CN105525354A - Quaternary thioarsenate compound semiconductor material as well as preparation method and application thereof - Google Patents

Quaternary thioarsenate compound semiconductor material as well as preparation method and application thereof Download PDF

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CN105525354A
CN105525354A CN201610064506.8A CN201610064506A CN105525354A CN 105525354 A CN105525354 A CN 105525354A CN 201610064506 A CN201610064506 A CN 201610064506A CN 105525354 A CN105525354 A CN 105525354A
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quaternary
compound semiconductor
thioarseniate
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semiconductor materials
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刘毅
刘畅
侯佩佩
郑雪绒
沈亚英
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Zhejiang University ZJU
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B1/00—Single-crystal growth directly from the solid state
    • C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
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Abstract

The invention discloses a quaternary thioarsenate compound semiconductor material as well as a preparation method and an application thereof. Alkaline earth metal hydroxide, metallic silver, binary solid solution As2S3 and elementary substance S are taken as raw materials, hydrazine hydrate is taken as a solvent, the mixture reacts in a drying oven at the temperature of 160 DEG C for 4-7 days, and the quaternary chalcogenide semiconductor material is obtained. The chemical composition formula is BaAgAsS3 and SrAg4As2S6*H2O. The quaternary thioarsenate compound semiconductor material as well as the preparation method and the application thereof have the advantages that the operation process is simple, raw materials are simple and low in cost, the reaction condition is mild, the synthesis temperature is low and the like. The quaternary chalcogenide has the yield of up to 50%, is high in chemical purity and is used for preparing optical semiconductor devices or solar cell transition layer materials.

Description

A kind of quaternary thioarseniate compound semiconductor materials and its production and use
Technical field
The invention belongs to inorganic semiconductor material field, be specifically related to a kind of quaternary thioarseniate compound semiconductor materials and its production and use.
Background technology
FTIR radiation transmittance can be made into the optics such as second harmonic generator, frequency converter, optical parametric oscillator, has important and applies widely, thus cause extensive concern in the field such as laser communications and military technique.Current application more widely oxide compound non-linear optic crystal comprises KTiOPO 4(KTP), β-BaB 2o 4(BBO), LiNbO 3etc., but be confined to ultraviolet-visible light and near-infrared region (LN).In recent years, multi-component sulfur compound-material, because of the constitutional features of its uniqueness and superior physical and chemical performance, is provided with irreplaceable vital role in optical semiconductor field, particularly in mid and far infrared second order nonlinear crystal research direction, as AgGaSe 2, AgGaS 2, GaSe etc.
Relative to ternary chalcogenide thing, quaternary chalcogen compound is made up of more element, the interphase interaction more complicated of element and various, and thus, the kind of crystalline obtained is more, structure is more complicated, performance is more diversified.Wherein structural unit [the As that forms of arsenic and chalcogen iIIqx] 3-(x=3,4,5) are due to As 3+the existence of 4s lone-pair electron, has very unique structural chemistry characteristic, the stereochemical effect of lone-pair electron and As 3+multiple sulphur atom coordination structure can make it to form a large amount of heterogeneities and composition.The physical and chemical performance of material depends on their the Nomenclature Composition and Structure of Complexes, thioarseniate owing to having abundant constitutional features, with [As iIIqx] 3-thioarseniate skeleton construction based on structural unit is in ion-exchange, and photochemical catalysis and non-linear optical field have very large application prospect.The frequency-doubled effect of many new semiconductor crystals can reach object of reference AgGaSe 2decades of times, as Li 1-xna xasS 2, A 3ta 2asS 11(A=K, Rb) etc.
Solvent-thermal method is the means of effective synthesis of ternary or quaternary arsenic chalcogen compound, and uses hydrazine to serve as solvent and strong reductant, can serve as structure directing agent and reaction medium in solvent thermal reaction simultaneously.In the reaction, the strong reducing power of hydrazine can change the chalcogen compound of neutrality into S 2-or S x 2-negatively charged ion is also dissolved.Same, hydrazine can, as part dispersed metal sulfide chain or layer, make us obtain stable low-dimensional skeleton structure.Develop new solvent-thermal process route, find new synthetic system, synthesize the emphasis that the structure with good physical-chemical performance is current synthesizing new multi-component sulfur compound, simultaneously, improving the productive rate of solvent thermal reaction product, simplify experimental procedure, is also the problem that correlative study is paid close attention to.Therefore, select suitable solvent and reaction environment, obtain the crystalline product of high yield, in association area, there is certain meaning.
Summary of the invention
The object of the invention is to solve problems of the prior art, and a kind of quaternary thioarseniate compound semiconductor materials and its production and use is provided.
A kind of quaternary thioarseniate compound semiconductor materials, its chemical constitution formula is respectively: BaAgAsS 3, belong to oblique system, P21/c spacer, unit cell parameters α=90 °, β=102.15 (11) °, γ=90 °, z=4, D c=4.706g/cm 3, single crystal is yellow block, and energy gap is 2.4eV.
A kind of described quaternary thioarseniate compound semiconductor materials BaAgAsS 3preparation method, be specially: be the mixing of the hydrated barta of 1.0-1.5:0.3-1.0:0.25:2.0-2.5, argent, binary solid solution red arsenic and elemental sulfur by mol ratio, every 0.61 ~ 0.86 gram of mixture adds 4mL85wt% hydrazine hydrate, in at 160 DEG C, reaction 4-7 days, obtains BaAgAsS after deionized water and washing with alcohol 3.
A kind of quaternary thioarseniate compound semiconductor materials, its chemical constitution formula is respectively: SrAg 4as 2s 6h 2o, belongs to oblique system, P21/m spacer, unit cell parameters α=90 °, β=115.895 (11) °, γ=90 °, z=2, D c=4.321g/cm 3, single crystal is yellow block, and energy gap is 2.3eV.
A kind of described quaternary thioarseniate compound semiconductor materials SrAg 4as 2s 6h 2the preparation method of O, be specially: be the mixing of the strontium hydroxide of 1.0-1.5:0.2-1.5:0.2-0.25:2.0-2.5, argent, binary solid solution red arsenic and elemental sulfur by mol ratio, every 0.39 ~ 0.69 gram of mixture adds 4mL85wt% hydrazine hydrate, in at 160 DEG C, reaction 4-7 days, obtains SrAg after deionized water and washing with alcohol 4as 2s 6h 2o.
A purposes for above-mentioned two kinds of quaternary thioarseniate compound semiconductor materials, is specially for the preparation of photoelectrochemistry semiconducter device or solar cell buffer layer material.
Beneficial effect of the present invention: synthetic method is simple, raw materials cost is low, and reaction conditions is gentle.Adopting the quaternary thioarseniate compound semiconductor materials prepared of present method, productive rate can reach ~ and 50%.The energy gap of semiconductor material is respectively 2.4 and 2.3eV, has potential using value in semiconductor optical.
Accompanying drawing explanation
Fig. 1 is BaAgAsS 3the shape appearance figure of crystal;
Fig. 2 is SrAg 4as 2s 6h 2the shape appearance figure of O crystal;
Fig. 3 is BaAgAsS 3the EDX collection of illustrative plates of crystal;
Fig. 4 is SrAg 4as 2s 6h 2the EDX collection of illustrative plates of O crystal;
Fig. 5 is BaAgAsS 3the structure iron of crystal;
Fig. 6 is SrAg 4as 2s 6h 2the structure iron of O crystal;
Fig. 7 is according to BaAgAsS 3crystal obtain XRD figure spectrum with monocrystalline simulated diffraction figure;
Fig. 8 is according to SrAg 4as 2s 6h 2o crystal obtain XRD figure spectrum with monocrystalline simulated diffraction figure;
Fig. 9 is BaAgAsS 3the visible diffuse reflection spectrum of solid-state UV;
Figure 10 is SrAg 4as 2s 6h 2the visible diffuse reflection spectrum of solid-state UV of O.
Embodiment
Below in conjunction with drawings and Examples the present invention be further elaborated and illustrate.In the present invention, the technical characteristic of each embodiment is not having under conflicting prerequisite, all can carry out respective combination.
Quaternary thioarseniate compound semiconductor materials, its chemical constitution formula is respectively: BaAgAsS 3, SrAg 4as 2s 6h 2o, both belong to isomorphism.
Wherein BaAgAsS 3belong to oblique system, P21/c spacer, unit cell parameters α=90 °, β=102.15 (11) °, γ=90 °, z=4, D c=4.706g/cm 3, single crystal is yellow block, and energy gap is 2.4eV.
Wherein SrAg 4as 2s 6h 2o belongs to oblique system, P21/m spacer, unit cell parameters α=90 °, β=115.895 (11) °, γ=90 °, z=2, D c=4.321g/cm 3, single crystal is yellow block, and energy gap is 2.3eV.
Described quaternary thioarseniate compound semiconductor materials BaAgAsS 3preparation method: by mol ratio be the hydrated barta of 1.0-1.5:0.3-1.0:0.25:2.0-2.5, argent, binary solid solution red arsenic and elemental sulfur mixing, every 0.61 ~ 0.86 gram of mixture adds 4mL85wt% hydrazine hydrate, in at 160 DEG C, reaction 4-7 days, obtains BaAgAsS after deionized water and washing with alcohol 3.
Described quaternary thioarseniate compound semiconductor materials SrAg 4as 2s 6h 2the preparation method of O: be the mixing of the strontium hydroxide of 1.0-1.5:0.2-1.5:0.2-0.25:2.0-2.5, argent, binary solid solution red arsenic and elemental sulfur by mol ratio, every 0.39 ~ 0.69 gram of mixture adds 4mL85wt% hydrazine hydrate, in at 160 DEG C, reaction 4-7 days, obtains SrAg after deionized water and washing with alcohol 4as 2s 6h 2o.
Embodiment 1:
BaAgAsS 3crystal, takes initial feed Ba (OH) 28H 2o1.50mmol (0.474g), Ag0.30mmol (0.032g), As 2s 30.25mmol (0.063g) and S2.00mmol (0.064g) puts into water heating kettle, then adds 85wt% hydrazine hydrate 4mL, reacts 7 days at water heating kettle being placed in 160 DEG C.Product uses distilled water and absolute ethanol washing 2 times respectively, obtains the yellow bulk crystals that productive rate is 40%.EDX ultimate analysis shows crystal only containing Ba, Ag, As, S tetra-kinds of elements, and each constituent content ratio is about 1:1:1:3.
Embodiment 2:
BaAgAsS 3crystal, takes initial feed Ba (OH) 28H 2o1.50mmol (0.474g), Ag0.50mmol (0.054g), As 2s 30.25mmol (0.063g) and S2.00mmol (0.064g) puts into water heating kettle, then adds 85wt% hydrazine hydrate 4mL, reacts 7 days at water heating kettle being placed in 160 DEG C.Product uses distilled water and absolute ethanol washing 2 times respectively, obtains the yellow bulk crystals that productive rate is 50%.EDX ultimate analysis shows crystal only containing Ba, Ag, As, S tetra-kinds of elements, and each constituent content ratio is about 1:1:1:3 (see Fig. 3).Through single-crystal X-ray diffraction analysis, this crystal composition formula is BaAgAsS 3, wherein heavier Sr, Ag, As, S tetra-kinds of elements are consistent with EDX results of elemental analyses, belong to oblique system, P21/c spacer, unit cell parameters α=90 °, β=102.15 (11) °, γ=90 °, z=4, D c=4.706g/cm 3, crystalline structure as shown in Figure 5.Carry out XRD test to crystal powder, result as shown in Figure 7.It is 2.4eV (see Fig. 9) that UV-vis collection of illustrative plates records semiconductor material energy gap.
Embodiment 3:
BaAgAsS 3crystal, takes initial feed Ba (OH) 28H 2o1.00mmol (0.316g), Ag1.00mmol (0.108g), As 2s 30.25mmol (0.063g) and S2.50mmol (0.080g) puts into water heating kettle, then adds 85wt% hydrazine hydrate 4mL, reacts 4 days at water heating kettle being placed in 160 DEG C.Product uses distilled water and absolute ethanol washing 2 times respectively, obtains the yellow bulk crystals that productive rate is 20%.EDX ultimate analysis shows crystal only containing Ba, Ag, As, S tetra-kinds of elements, and each constituent content ratio is about 1:1:1:3.
Embodiment 4:
SrAg 4as 2s 6h 2o crystal, takes initial feed Sr (OH) 28H 2o1.00mmol (0.266g), Ag0.20mmol (0.022g), As 2s 30.20mmol (0.049g) and S2.00mmol (0.064g) puts into water heating kettle, then adds 85wt% hydrazine hydrate 4mL, reacts 7 days at water heating kettle being placed in 160 DEG C.Product uses distilled water and absolute ethanol washing 2 times respectively, obtains the yellow bulk crystals that productive rate is 30%.EDX ultimate analysis shows crystal only containing Sr, Ag, As, S tetra-kinds of elements, and each constituent content ratio is about 1:4:2:6.
Embodiment 5:
SrAg 4as 2s 6h 2o crystal, takes initial feed Sr (OH) 28H 2o1.50mmol (0.399g), Ag0.3mmol (0.032g), As 2s 30.25mmol (0.063g) and S2.00mmol (0.064g) puts into water heating kettle, then adds 85wt% hydrazine hydrate 4mL, reacts 7 days at water heating kettle being placed in 160 DEG C.Product uses distilled water and absolute ethanol washing 2 times respectively, obtains the yellow bulk crystals that productive rate is 60%.EDX ultimate analysis shows that crystal contains Sr, Ag, As, S tetra-kinds of elements, and each constituent content ratio is about 1:4:2:6 (see Fig. 4).Through single-crystal X-ray diffraction analysis, this crystal composition formula is SrAg 4as 2s 6h 2o, wherein heavier Sr, Ag, As, S tetra-kinds of elements are consistent with EDX results of elemental analyses, belong to oblique system, P21/m spacer, unit cell parameters unit cell parameters α=90 °, β=115.895 (11) °, γ=90 °, z=2, D c=4.321g/cm 3, crystalline structure as shown in Figure 6.Carry out XRD test to crystal powder, result as shown in Figure 8.It is 2.3eV (see Figure 10) that UV-vis collection of illustrative plates records semiconductor material energy gap.
Embodiment 6:
SrAg 4as 2s 6h 2o crystal, takes initial feed Sr (OH) 28H 2o1.50mmol (0.399g), Ag1.50mmol (0.162g), As 2s 30.25mmol (0.063g) and S2.50mmol (0.080g) puts into water heating kettle, then adds 85wt% hydrazine hydrate 4mL, reacts 7 days at water heating kettle being placed in 160 DEG C.Product uses distilled water and absolute ethanol washing 2 times respectively, obtain productive rate be 10% pure yellow bulk crystals and a large amount of inside comprise the not clean crystals of black impurity.EDX ultimate analysis shows crystal only containing Sr, Ag, As, S tetra-kinds of elements, and each constituent content ratio is about 1:4:2:6.
Above-mentioned quaternary thioarseniate compound semiconductor materials BaAgAsS 3, SrAg 4as 2s 6h 2o all can be used for preparation photoelectrochemistry semiconducter device or solar cell buffer layer material.
Above-described embodiment is one of the present invention preferably scheme, and so it is not intended to limiting the invention, and all technical schemes taking the mode of equivalent replacement or equivalent transformation to obtain, all drop in protection scope of the present invention.

Claims (5)

1. a quaternary thioarseniate compound semiconductor materials, is characterized in that, its chemical constitution formula is respectively: BaAgAsS 3, belong to oblique system, P21/c spacer, unit cell parameters α=90 °, β=102.15 (11) °, γ=90 °, z=4, D c=4.706g/cm 3, single crystal is yellow block, and energy gap is 2.4eV.
2. the preparation method of a quaternary thioarseniate compound semiconductor materials as claimed in claim 1, it is characterized in that being the mixing of the hydrated barta of 1.0-1.5:0.3-1.0:0.25:2.0-2.5, argent, binary solid solution red arsenic and elemental sulfur by mol ratio, every 0.61 ~ 0.86 gram of mixture adds 4mL85wt% hydrazine hydrate, in at 160 DEG C, reaction 4-7 days, obtains BaAgAsS after deionized water and washing with alcohol 3.
3. a quaternary thioarseniate compound semiconductor materials, is characterized in that, its chemical constitution formula is respectively: SrAg 4as 2s 6h 2o, belongs to oblique system, P21/m spacer, unit cell parameters α=90 °, β=115.895 (11) °, γ=90 °, z=2, D c=4.321g/cm 3, single crystal is yellow block, and energy gap is 2.3eV.
4. the preparation method of a quaternary thioarseniate compound semiconductor materials as claimed in claim 3, it is characterized in that being the mixing of the strontium hydroxide of 1.0-1.5:0.2-1.5:0.2-0.25:2.0-2.5, argent, binary solid solution red arsenic and elemental sulfur by mol ratio, every 0.39 ~ 0.69 gram of mixture adds 4mL85wt% hydrazine hydrate, in at 160 DEG C, reaction 4-7 days, obtains SrAg after deionized water and washing with alcohol 4as 2s 6h 2o.
5. a purposes for the quaternary thioarseniate compound semiconductor materials as described in claim 1 or 3, is characterized in that: for the preparation of photoelectrochemistry semiconducter device or solar cell buffer layer material.
CN201610064506.8A 2016-01-29 2016-01-29 Quaternary thioarsenate compound semiconductor material as well as preparation method and application thereof Pending CN105525354A (en)

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Cited By (2)

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CN106149059A (en) * 2016-06-20 2016-11-23 浙江大学 Quaternary sulfide semiconductor material and preparation method for concrete sterilization and anticorrosion
CN106423215A (en) * 2016-08-03 2017-02-22 浙江大学 Bacteriostatic and preservative quaternary sulfide semiconductor photocatalytic material for coastal concrete structure, preparation method and application thereof

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CN104862782A (en) * 2015-03-31 2015-08-26 浙江大学 Quaternary sulfide semiconductor material, and preparation method and application thereof
CN105036192A (en) * 2015-06-08 2015-11-11 浙江大学 Quaternary sulfo-antimonate compound semiconductor material as well as preparation method and application thereof
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CN106149059A (en) * 2016-06-20 2016-11-23 浙江大学 Quaternary sulfide semiconductor material and preparation method for concrete sterilization and anticorrosion
CN106423215A (en) * 2016-08-03 2017-02-22 浙江大学 Bacteriostatic and preservative quaternary sulfide semiconductor photocatalytic material for coastal concrete structure, preparation method and application thereof
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Application publication date: 20160427