CN106904652B - A kind of pentatomic sulphur antimonial semi-conducting material and its production and use - Google Patents
A kind of pentatomic sulphur antimonial semi-conducting material and its production and use Download PDFInfo
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Abstract
The invention discloses a kind of pentatomic sulphur antimonial semi-conducting material and its production and use.With alkali metal salt, alkaline earth metal hydroxide, metallic copper, binary solid solution Sb2S3It is raw material with simple substance S, polyethylene glycol, propane diamine, hydrazine hydrate is solvent, is reacted 57 days in 140 DEG C of baking ovens, obtains pentatomic sulphur category compound semiconductor materials.Chemical constitution formula is respectively：K2Ba3Cu2Sb2S10,Rb2Ba3Cu2Sb2S10And Cs2Ba3Cu2Sb2S10, compound of the invention has new skeleton structure, and preparing raw material is simple and cost is low, and reaction condition is gentle, and synthesis temperature is low.The pentatomic sulphur category compound obtained using the present invention can be used for preparing optical semiconductor device or solar cell buffer layer material.
Description
Technical field
The invention belongs to inorganic semiconductor material field, and in particular to a kind of pentatomic sulphur antimonial semi-conducting material and its
Preparation method and purposes.
Background technology
Between in the past few decades, the research of chalcogen compound is never interrupted, due to the rich caused thing of its structure
Physicochemical performance diversity, there is greatly potential answer in fields such as nonlinear optics, ion exchange, photocatalysis, solar cells
With value.5th major element can possess flexible coordination structure due to the presence of lone pair electrons, therefore be commonly used for
Prepare the compound of various new constructions.For possessing 5s2The Sb of electronics pair3+For ion, the structure of antimony and chalcogen composition
Unit [SbIIIQx]3-(x=3,4,5) also it is possible thereby under the regulation and control of different structure directed agents, the positive electricity with organic or inorganic
Lotus unit forms the chalcogen compound of a large amount of configurations.
Alkali and alkaline earth metal ions ion, can be to M due to the difference of its radius and electric charge in chalcogen compoundxQy(M=mistakes
Cross metal Q=chalcogens) connection of construction unit produces Different Effects, so as to change the structure of multi-element compounds.ECDC
Into the inorganic quaternary chalcogen compound such as Cs for including transition metal2Cu2Sb2Se5, K2CuSbS3, Rb2Cu2Sb2S5And
KCu2SbS3Lamellar structure compound of the alkali metal cation between two-dimensional framework is belonged to, but the sulphur antimony synthesized recently
In compound structure, the same ACuSb for including alkali metal cation2S4What (A=Rb, Cs) was presented is three dimensional skeletal structure.Comprising
The compound of alkaline-earth metal synthesizes less, newly to synthesize BaCuSbQ in the past3(Q=S, Se) falls within three-dimensional open-framework.For
Chalcogen compound crystal comprising alkali metal and alkaline-earth metal cation simultaneously, it is most of in current report to show zero
Tie up structure, such as KBaNbS4, K4Ba2(Nb2S11)2, K4Ba[VS4]2, KBa4(BS3)3, K4Ba11(BS3)8S and ABaMQ4(A=
Rb,Cs；M=V, P；Q=S, Se).KBaMSe3(M=As, Sb) is used as wherein unique chalcogen antimonide, K+, Ba2+Ion position
In independent MSe3Between (M=As, Sb) pyrometric cone, equally with zero-dimension structural.As can be seen here, cation is deposited in compound
In mode, the integral skeleton structure of chalcogen compound is affected.
Solvent-thermal method is the means of effective synthesis multi-component sulfur compound.By being had in solvent thermal reaction using difference
Machine amine is as reducing agent, and for different surfaces activating agent as structure directing agent, we can equally obtain the skeleton knot of different dimensions
Structure.New solvent-thermal process route is developed, finds new synthetic system, structure of the synthesis with good physical-chemical performance is mesh
The emphasis of preceding synthesizing new multi-component sulfur compound, and the problem of correlative study concern.
The content of the invention
It is an object of the invention to solve problems of the prior art, and a kind of pentatomic sulphur antimonial is provided and partly led
Body material and preparation method thereof.The concrete technical scheme that the present invention uses is as follows：
Pentatomic sulphur antimonial semi-conducting material, its chemical constitution formula are one of following three kinds, are respectively：
K2Ba3Cu2Sb2S10,Rb2Ba3Cu2Sb2S10And Cs2Ba3Cu2Sb2S10, three kinds of compounds are isomorphism；
Wherein K2Ba3Cu2Sb2S10Belong to monoclinic system, C2/m space groups, cell parameter α=90 °, β=115.257 (13) °, γ=90 °, Z
=2, Dc=4.605g/cm3, monocrystal is that peony is block.
Wherein Rb2Ba3Cu2Sb2S10Belong to monoclinic system, C2/m space groups, cell parameter α=90 °, β=115.992 (11) °, γ=90 °, Z
=2, Dc=4.332g/cm3, monocrystal is that peony is block, energy gap 1.7eV, and photoelectric current is about 4 μ under simulated solar light irradiation
A/cm2。
Wherein Cs2Ba3Cu2Sb2S10Belong to monoclinic system, C2/m space groups, cell parameter α=90 °, β=116.514 (15) °, γ=90 °, Z=2,
Dc=4.524g/cm3, monocrystal is that peony is block.
Pentatomic sulphur antimonial semi-conducting material K2Ba3Cu2Sb2S10Preparation method, be specially：It is 1.0- by mol ratio
1.5：1.3-0.8：0.5-1.0：0.25：2.0-2.5 barium hydroxide, potassium hydroxide, metallic copper, binary solid solution antimony trisulfide and
Elemental sulfur mixes, and with 2.0mL polyethylene glycol (PEG400), 0.5mL 85wt% hydrazine hydrates, 0.5mL propane diamine is solvent, 140
Middle reaction 5-7 days at DEG C, K is obtained after deionized water and ethanol washing2Ba3Cu2Sb2S10。
Pentatomic sulphur antimonial semi-conducting material Rb2Ba3Cu2Sb2S10Preparation method, be specially：It is 1.0 by mol ratio：
1.3-0.8：0.5-1.0：0.25：2.0-2.5 barium hydroxide, rubidium chloride, metallic copper, binary solid solution antimony trisulfide and elemental sulfur
Mixing, with 2.0mL polyethylene glycol (PEG400), 0.5-1.0mL 85wt% hydrazine hydrates, 0-0.5mL propane diamine is solvent, 140
Middle reaction 5-7 days at DEG C, Rb is obtained after deionized water and ethanol washing2Ba3Cu2Sb2S10。
Pentatomic sulphur antimonial semi-conducting material Cs2Ba3Cu2Sb2S10Preparation method, be specially：It is 1.0- by mol ratio
1.5：1.3-0.8：0.5-1.0：0.25：2.0-2.5 barium hydroxide, cesium hydroxide, metallic copper, binary solid solution antimony trisulfide and
Elemental sulfur mixes, and with 2.0mL polyethylene glycol 400s, 0.5mL 85wt% hydrazine hydrates, 0.5mL propane diamine is solvent, at 140 DEG C
Middle reaction 5-7 days, Cs is obtained after deionized water and ethanol washing2Ba3Cu2Sb2S10。
Above-mentioned pentatomic sulphur antimonial semi-conducting material can be used for preparing optical electro-chemistry semiconductor devices or solar cell
Buffer layer material.
Beneficial effects of the present invention：Compound of the synthesis with new construction, cost of material is low, and reaction condition is gentle.Using
Pentatomic sulphur antimonial semi-conducting material prepared by this method, yield can reach~50%.Semi-conducting material Rb2Ba3Cu2Sb2S10
Energy gap be 1.7eV, the photoelectric current under simulated solar irradiation is 4 μ A/cm2, have in terms of semiconductor optical and solar cell
There is potential application value.
Brief description of the drawings
Fig. 1 is a) K2Ba3Cu2Sb2S10,b)Rb2Ba3Cu2Sb2S10And c) Cs2Ba3Cu2Sb2S10The EDX collection of illustrative plates of crystal；
Fig. 2 is Rb2Ba3Cu2Sb2S10The structure chart of crystal；
Fig. 3 is according to Rb2Ba3Cu2Sb2S10The XRD spectrum that crystal obtains and monocrystalline simulated diffraction comparison diagram；
Fig. 4 is Rb2Ba3Cu2Sb2S10The visible diffusing reflection spectrum of solid-state UV；
Fig. 5 is Rb2Ba3Cu2Sb2S10Photoresponse collection of illustrative plates under simulated solar irradiation.
Embodiment
The present invention is further elaborated and illustrated with reference to the accompanying drawings and examples.Each embodiment in the present invention
Technical characteristic can carry out respective combination on the premise of not colliding with each other.
Pentatomic sulphur antimonial semi-conducting material, its chemical constitution formula are respectively：K2Ba3Cu2Sb2S10,
Rb2Ba3Cu2Sb2S10And Cs2Ba3Cu2Sb2S10, three kinds of compounds are isomorphism.
Wherein K2Ba3Cu2Sb2S10Belong to monoclinic system, C2/m space groups, cell parameter α=90 °, β=115.257 (13) °, γ=90 °, Z
=2, Dc=4.605g/cm3, monocrystal is that peony is block.
Wherein Rb2Ba3Cu2Sb2S10Belong to monoclinic system, C2/m space groups, cell parameter α=90 °, β=115.992 (11) °, γ=90 °, Z
=2, Dc=4.332g/cm3, monocrystal is that peony is block, energy gap 1.7eV, and photoelectric current is 4 μ A/ under simulated solar light irradiation
cm2。
Wherein Cs2Ba3Cu2Sb2S10Belong to monoclinic system, C2/m space groups, cell parameter α=90 °, β=116.514 (15) °, γ=90 °, Z=2,
Dc=4.524g/cm3, monocrystal is that peony is block.
Pentatomic sulphur antimonial semi-conducting material K2Ba3Cu2Sb2S10Preparation method, be specially：It is 1.0- by mol ratio
1.5：1.3-0.8：0.5-1.0：0.25：2.0-2.5 barium hydroxide, potassium hydroxide, metallic copper, binary solid solution antimony trisulfide and
Elemental sulfur mixes, and with 2.0mL polyethylene glycol (PEG400), 0.5mL 85wt% hydrazine hydrates, 0.5mL propane diamine is solvent, 140
Middle reaction 5-7 days at DEG C, K is obtained after deionized water and ethanol washing2Ba3Cu2Sb2S10。
Potassium hydroxide in above-mentioned preparation method is replaced with into cesium hydroxide, at 140 DEG C it is middle reaction 5-7 days, through go from
Cs is obtained after sub- water and ethanol washing2Ba3Cu2Sb2S10。
Pentatomic sulphur antimonial semi-conducting material Rb2Ba3Cu2Sb2S10Preparation method, be specially：It is 1.0 by mol ratio：
1.3-0.8：0.5-1.0：0.25：2.0-2.5 barium hydroxide, rubidium chloride, metallic copper, binary solid solution antimony trisulfide and elemental sulfur
Mixing, with 2.0mL polyethylene glycol (PEG400), 0.5-1.0mL 85wt% hydrazine hydrates, 0-0.5mL propane diamine is solvent, 140
Middle reaction 5-7 days at DEG C, Rb is obtained after deionized water and ethanol washing2Ba3Cu2Sb2S10。
Embodiment 1：
K2Ba3Cu2Sb2S10Crystal, weigh initial feed KOH 0.80mmol (0.048g), Ba (OH)2·8H2O
1.00mmol(0.316g)、Cu 0.50mmol(0.032g)、Sb2S30.25mmol (0.085g) and S 2.00mmol
(0.064g) is put into water heating kettle, adds 2.0mL polyethylene glycol (PEG400), 0.5mL 85wt% hydrazine hydrates, 0.5mL the third two
Amine, water heating kettle is placed at 140 DEG C and reacted 7 days.Product is washed 2 times with distilled water and absolute ethyl alcohol respectively, is obtained yield and is
10% peony slab-like crystal.EDX elementary analyses show crystal containing only five kinds of elements of K, Ba, Cu, Sb, S, and each element contains
Measure ratio about 2:3:2:2:10.
Embodiment 2：
K2Ba3Cu2Sb2S10Crystal, weigh initial feed KOH 1.00mmol (0.056g), Ba (OH)2·8H2O
1.00mmol(0.316g)、Cu 1.00mmol(0.064g)、Sb2S30.25mmol (0.085g) and S 2.50mmol
(0.080g) is put into water heating kettle, adds 2.0mL polyethylene glycol (PEG400), 0.5mL 85wt% hydrazine hydrates, 0.5mL the third two
Amine, water heating kettle is placed at 140 DEG C and reacted 7 days.Product is washed 2 times with distilled water and absolute ethyl alcohol respectively, is obtained yield and is
50% peony bulk crystals.EDX elementary analyses show crystal containing only five kinds of elements of K, Ba, Cu, Sb, S, and each element content
Than being about 2:3:2:2:10.(see Fig. 1).Through single-crystal X-ray diffraction analysis, the crystal composition formula is K2Ba3Cu2Sb2S10, wherein
Heavier five kinds of elements of K, Ba, Cu, Sb, S are consistent with EDX elementary analysis results, belong to monoclinic system, C2/m space groups, structure cell
Parameter α=90 °, β=115.257 (13) °, γ=90 °,Z=2, Dc=4.605g/cm3, crystal structure is as shown in Figure 2.
Embodiment 3：
K2Ba3Cu2Sb2S10Crystal, weigh initial feed KOH 1.30mmol (0.073g), Ba (OH)2·8H2O
1.50mmol(0.474g)、Cu 1.00mmol(0.032g)、Sb2S30.25mmol (0.085g) and S 2.50mmol
(0.064g) is put into water heating kettle, adds 2.0mL polyethylene glycol (PEG400), 0.5mL 85wt% hydrazine hydrates, 0.5mL the third two
Amine, water heating kettle is placed at 140 DEG C and reacted 5 days.Product is washed 2 times with distilled water and absolute ethyl alcohol respectively, is obtained yield and is
20% peony bulk crystals.EDX elementary analyses show crystal containing only five kinds of elements of K, Ba, Cu, Sb, S, and each element content
Than being about 2:3:2:2:10.
Embodiment 4：
Rb2Ba3Cu2Sb2S10Crystal, weigh initial feed RbCl 0.80mmol (0.096g), Ba (OH)2·8H2O
1.00mmol(0.316g)、Cu 0.50mmol(0.032g)、Sb2S30.25mmol (0.085g) and S 2.00mmol
(0.064g) is put into water heating kettle, adds 2.0mL polyethylene glycol (PEG400), 0.5mL 85wt% hydrazine hydrates, 0.5mL the third two
Amine, water heating kettle is placed at 140 DEG C and reacted 5 days.Product is washed 2 times with distilled water and absolute ethyl alcohol respectively, is obtained yield and is
30% peony bulk crystals.EDX elementary analyses show crystal containing only five kinds of elements of Rb, Ba, Cu, Sb, S, and each element contains
Measure ratio about 2:3:2:2:10.
Embodiment 5：
Rb2Ba3Cu2Sb2S10Crystal, weigh initial feed RbCl 1.00mmol (0.120g), Ba (OH)2·8H2O
1.00mmol(0.316g)、Cu 1.00mmol(0.064g)、Sb2S30.25mmol (0.085g) and S 2.50mmol
(0.080g) is put into water heating kettle, adds 2.0mL polyethylene glycol (PEG400), 0.5mL 85wt% hydrazine hydrates, 0.5mL the third two
Amine, water heating kettle is placed at 140 DEG C and reacted 7 days.Product is washed 2 times with distilled water and absolute ethyl alcohol respectively, is obtained yield and is
50% peony bulk crystals.EDX elementary analyses show crystal containing only five kinds of elements of Rb, Ba, Cu, Sb, S, and each element contains
Measure ratio about 2:3:2:2:10.(see Fig. 1).Through single-crystal X-ray diffraction analysis, the crystal composition formula is Rb2Ba3Cu2Sb2S10, its
In heavier five kinds of elements of Rb, Ba, Cu, Sb, S it is consistent with EDX elementary analysis results, belong to monoclinic system, C2/m space groups are brilliant
Born of the same parents' parameter α=90 °, β=115.992 (11) °, γ=
90 °,Z=2, Dc=4.332g/cm3, crystal structure is as shown in Figure 2.XRD surveys are carried out to crystal powder
Examination, as a result as shown in Figure 3.It is 1.7eV (see Fig. 4) that UV-vis collection of illustrative plates, which measures semi-conducting material energy gap, and light rings under simulated solar irradiation
Induced current is 4 μ A/cm2(see Fig. 5).
Embodiment 6：
Rb2Ba3Cu2Sb2S10Crystal, weigh initial feed RbCl 1.30mmol (0.156g), Ba (OH)2·8H2O
1.00mmol(0.316g)、Cu 1.00mmol(0.064g)、Sb2S30.25mmol (0.085g) and S 2.50mmol
(0.080g) is put into water heating kettle, adds 2.0mL polyethylene glycol (PEG400), 1.0mL 85wt% hydrazine hydrates, by water heating kettle
It is placed at 140 DEG C and reacts 7 days.Product is washed 2 times with distilled water and absolute ethyl alcohol respectively, obtains the dark red color lump that yield is 30%
Shape crystal.EDX elementary analyses show crystal containing only five kinds of elements of Rb, Ba, Cu, Sb, S, and each element content ratio about 2:3:2:
2:10。
Embodiment 7：
Cs2Ba3Cu2Sb2S10Crystal, weigh initial feed CsOH8H2The aqueous solution 0.536g (0.80mmol) of O 50%,
Ba(OH)2·8H2O 1.00mmol(0.316g)、Cu 0.50mmol(0.032g)、Sb2S30.25mmol (0.085g) and S
2.00mmol (0.064g) is put into water heating kettle, adds 2.0mL polyethylene glycol (PEG400), 0.5mL 85wt% hydrazine hydrates,
0.5mL propane diamine, water heating kettle is placed at 140 DEG C and reacted 5 days.Product is washed 2 times with distilled water and absolute ethyl alcohol respectively, is obtained
Yield is 10% peony bulk crystals.EDX elementary analyses show crystal containing only five kinds of elements of Cs, Ba, Cu, Sb, S, and respectively
Constituent content ratio about 2:3:2:2:10.
Embodiment 8：
Cs2Ba3Cu2Sb2S10Crystal, Cs2Ba3Cu2Sb2S10Crystal, weigh initial feed CsOH8H2The aqueous solution of O 50%
0.670g(0.10mmol)、Ba(OH)2·8H2O 1.00mmol(0.316g)、Cu 1.00mmol(0.064g)、Sb2S3
0.25mmol (0.085g) and S 2.50mmol (0.080g) are put into water heating kettle, add 2.0mL polyethylene glycol (PEG400),
0.5mL 85wt% hydrazine hydrates, 0.5mL propane diamine, water heating kettle is placed at 140 DEG C and reacted 7 days.Product respectively with distilled water and
Absolute ethyl alcohol washs 2 times, obtains the peony bulk crystals that yield is 40%.EDX elementary analyses show crystal containing only Cs, Ba,
Five kinds of elements of Cu, Sb, S, and each element content ratio about 2:3:2:2:10.(see Fig. 1).Through single-crystal X-ray diffraction analysis, the crystalline substance
Body composition formula is Cs2Ba3Cu2Sb2S10, wherein heavier five kinds of elements of Cs, Ba, Cu, Sb, S are consistent with EDX elementary analysis results,
Belong to monoclinic system, C2/m space groups, cell parameter α=
90 °, β=116.514 (15) °, γ=90 °, Z=2, Dc=4.524g/cm3, crystal structure such as Fig. 2 institutes
Show.
Embodiment 9：
Cs2Ba3Cu2Sb2S10Crystal, weigh initial feed CsOH8H2The aqueous solution 0.871g (0.13mmol) of O 50%,
Ba(OH)2·8H2O 1.50mmol(0.474g)、Cu 1.00mmol(0.032g)、Sb2S30.25mmol (0.085g) and S
2.50mmol (0.064g) is put into water heating kettle, adds 2.0mL polyethylene glycol (PEG400), 0.5mL 85wt% hydrazine hydrates,
0.5mL propane diamine, water heating kettle is placed at 140 DEG C and reacted 7 days.Product is washed 2 times with distilled water and absolute ethyl alcohol respectively, is obtained
Yield is 20% peony bulk crystals.EDX elementary analyses show crystal containing only five kinds of elements of Cs, Ba, Cu, Sb, S, and respectively
Constituent content ratio about 2:3:2:2:10.
Embodiment described above is a kind of preferable scheme of the present invention, and so it is not intended to limiting the invention, all
The technical scheme for taking the mode of equivalent substitution or equivalent transformation to be obtained, all falls within protection scope of the present invention.
Claims (5)
1. a kind of pentatomic sulphur antimonial semi-conducting material, it is characterised in that its chemical constitution formula is respectively：
K2Ba3Cu2Sb2S10, Rb2Ba3Cu2Sb2S10And Cs2Ba3Cu2Sb2S10, three kinds of compounds are isomorphism；
Wherein K2Ba3Cu2Sb2S10Belong to monoclinic system, C2/m space groups, cell parameter α=90 °, β=115.257 °, γ=90 °,Z=2, Dc=4.605g/
cm3, monocrystal is that peony is block；
Wherein Rb2Ba3Cu2Sb2S10Belong to monoclinic system, C2/m space groups, cell parameter α=90 °, β=115.992 °, γ=90 °,Z=2, Dc=4.332g/
cm3, monocrystal is that peony is block, energy gap 1.7eV, and photoelectric current is 4 μ A/cm under simulated solar light irradiation2；
Wherein Cs2Ba3Cu2Sb2S10Belong to monoclinic system, C2/m space groups, cell parameter α=90 °, β=116.514 °, γ=90 °,Z=2, Dc=
4.524g/cm3, monocrystal is that peony is block.
2. a kind of preparation method of pentatomic sulphur antimonial semi-conducting material as claimed in claim 1, it is characterised in that will rub
Your ratio is 1.0-1.5：1.3-0.8：0.5-1.0：0.25：2.0-2.5 barium hydroxide, potassium hydroxide, metallic copper, binary solid solution
Body antimony trisulfide and elemental sulfur mixing, using 2.0mL polyethylene glycol 400s, 0.5mL85wt% hydrazine hydrates and 0.5mL propane diamine as solvent,
Middle reaction 5-7 days at 140 DEG C, K is obtained after deionized water and ethanol washing2Ba3Cu2Sb2S10。
3. a kind of preparation method of pentatomic sulphur antimonial semi-conducting material as claimed in claim 1, it is characterised in that will rub
You are than being 1.0：1.3-0.8：0.5-1.0：0.25：2.0-2.5 barium hydroxide, rubidium chloride, metallic copper, binary solid solution vulcanization
Antimony and elemental sulfur mixing, using 2.0mL polyethylene glycol 400s, 0.5-1.0mL85wt% hydrazine hydrates and 0-0.5mL propane diamine as solvent,
Middle reaction 5-7 days at 140 DEG C, Rb is obtained after deionized water and ethanol washing2Ba3Cu2Sb2S10。
4. a kind of preparation method of pentatomic sulphur antimonial semi-conducting material as claimed in claim 1, it is characterised in that will rub
Your ratio is 1.0-1.5：1.3-0.8：0.5-1.0：0.25：2.0-2.5 barium hydroxide, cesium hydroxide, metallic copper, binary solid solution
Body antimony trisulfide and elemental sulfur mixing, using 2.0mL polyethylene glycol 400s, 0.5mL85wt% hydrazine hydrates and 0.5mL propane diamine as solvent,
Middle reaction 5-7 days at 140 DEG C, Cs is obtained after deionized water and ethanol washing2Ba3Cu2Sb2S10。
A kind of 5. purposes of pentatomic sulphur antimonial semi-conducting material as claimed in claim 1, it is characterised in that：For preparing
Optical electro-chemistry semiconductor devices or solar cell buffer layer material.
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