obtain the prepared beta-ZnS nano-particle material which is marked as beta-ZnS-4.
(4) 0.72g of urea ((NH) was weighed out2)2CO) dissolved in 99.28g of deionized waterAnd preparing the solution with the urea mass content of 0.72 wt% in the sub-water, and recording the solution as D4 solution.
(5) 1.17g of prepared beta-ZnS-1 is weighed and added into the D4 solution, after being stirred uniformly, the solution is subjected to ultrasonic treatment for 60min under 100W of ultrasonic power, and the reaction solution is kept stand for 8 hours at room temperature.
(6) And (3) carrying out centrifugal separation on the reaction liquid after standing, and roasting the solid for 2 hours at 520 ℃ under the vacuum condition to obtain the prepared alpha-ZnS nano-particle material. The label is alpha-ZnS-4.
Example 5
(1) Weighing 8.05g of ZnSO4·7H2Dissolving O in 91.95g deionized water to obtain ZnSO4The solution with a mass content of 4.52 wt.% was designated as A5 solution. 6.72g of Na were weighed2S·6H2O was dissolved in 93.28g of deionized water to prepare Na2The solution with an S content of 2.19% by weight was designated as B5 solution. Weighing 1.04g of KCl and dissolving in 48.96g of deionized water to prepare a solution with the KCl mass content of 2.08 wt%, and marking as a C5 solution.
(2) C5 is dripped into A5 liquid under the condition of room temperature, the B5 liquid is slowly dripped after the full stirring, the ultrasonic treatment is carried out for 50min under the ultrasonic power of 140W after the dripping is finished, and the reaction liquid is aged for 12 hours under the room temperature.
(3) The aged reaction solution was subjected to centrifugal separation, and then the solid was washed with 100g of deionized water, subjected to centrifugal separation, and repeated 3 times. And finally, drying the solid for 8 hours in vacuum at the temperature of 80 ℃ to obtain the prepared beta-ZnS nano-particle material which is marked as beta-ZnS-5.
(4) 1.68g of urea ((NH) was weighed out2)2CO) was dissolved in 98.32g of deionized water to make a solution with a urea mass content of 1.68 wt%, which was designated as D5 solution.
(5) 2.73g of prepared beta-ZnS-1 is weighed and added into the D5 solution, after being stirred uniformly, the solution is subjected to ultrasonic treatment for 70min under the ultrasonic power of 90W, and the reaction solution is kept stand at the room temperature for 8 hours.
(6) And (3) carrying out centrifugal separation on the reaction liquid after standing, and roasting the solid for 1.5 hours at 540 ℃ under the vacuum condition to obtain the prepared alpha-ZnS nano-particle material. The label is alpha-ZnS-5.
Example 6
(1) Weighing 4.03g of ZnSO4·7H2Dissolving O in 95.97g deionized water to obtain ZnSO4The solution with a mass content of 2.26% by weight is designated as A6 solution. 3.65g (NH) are weighed4)2S was dissolved in 96.35g of deionized water to prepare (NH)4)2The solution with an S content of 0.95 wt% was designated as B6 solution. 1.18g of CsCl was weighed out and dissolved in 48.82g of deionized water to prepare a solution with a CsCl mass content of 2.36 wt%, which was designated as C6 solution.
(2) C6 is dripped into A6 liquid under the condition of room temperature, the B6 liquid is slowly dripped after the full stirring, the ultrasonic treatment is carried out for 45min under the ultrasonic power of 150W after the dripping is finished, and the reaction liquid is aged for 12 hours under the room temperature.
(3) The aged reaction solution was subjected to centrifugal separation, and then the solid was washed with 100g of deionized water, subjected to centrifugal separation, and repeated 3 times. And finally, drying the solid for 8 hours in vacuum at the temperature of 80 ℃ to obtain the prepared beta-ZnS nano-particle material which is marked as beta-ZnS-6.
(4) 0.84g of urea ((NH) was weighed out2)2CO) was dissolved in 99.16g of deionized water to make a solution with a urea mass content of 0.84 wt%, denoted as D6 solution.
(5) 1.36g of prepared beta-ZnS-6 is weighed and added into the D6 solution, after being stirred uniformly, the solution is subjected to ultrasonic treatment for 60min under 100W of ultrasonic power, and the reaction solution is kept stand for 8 hours at room temperature.
(6) And (3) carrying out centrifugal separation on the reaction liquid after standing, and roasting the solid for 2 hours at 550 ℃ under the vacuum condition to obtain the prepared alpha-ZnS nano-particle material. Labeled as alpha-ZnS-6.

Claims (8)

1. A preparation method of a hexagonal system alpha-ZnS nano material is characterized by comprising the following specific steps:
(1) respectively preparing soluble zinc salt solution, sulfide salt solution and alkali metal chloride solution;
(2) at room temperature, dropwise adding an alkali metal chloride solution into a soluble zinc salt solution, fully stirring, dropwise adding a sulfide salt solution, performing ultrasonic treatment at the power of 100-150W for 40-60min, and finally aging at room temperature for 8-20 h;
(3) centrifugally separating the reaction liquid aged in the step (2), centrifugally washing the precipitate with deionized water, and finally drying in vacuum at 60-100 ℃ for 5-10 hours to obtain the beta-ZnS nano material;
(4) adding the beta-ZnS nano material into a urea solution, uniformly stirring, carrying out ultrasonic treatment for 60-80min under the power of 60-100W, and finally standing for 5-12 h at room temperature;
(5) and (4) centrifugally separating the reaction liquid obtained in the step (4), and roasting the solid under the vacuum condition to obtain the hexagonal system alpha-ZnS nano material.
2. The preparation method according to claim 1, wherein the soluble zinc salt is one or more of zinc chloride, zinc nitrate and zinc sulfate.
3. The method of claim 1, wherein the sulfide salt is sodium sulfide and/or ammonium sulfide.
4. The preparation method of claim 1, wherein the alkali metal chloride is one or more of sodium chloride, potassium chloride and cesium chloride.
5. The process according to claim 1, wherein the urea solution has a mass concentration of 0.2 to 3%.
6. The method according to claim 1, wherein the β -ZnS nanomaterial is added to the urea solution in an amount of 1-5 wt%.
7. The method as claimed in claim 1, wherein the calcination temperature in step (5) is 500-600 ℃.
8. The method according to claim 1, wherein the calcination time in the step (5) is 1 to 2 hours.
CN202111427183.1A 2021-11-28 2021-11-28 Preparation method of hexagonal system alpha-ZnS nano material Pending CN114132955A (en)

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CN102515285A (en) * 2011-11-23 2012-06-27 陕西科技大学 Preparation method of cobalt sulfide nanocrystalline
US20140255293A1 (en) * 2013-03-11 2014-09-11 Oregon State University Controlled synthesis of nanoparticles using ultrasound in continuous flow
CN104512924A (en) * 2013-10-08 2015-04-15 杜淑卿 Technology for preparing ZnS nano material through solid-phase method
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