CN103626228A - Flaky Bi2S3 powder preparation method - Google Patents

Flaky Bi2S3 powder preparation method Download PDF

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CN103626228A
CN103626228A CN201310643716.9A CN201310643716A CN103626228A CN 103626228 A CN103626228 A CN 103626228A CN 201310643716 A CN201310643716 A CN 201310643716A CN 103626228 A CN103626228 A CN 103626228A
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bismuth
massfraction
powder
value
hours
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CN103626228B (en
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高斐
马笑轩
武怡
张陆萍
陈彦伟
王皓石
宋飞莺
刘生忠
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Shaanxi Normal University
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Shaanxi Normal University
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Abstract

The invention discloses a flaky Bi2S3 powder preparation method. The flaky Bi2S3 powder preparation method comprises the following steps: regulating the pH value of a bismuth source solution to acquire a hydrolysate of the bismuth source, then adding a sulfur source, and reacting under different pH conditions to prepare flaky Bi2S3. According to the invention, reaction can be conducted in a water solution at the presence of the sulfur source and the bismuth source but not a dispersant, a surfactant and the like, and poisonous organic solvents easily contaminating the environment are also not required. Compared with the conventional method, the flaky Bi2S3 powder preparation method is simple to operate and the product appearance is controllable.

Description

A kind of sheet Bi 2s 3the preparation method of powder
Technical field
The invention belongs to the preparing technical field of bismuth sulfide nano particle, be specifically related to a kind of sheet Bi 2s 3the preparation method of powder.
Background technology
Nano material, due to the singularity of its size, has many peculiar physicochemical property, is widely used in recent years the fields such as medicine, chemical industry, weaving, aerospace, military affairs and electronics.Bi 2s 3be a kind of direct narrow bandgap semiconductor material, its energy gap is 1.3eV, is widely used in photocell material, photorectifier material, sensor and catalytic field.
At present, the preparation method of bismuth sulfide nano material mainly contains: via sol-gel template method, the precipitator method, microemulsion method, hydrothermal method, solvent-thermal method, gammairradiation method, microwave method, circumfluence method and template, prepared particulate state, bar-shaped, banded, hedgehog and flower-shaped bismuth sulfide.Although adopt aforesaid method, can prepare the Bi of pattern uniqueness 2s 3nano material, but also there is a lot of weak points: and microemulsion method, hydrothermal method, solvent-thermal method be unable to do without special tensio-active agent or solvent, and solvent is toxic, easily causes environmental pollution; Gammairradiation method, microwave method, circumfluence method and template be unable to do without special equipment.These weak points have limited Bi 2s 3the industrial production of nano material and large-scale application.
Summary of the invention
Technical problem to be solved by this invention is to overcome the Bi of existing pattern uniqueness 2s 3the deficiency of preparation method of nano material, provides a kind of simple to operate, only needs ,Bi source, sulphur source, without organic solvent toxic, easy contaminate environment, under cold condition, can be prepared into sheet Bi 2s 3the method of powder.
Solving the problems of the technologies described above adopted technical scheme is: by bismuth source, be that 1g:1～1.5mL mixes with concentrated acid by quality-volume ratio, add distilled water, be mixed with the bismuth source solution of 0.12～0.24mol/L, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 2～4 of bismuth source solution, 60～80 ℃ standing 6～8 hours, the ultrasonic suspension liquid that is dispersed into, according to the mol ratio of bismuth atom and sulphur atom, be 1:2～3, to the sulphur source aqueous solution that adds 0.24～0.36mol/L in suspension liquid, stir, the ammoniacal liquor that is 22%～25% with massfraction or dense acid for adjusting pH value to 2～9, 60～80 ℃ standing 36～48 hours, be cooled to room temperature, with absolute ethanol washing, centrifugal, dry, obtain sheet Bi 2s 3powder.
Above-mentioned bismuth source is Bismuth trinitrate or bismuth chloride; Concentrated acid is that massfraction is the aqueous nitric acid that 37% aqueous hydrochloric acid or massfraction are 65%; Sulphur source is thioacetamide or Sulfothiorine.
Above-mentioned sheet Bi 2s 3in the preparation method of powder, the aqueous hydrochloric acid that is preferably 37% by bismuth source with massfraction is that 1g:1～1.5mL mixes by quality-volume ratio, add distilled water, be mixed with the bismuth source solution of 0.12mol/L, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 2～3 of bismuth source solution, 80 ℃ standing 8 hours, the ultrasonic suspension liquid that is dispersed into, according to the mol ratio of bismuth atom and sulphur atom, be 1:3, to the sulphur source aqueous solution that adds 0.36mol/L in suspension liquid, stir, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 3 or 9, 80 ℃ standing 48 hours, be cooled to room temperature, with absolute ethanol washing, centrifugal, dry, obtain sheet Bi 2s 3powder.
Above-mentioned sheet Bi 2s 3in the preparation method of powder, or the aqueous hydrochloric acid that is preferably 37% by bismuth source with massfraction is that 1g:1～1.5mL mixes by quality-volume ratio, add distilled water, be mixed with the bismuth source solution of 0.12mol/L, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2.5 of bismuth source solution, 60 ℃ standing 8 hours, the ultrasonic suspension liquid that is dispersed into, according to the mol ratio of bismuth atom and sulphur atom, be 1:3, to the sulphur source aqueous solution that adds 0.36mol/L in suspension liquid, stir, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 4～7.5, 60 ℃ standing 48 hours, be cooled to room temperature, with absolute ethanol washing, centrifugal, dry, obtain sheet Bi 2s 3powder.
Above-mentioned sheet Bi 2s 3in the preparation method of powder, or the aqueous nitric acid that is preferably 65% by bismuth source with massfraction is that 1g:1～1.5mL mixes by quality-volume ratio, add distilled water, be mixed with the bismuth source solution of 0.12mol/L, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 2～2.5 of bismuth source solution, 60～80 ℃ standing 8 hours, the ultrasonic suspension liquid that is dispersed into, according to the mol ratio of bismuth atom and sulphur atom, be 1:3, to the sulphur source aqueous solution that adds 0.36mol/L in suspension liquid, stir, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 4.5～9, 60～80 ℃ standing 48 hours, be cooled to room temperature, with absolute ethanol washing, centrifugal, dry, obtain sheet Bi 2s 3powder.
The present invention reacts in the aqueous solution, only needs ,Bi source, sulphur source, does not need dispersion agent, tensio-active agent etc., and also without organic solvent toxic, easy contaminate environment, compared with the existing methods, simple to operate, product pattern is controlled.
Accompanying drawing explanation
Fig. 1 is the sheet Bi of embodiment 1 preparation 2s 3the X-ray diffractogram of powder.
Fig. 2 is the sheet Bi of embodiment 1 preparation 2s 3the scanning electron microscope (SEM) photograph of powder.
Fig. 3 is the sheet Bi of embodiment 2 preparations 2s 3the scanning electron microscope (SEM) photograph of powder.
Fig. 4 is the sheet Bi of embodiment 3 preparations 2s 3the scanning electron microscope (SEM) photograph of powder.
Fig. 5 is the sheet Bi of embodiment 4 preparations 2s 3the scanning electron microscope (SEM) photograph of powder.
Fig. 6 is the sheet Bi of embodiment 5 preparations 2s 3the scanning electron microscope (SEM) photograph of powder.
Fig. 7 is the sheet Bi of embodiment 6 preparations 2s 3the scanning electron microscope (SEM) photograph of powder.
Fig. 8 is the sheet Bi of embodiment 7 preparations 2s 3the scanning electron microscope (SEM) photograph of powder.
Fig. 9 is the sheet Bi of embodiment 8 preparations 2s 3the scanning electron microscope (SEM) photograph of powder.
Figure 10 is the sheet Bi of embodiment 9 preparations 2s 3the scanning electron microscope (SEM) photograph of powder.
Figure 11 is the sheet Bi of embodiment 10 preparations 2s 3the scanning electron microscope (SEM) photograph of powder.
Figure 12 is the sheet Bi of embodiment 11 preparations 2s 3the scanning electron microscope (SEM) photograph of powder.
Figure 13 is the sheet Bi of embodiment 12 preparations 2s 3the scanning electron microscope (SEM) photograph of powder.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in more detail, but the invention is not restricted to these embodiment.
Embodiment 1
It is in 37% aqueous hydrochloric acid that 0.582g Bismuth trinitrate is dissolved in to 0.8mL massfraction, add deionized water, be mixed with the bismuth nitrate solution of 10mL0.12mol/L, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 3 of bismuth nitrate solution, heating in water bath to 80 ℃, standing 8 hours of constant temperature, with the ultrasonic dispersion of ultrasonic cleaning instrument 3 minutes, forms suspension liquid; According to the mol ratio of bismuth atom and sulphur atom, be 1:3, to the thioacetyl amine aqueous solution that adds 10mL0.36mol/L in suspension liquid, stir, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 3,80 ℃ standing 48 hours, be cooled to room temperature, with absolute ethanol washing, centrifugation, 60 ℃ are dried 36 hours, obtain sheet Bi 2s 3powder, its X-ray diffractogram is shown in Fig. 1, scanning electron microscope (SEM) photograph is shown in Fig. 2.As seen from Figure 1, prepared sheet Bi 2s 3powder is orthorhombic structure, and the unit cell parameters of crystal on tri-change in coordinate axis direction of XYZ is respectively 1.113nm, 1.127nm and 0.398nm, as seen from Figure 2, and sheet Bi 2s 3length be 4～7 μ m, wide be 2～4 μ m, the thick 160 ± 10nm of sheet.
Embodiment 2
In the present embodiment, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2 of bismuth nitrate solution, adds after thioacetyl amine aqueous solution, and the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 2, and other step is identical with embodiment 1, obtains sheet Bi 2s 3powder, its scanning electron microscope (SEM) photograph is shown in Fig. 3.
Embodiment 3
In the present embodiment, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2.5 of bismuth nitrate solution, adds after thioacetyl amine aqueous solution, and the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 5.5, and other step is identical with embodiment 1, obtains sheet Bi 2s 3powder, its scanning electron microscope (SEM) photograph is shown in Fig. 4.
Embodiment 4
In the present embodiment, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2.5 of bismuth nitrate solution, adds after thioacetyl amine aqueous solution, and the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 9, and other step is identical with embodiment 1, obtains sheet Bi 2s 3powder, its scanning electron microscope (SEM) photograph is shown in Fig. 5.
Embodiment 5
It is in 65% aqueous nitric acid that 0.582g Bismuth trinitrate is dissolved in to 0.8mL massfraction, add deionized water, be mixed with the bismuth nitrate solution of 10mL0.12mol/L, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2.5 of bismuth nitrate solution, heating in water bath to 80 ℃, standing 8 hours of constant temperature, with the ultrasonic dispersion of ultrasonic cleaning instrument 10 minutes, forms suspension liquid; According to the mol ratio of bismuth atom and sulphur atom, be 1:3, to the thioacetyl amine aqueous solution that adds 10mL0.36mol/L in suspension liquid, stir, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 6.5,80 ℃ standing 48 hours, be cooled to room temperature, with absolute ethanol washing, centrifugation, 60 ℃ are dried 36 hours, obtain sheet Bi 2s 3powder, its scanning electron microscope (SEM) photograph is shown in Fig. 6.
Embodiment 6
In the present embodiment, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2.5 of bismuth nitrate solution, adds after thioacetyl amine aqueous solution, and the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 8.5, and other step is identical with embodiment 5, obtains sheet Bi 2s 3powder, its scanning electron microscope (SEM) photograph is shown in Fig. 7.
Embodiment 7
In the present embodiment, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2.5 of bismuth nitrate solution, 60 ℃ standing 8 hours, add after thioacetyl amine aqueous solution, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 2.5,60 ℃ standing 48 hours, other step is identical with embodiment 1, obtains sheet Bi 2s 3powder, its scanning electron microscope (SEM) photograph is shown in Fig. 8.
Embodiment 8
In the present embodiment, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2.5 of bismuth nitrate solution, 60 ℃ standing 8 hours, add after thioacetyl amine aqueous solution, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 4,60 ℃ standing 48 hours, other step is identical with embodiment 1, obtains sheet Bi 2s 3powder, its scanning electron microscope (SEM) photograph is shown in Fig. 9.
Embodiment 9
In the present embodiment, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2.5 of bismuth nitrate solution, 60 ℃ standing 8 hours, add after thioacetyl amine aqueous solution, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 7.5,60 ℃ standing 48 hours, other step is identical with embodiment 1, obtains sheet Bi 2s 3powder, its scanning electron microscope (SEM) photograph is shown in Figure 10.
Embodiment 10
In the present embodiment, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2.5 of bismuth nitrate solution, 60 ℃ standing 8 hours, add after thioacetyl amine aqueous solution, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 4.5,60 ℃ standing 48 hours, other step is identical with embodiment 5, obtains sheet Bi 2s 3powder, its scanning electron microscope (SEM) photograph is shown in Figure 11.
Embodiment 11
In the present embodiment, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2.5 of bismuth nitrate solution, 60 ℃ standing 8 hours, add after thioacetyl amine aqueous solution, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 6,60 ℃ standing 48 hours, other step is identical with embodiment 5, obtains sheet Bi 2s 3powder, its scanning electron microscope (SEM) photograph is shown in Figure 12.
Embodiment 12
In the present embodiment, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2.5 of bismuth nitrate solution, 60 ℃ standing 8 hours, add after thioacetyl amine aqueous solution, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 9,60 ℃ standing 48 hours, other step is identical with embodiment 5, obtains sheet Bi 2s 3powder, its scanning electron microscope (SEM) photograph is shown in Figure 13.
Embodiment 13
It is in 65% aqueous nitric acid that 1.164g Bismuth trinitrate is dissolved in to 1.8mL massfraction, add deionized water, be mixed with the bismuth nitrate solution of 10mL0.24mol/L, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 4 of bismuth nitrate solution, heating in water bath to 80 ℃, standing 6 hours of constant temperature, with the ultrasonic dispersion of ultrasonic cleaning instrument 10 minutes, forms suspension liquid; According to the mol ratio of bismuth atom and sulphur atom, be 1:2, to the thioacetyl amine aqueous solution that adds 20mL0.24mol/L in suspension liquid, stir, the aqueous nitric acid that is 65% with massfraction regulates pH value to 2,80 ℃ standing 36 hours, be cooled to room temperature, with absolute ethanol washing, centrifugation, 60 ℃ are dried 36 hours, obtain sheet Bi 2s 3powder.
Embodiment 14
In embodiment 1～13, Bismuth trinitrate used is replaced with equimolar bismuth chloride, and thioacetamide is replaced with equimolar Sulfothiorine, and other step is identical with corresponding embodiment, obtains sheet Bi 2s 3powder.

Claims (4)

1. a sheet Bi 2s 3the preparation method of powder, it is characterized in that: by bismuth source, by quality-volume ratio, be that 1g:1～1.5mL mixes with concentrated acid, add distilled water, be mixed with the bismuth source solution of 0.12～0.24mol/L, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 2～4 of bismuth source solution, 60～80 ℃ standing 6～8 hours, the ultrasonic suspension liquid that is dispersed into, according to the mol ratio of bismuth atom and sulphur atom, be 1:2～3, to the sulphur source aqueous solution that adds 0.24～0.36mol/L in suspension liquid, stir, the ammoniacal liquor that is 22%～25% with massfraction or dense acid for adjusting pH value to 2～9, 60～80 ℃ standing 36～48 hours, be cooled to room temperature, with absolute ethanol washing, centrifugal, dry, obtain sheet Bi 2s 3powder,
Above-mentioned bismuth source is Bismuth trinitrate or bismuth chloride; Concentrated acid is that massfraction is the aqueous nitric acid that 37% aqueous hydrochloric acid or massfraction are 65%; Sulphur source is thioacetamide or Sulfothiorine.
2. sheet Bi according to claim 1 2s 3the preparation method of powder, it is characterized in that: the aqueous hydrochloric acid that is 37% with massfraction by bismuth source is that 1g:1～1.5mL mixes by quality-volume ratio, add distilled water, be mixed with the bismuth source solution of 0.12mol/L, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 2～3 of bismuth source solution, 80 ℃ standing 8 hours, the ultrasonic suspension liquid that is dispersed into, according to the mol ratio of bismuth atom and sulphur atom, be 1:3, to the sulphur source aqueous solution that adds 0.36mol/L in suspension liquid, stir, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 3 or 9, 80 ℃ standing 48 hours, be cooled to room temperature, with absolute ethanol washing, centrifugal, dry, obtain sheet Bi 2s 3powder.
3. sheet Bi according to claim 1 2s 3the preparation method of powder, it is characterized in that: the aqueous hydrochloric acid that is 37% with massfraction by bismuth source is that 1g:1～1.5mL mixes by quality-volume ratio, add distilled water, be mixed with the bismuth source solution of 0.12mol/L, the ammoniacal liquor that is 22%～25% with massfraction regulates the pH value to 2.5 of bismuth source solution, 60 ℃ standing 8 hours, the ultrasonic suspension liquid that is dispersed into, according to the mol ratio of bismuth atom and sulphur atom, be 1:3, to the sulphur source aqueous solution that adds 0.36mol/L in suspension liquid, stir, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 4～7.5, 60 ℃ standing 48 hours, be cooled to room temperature, with absolute ethanol washing, centrifugal, dry, obtain sheet Bi 2s 3powder.
4. sheet Bi according to claim 1 2s 3the preparation method of powder, it is characterized in that: the aqueous nitric acid that is 65% with massfraction by bismuth source is that 1g:1～1.5mL mixes by quality-volume ratio, add distilled water, be mixed with the bismuth source solution of 0.12mol/L, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 2～2.5 of bismuth source solution, 60～80 ℃ standing 8 hours, the ultrasonic suspension liquid that is dispersed into, according to the mol ratio of bismuth atom and sulphur atom, be 1:3, to the sulphur source aqueous solution that adds 0.36mol/L in suspension liquid, stir, the ammoniacal liquor that is 22%～25% with massfraction regulates pH value to 4.5～9, 60～80 ℃ standing 48 hours, be cooled to room temperature, with absolute ethanol washing, centrifugal, dry, obtain sheet Bi 2s 3powder.
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CN104707628A (en) * 2015-02-27 2015-06-17 济南大学 Bi2S3/Bi2MoO6 compound visible-light-induced photocatalyst as well as preparation method and application thereof
CN104894647A (en) * 2015-04-01 2015-09-09 中国科学院上海高等研究院 Low-thermal conductivity bismuth sulfide polycrystalline thermoelectric material and preparation method thereof
CN104894646A (en) * 2015-04-01 2015-09-09 中国科学院上海高等研究院 Method for improving conductivity of bismuth sulfide polycrystal
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CN104876266A (en) * 2015-04-21 2015-09-02 南京邮电大学 Aqueous-phase preparation method of bismuth sulfide/protein composite nanospheres
CN112299481A (en) * 2020-08-31 2021-02-02 武汉工程大学 Bi2S3Preparation method of (1)
CN112299481B (en) * 2020-08-31 2023-06-16 武汉工程大学 Bi (Bi) 2 S 3 Is prepared by the preparation method of (2)

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