CN114132955A - Preparation method of hexagonal system alpha-ZnS nano material - Google Patents
Preparation method of hexagonal system alpha-ZnS nano material Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000004202 carbamide Substances 0.000 claims abstract description 24
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract 3
- 239000000243 solution Substances 0.000 claims description 86
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000008367 deionised water Substances 0.000 claims description 31
- 229910021641 deionized water Inorganic materials 0.000 claims description 31
- 239000007787 solid Substances 0.000 claims description 20
- 239000012295 chemical reaction liquid Substances 0.000 claims description 16
- 238000009210 therapy by ultrasound Methods 0.000 claims description 16
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- 239000012266 salt solution Substances 0.000 claims description 12
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 150000004763 sulfides Chemical class 0.000 claims description 8
- 150000003751 zinc Chemical class 0.000 claims description 8
- 239000001103 potassium chloride Substances 0.000 claims description 6
- 235000011164 potassium chloride Nutrition 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 6
- 239000011592 zinc chloride Substances 0.000 claims description 5
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical group [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 2
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 229960001763 zinc sulfate Drugs 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 20
- 239000002105 nanoparticle Substances 0.000 abstract description 20
- 238000000926 separation method Methods 0.000 abstract description 20
- 238000006243 chemical reaction Methods 0.000 abstract description 17
- 239000011701 zinc Substances 0.000 abstract description 10
- 239000002351 wastewater Substances 0.000 abstract description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000011593 sulfur Substances 0.000 abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 abstract description 5
- 229910052725 zinc Inorganic materials 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000002270 dispersing agent Substances 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 229910017053 inorganic salt Inorganic materials 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000011858 nanopowder Substances 0.000 abstract description 2
- 239000005416 organic matter Substances 0.000 abstract description 2
- 238000010668 complexation reaction Methods 0.000 abstract 1
- 238000002425 crystallisation Methods 0.000 abstract 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 48
- 229910052950 sphalerite Inorganic materials 0.000 description 45
- 239000007788 liquid Substances 0.000 description 13
- 238000005303 weighing Methods 0.000 description 6
- 239000011734 sodium Substances 0.000 description 5
- 239000011686 zinc sulphate Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000001215 fluorescent labelling Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- -1 photocatalysis Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004597 plastic additive Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
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- 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
-
- 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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- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
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Abstract
本发明公开了一种六方晶系α‑ZnS纳米材料的制备方法。该方法首先以无机锌源和硫源为原料，以碱金属氯化物作为纳米颗粒控制和分散剂，采用超声波法室温下制备出高分散的β‑ZnS纳米颗粒；然后将β‑ZnS纳米颗粒与尿素溶液在超声波作用下进行反应，经离心分离后，在真空条件下高温焙烧，即可制备出α‑ZnS纳米粉体材料。本发明采用无机锌源、硫源、碱金属氯化物、尿素等为原料，因此在生产过程中只有含无机盐的废水，不产生含有机物的废水，废水比较容易处理。本发明采用尿素对β‑ZnS的配位络合和转晶，使得β‑ZnS转变为α‑ZnS的温度大大降低，并且反应工艺流程简单，操作方便，因此具有重要的工业应用价值。
The invention discloses a preparation method of a hexagonal α-ZnS nanomaterial. The method firstly uses inorganic zinc source and sulfur source as raw materials, uses alkali metal chloride as nanoparticle control and dispersant, and adopts ultrasonic method to prepare high-dispersion β-ZnS nanoparticles at room temperature; then the β-ZnS nanoparticles are mixed with The urea solution is reacted under the action of ultrasonic waves, and after centrifugal separation, α-ZnS nano-powder material can be prepared by calcining at high temperature under vacuum conditions. The present invention adopts inorganic zinc source, sulfur source, alkali metal chloride, urea, etc. as raw materials, so in the production process, only waste water containing inorganic salt is produced, and waste water containing organic matter is not produced, and the waste water is relatively easy to handle. The invention adopts urea to coordinate complexation and crystallisation of β-ZnS, so that the temperature at which β-ZnS is converted into α-ZnS is greatly reduced, the reaction process is simple, and the operation is convenient, so it has important industrial application value.
Description
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.
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| CN116621215A (en) * | 2023-06-03 | 2023-08-22 | 山东中教金源精密仪器有限公司 | Continuous preparation method of nano zinc sulfide based on circulating precipitation reactor |
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| CN120117646A (en) * | 2025-04-28 | 2025-06-10 | 艾肯希红外科技(广东)有限公司 | A kind of β-zinc sulfide nanoparticles and its preparation and application |
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