CN105696080A - Quaternary chalcogenide semiconductor material, and preparation method and application thereof - Google Patents

Quaternary chalcogenide semiconductor material, and preparation method and application thereof Download PDF

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CN105696080A
CN105696080A CN201610063977.7A CN201610063977A CN105696080A CN 105696080 A CN105696080 A CN 105696080A CN 201610063977 A CN201610063977 A CN 201610063977A CN 105696080 A CN105696080 A CN 105696080A
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semiconductor material
ass
quaternary
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quaternary sulfide
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刘毅
侯佩佩
刘畅
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
    • 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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  • Crystallography & Structural Chemistry (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

The invention discloses a quaternary chalcogenide semiconductor material, and a preparation method and application thereof. The preparation method comprises the following step: by using alkali metal oxyhydroxide, metal silver, a binary solid solution As2S3 and a simple substance S as raw materials and polyethyleneglycol, hydrazine hydrate and ethylenediamine as solvents, carrying out reaction in a 120-140-DEG C drying oven for 5-8 days, thereby obtaining the quaternary chalcogenide semiconductor material. The chemical composition formulae are NaAg2AsS3.H2O and KAg2AsS3. The preparation method has the advantages of high synthesis yield, simple operational process, simple raw materials, low cost, mild reaction conditions, low synthesis temperature and the like. The yield of the quaternary chalcogenides NaAg2AsS3.H2O and KAg2AsS3 is up to 80% or above; and the quaternary chalcogenides have high chemical purity, and can be used for preparing optical semiconductor device materials.

Description

A kind of quaternary sulfide compound semiconductor material and its production and use
Technical field
The invention belongs to inorganic semiconductor material field, be specifically related to a kind of quaternary sulfide compound semiconductor material and its production and use。
Background technology
Chalcogen compound crystalline material is the defect semiconductor material that a class is generally acknowledged, and the difference that this compounds is according to the Nomenclature Composition and Structure of Complexes, it is possible to have important purposes in many-sides such as optical, electrical, magnetic。This compounds has special structure, and ionic bond, covalent bond are mixed, it is possible to constitute various one-dimensional chain, two-dimensional layer or three dimensional skeletal structure。What chalcogen compound was unique becomes key feature to cause that it has abundant structure, according to structure, composition difference, this compound can be insulator, quasiconductor, electronic conductor or even superconductor, and be used widely technically, their study on the synthesis also becomes a very active research field in current Inorganic synthese chemistry。
At present, the typical method preparing quaternary chalcogen compound both at home and abroad mainly includes following three kinds: flux growth metrhod, solid-phase synthesis, solvent-thermal method。(1) flux growth metrhod is the important method of growth crystal, its ultimate principle is that crystalline material is at high temperature dissolved in the flux solution of low melting point, form uniform saturated solution, then pass through slow cooling or other method, enter hypersaturated state and make crystal precipitate out。Flux growth metrhod is similar to solwution method in principle, but by its state again as melt growth method, its shortcoming is that growth cycle is longer, and many fluxs all have toxicity in various degree, and human body is usually worked the mischief by its volatility；The crystal of growth is typically small, is relatively suitable for research and uses；(2) solid state reaction refers to the heterogeneous phase chemical reaction that solid reactant directly participates in, owing to the atom in solid-state, ion, molecule are all fixed on lattice, in the rigidity environment of solid-state, unlike the atom in liquid phase or gas phase, ion, molecule, there is mobility, thus solid state reaction has and is different from liquid reactive uniqueness, both have this qualitative difference in reaction mechanism。Solid state reaction does not use solvent, has high selectivity, high yield, simple technological process and other advantages, it has also become one of people's main method preparing novel solid materials；(3) solvent thermal (hydro-thermal) synthesis is an important branch of Inorganic synthese chemistry, the synthetic method of solvent thermal growth crystal is in an airtight system, under the spontaneous pressure of certain temperature and solvent, reaction raw materials is gradual is synthesized end product。Solvent thermal (hydro-thermal) reaction is the effective ways of synthesis chalcogenide。Solvent thermal (hydro-thermal) synthetic system is typically in imperfect poised state, therefore should synthesize Chemical Problem by this class of non-equilibrium mechanics study。At high temperature under high pressure, the solvent of synthetic reaction is in critical or near critical state, reactant process based prediction model in a solvent has bigger change, solvent thermal chemical reaction is made to differ greatly from normality, the functional material being thus synthesized or crystal, have the good characteristic of self at aspect of performance。
Therefore, developing new solvent-thermal process route, explore new synthetic system, and experimentation is more simple and convenient, reaction condition milder, synthesis temperature is lower, and productivity is higher, will be the important research direction preparing multi-component sulfur compound semiconductor materials future。
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, and a kind of quaternary sulfide compound semiconductor material and its production and use is provided。Concrete technical scheme is as follows:
A kind of quaternary sulfide compound semiconductor material, its chemical constitution formula is: NaAg2AsS3·H2O, belongs to anorthic system, P-1 space group, cell parameterα=74.909 (10) °, β=82.608 (10) °, γ=62.967 (12) °,Z=2, Dc=5.531g/cm3, monocrystal is yellow green lamellar, and energy gap is 2.18eV；
A kind of described quaternary sulfide semiconductor material NaAg2AsS3·H2The preparation method of O, particularly as follows: with mol ratio be 1.0-2.0:1.0-2.0:0.5-1.0:2.0-3.0 sodium hydroxide, argent, binary solid solution orpiment and elemental sulfur for raw material；With volume ratio be 0.5-1.0:2.0-3.0 85wt% hydrazine hydrate and Polyethylene Glycol for solvent；Every 0.334-0.513 gram of raw material is added in the above-mentioned mixed solvent of 2.5-4.0mL, and reacts 5-8 days in 120-140 DEG C of baking oven, after deionized water and washing with alcohol, obtain quaternary sulfide semiconductor material NaAg2AsS3·H2O。
A kind of quaternary sulfide compound semiconductor material, its chemical constitution formula is KAg2AsS3, belong to anorthic system, P-1 space group, cell parameterα=91.205 (9) °, β=92.884 (9) °, γ=90.335 (8) °,Z=4, Dc=4.590g/cm3, monocrystal is yellow lamellar, and energy gap is 2.21eV。
A kind of described quaternary sulfide semiconductor material KAg2AsS3Preparation method, particularly as follows: with mol ratio be 1.0-2.0:1.0-2.0:0.5-1.0:2.0-3.0 potassium hydroxide, argent, binary solid solution orpiment and elemental sulfur for raw material；With volume ratio be 0.5-1.0:0.5-1.0:2.0-3.0 85wt% hydrazine hydrate, ethylenediamine and Polyethylene Glycol for solvent；Every 0.35-0.545 gram of raw material is added in the above-mentioned mixed solvent of 3.0-5.0mL, reacts 5-8 days in 120-140 DEG C of baking oven, after deionized water and washing with alcohol, obtain quaternary sulfide semiconductor material KAg2AsS3。
A kind of described quaternary sulfide compound semiconductor material NaAg2AsS3·H2O、KAg2AsS3Purposes, particularly for preparation Optical Electro-Chemistry semiconductor device or solaode buffer layer material。
Operating process of the present invention is simple and convenient, and cost of material is low, and reaction condition is gentle, and synthesis temperature is low, adopts quaternary sulfide semiconductor material prepared by this method, and productivity can reach more than 80%, and crystallite dimension reaches more than micron order, and chemical purity is high。The energy gap of semi-conducting material respectively 2.18eV and 2.21eV, has potential using value in semiconductor optical。
Accompanying drawing explanation
Fig. 1 is NaAg2AsS3·H2The shape appearance figure of O crystal；
Fig. 2 is KAg2AsS3The shape appearance figure of crystal；
Fig. 3 is NaAg2AsS3·H2The EDX collection of illustrative plates of O crystal, it was shown that Na, the existence of Ag, As and S element and content thereof；
Fig. 4 is KAg2AsS3The EDX collection of illustrative plates of crystal, it was shown that K, the existence of Ag, As and S element and content thereof；
Fig. 5 is NaAg2AsS3·H2The structure chart of O；
Fig. 6 is KAg2AsS3Structure chart；
Fig. 7 is according to NaAg2AsS3·H2What O crystal obtained XRD figure is composed and monocrystalline simulated diffraction figure；
Fig. 8 is according to KAg2AsS3What crystal obtained XRD figure is composed and monocrystalline simulated diffraction figure；
Fig. 9 is NaAg2AsS3·H2O and KAg2AsS3The visible diffuse-reflectance spectrum of solid-state UV。
Detailed description of the invention
Below in conjunction with drawings and Examples the present invention it is further elaborated and illustrates。In the present invention, the technical characteristic of each embodiment is not under having conflicting premise, all can carry out respective combination。
The chemical constitution formula of quaternary sulfide semiconductor material is: AxAgyAszS(x+y+3z)/2, wherein A is the alkali metal atom of balance anion skeleton, and for the one in Na, K, x represents the mole of alkali metal atom, and y represents the mole constituting skeleton transition metal atoms, and z represents the mole constituting skeletal atom。The present invention specifically discloses following two material NaAg2AsS3·H2O and KAg2AsS3, both belong to isomorphism。
A kind of high yield quaternary sulfide compound semiconductor material, its chemical constitution formula is: NaAg2AsS3·H2O, belongs to anorthic system, P-1 space group, cell parameterα=74.909 (10) °, β=82.608 (10) °, γ=62.967 (12) °,Z=2, Dc=5.531g/cm3, monocrystal is yellow green lamellar, and energy gap is 2.18eV；
Described quaternary sulfide semiconductor material NaAg2AsS3·H2The preparation method of O: with mol ratio be 1.0-2.0:1.0-2.0:0.5-1.0:2.0-3.0 sodium hydroxide, argent, binary solid solution orpiment and elemental sulfur for raw material；With volume ratio be 0.5-1.0:2.0-3.0 85wt% hydrazine hydrate and PEG400 for solvent；Every 0.334-0.513 gram of raw material is added in the mixed solvent of the above-mentioned hydrazine hydrate of 2.5-4.0mL and PEG400, and react 5-8 days in 120-140 DEG C of baking oven, after deionized water and washing with alcohol, obtain quaternary sulfide semiconductor material NaAg2AsS3·H2O。
Another kind of high yield quaternary sulfide compound semiconductor material, its chemical constitution formula is KAg2AsS3, belong to anorthic system, P-1 space group, cell parameterα=91.205 (9) °, β=92.884 (9) °, γ=90.335 (8) °,Z=4, Dc=4.590g/cm3, monocrystal is yellow lamellar, and energy gap is 2.21eV。
Described quaternary sulfide semiconductor material KAg2AsS3Preparation method: with mol ratio be 1.0-2.0:1.0-2.0:0.5-1.0:2.0-3.0 potassium hydroxide, argent, binary solid solution orpiment and elemental sulfur for raw material；With volume ratio be 0.5-1.0:0.5-1.0:2.0-3.0 85wt% hydrazine hydrate, ethylenediamine and PEG400 for solvent；Every 0.35-0.545 gram of raw material is added in the mixed solvent of the above-mentioned hydrazine hydrate of 3.0-5.0mL, ethylenediamine and PEG400, react 5-8 days in 120-140 DEG C of baking oven, after deionized water and washing with alcohol, obtain quaternary sulfide semiconductor material KAg2AsS3。
The preparation method of described binary solid solution arsenic sulfide is: As and the S that mol ratio is 2:3 is loaded quartz ampoule and carries out tube sealing, again the quartz ampoule sealed is put in Muffle furnace, it is to slowly warm up to 650 DEG C, and it is incubated 10 hours, naturally cool to room temperature again, open quartz ampoule by standby for block stock grind into powder。
Embodiment 1
NaAg2AsS3·H2O crystal。Weigh initial feed NaOH2.0mmol (0.080g), Ag1.0mmol (0.107g), As2S30.5mmol (0.123g) and S2.0mmol (0.064g) puts in water heating kettle, adds 85wt% hydrazine hydrate 1.0mL and PEG400 2.0mL, is placed in by water heating kettle at 130 DEG C and reacts 7 days。Reaction opens water heating kettle after terminating, and takes out product, respectively with distilled water and absolute ethanol washing 2 times, obtains yellow green flat crystal, and productivity is 100%, crystallite dimension 160-250 μm (see Fig. 1)。Through single-crystal X-ray diffraction analysis, this crystal composition formula is NaAg2AsS3·H2O, belongs to anorthic system, and space group is P-1 (2),α=74.909 °, β=82.608 °, γ=62.967 °, Z=2,Crystal structure figure is as figure 5 illustrates。EDX elementary analysis shows that crystal is containing tetra-kinds of elements of Na, Ag, As, S, and each constituent content analyzes result consistent (see Fig. 3) than with single crystal diffraction。It is 2.18eV (see Fig. 9) that UV-vis collection of illustrative plates records semi-conducting material energy gap。
Embodiment 2
NaAg2AsS3·H2O crystal。Weigh initial feed NaOH1.0mmol (0.040g), Ag1.0mmol (0.107g), As2S30.5mmol (0.123g) and S2.5mmol (0.080g) puts in water heating kettle, adds 85wt% hydrazine hydrate 1.0mL and PEG400 2.0mL, is placed in by water heating kettle at 130 DEG C and reacts 5 days。Reaction opens water heating kettle after terminating, and takes out product, respectively with distilled water and absolute ethanol washing 2 times, obtains yellow green flat crystal, and productivity is 80%。
Embodiment 3
KAg2AsS3Crystal。Weigh initial feed KOH1.0mmol (0.056g), Ag1.0mmol (0.107g), As2S30.5mmol (0.123g) and S2.0mmol (0.064g) puts in water heating kettle, adds 85wt% hydrazine hydrate 0.5ml, ethylenediamine 0.5ml and PEG400 2.0mL, is placed in by water heating kettle at 130 DEG C and reacts 7 days。Reaction opens water heating kettle after terminating, and takes out product, respectively with distilled water and absolute ethanol washing 2 times, obtains yellow flat crystal, and productivity is 100%, crystallite dimension 100-300 μm (see Fig. 2)。Through single-crystal X-ray diffraction analysis, this crystal composition formula is KAg2AsS3, belonging to anorthic system, space group is P-1 (2),α=91.205 (9) °, β=92.884 (9) °, γ=90.335 (8) °,Z=4, crystal structure figure is as indicated with 6。EDX elementary analysis shows that crystal is containing only tetra-kinds of elements of K, Ag, As, S, and each constituent content analyzes result consistent (see Fig. 4) than with single crystal diffraction。It is 2.21eV (see Fig. 9) that UV-vis collection of illustrative plates records semi-conducting material energy gap。
Embodiment 4
KAg2AsS3Crystal。Weigh initial feed KOH2mmol (0.112g), Ag1.0mmol (0.107g), As2S30.5mmol (0.123g) and S3.0mmol (0.096g) puts in water heating kettle, adds 85wt% hydrazine hydrate 0.5ml, ethylenediamine 0.5ml and PEG400 2mL, is placed in by water heating kettle at 130 DEG C and reacts 8 days。Reaction opens water heating kettle after terminating, and takes out product, respectively with distilled water and absolute ethanol washing 2 times, obtains yellow flat crystal, and productivity is 90%。
Above two quaternary sulfide semiconductor material NaAg2AsS3·H2O and KAg2AsS3Being used equally to prepare optical semiconductor device, optical semiconductor device is solaode buffer layer material。
Embodiment described above is the one preferably scheme of the present invention, and so it is not intended to limiting the invention, the technical scheme that all modes taking equivalent replacement or equivalent transformation obtain, and all falls within protection scope of the present invention。

Claims (5)

1. a quaternary sulfide compound semiconductor material, it is characterised in that its chemical constitution formula is: NaAg2AsS3·H2O, belongs to anorthic system, P-1 space group, cell parameter α=74.909 (10) °, β=82.608 (10) °, γ=62.967 (12) °,Z=2, Dc=5.531g/cm3, monocrystal is yellow green lamellar, and energy gap is 2.18eV。
2. the preparation method of a quaternary sulfide semiconductor material as claimed in claim 1, it is characterised in that with mol ratio be 1.0-2.0:1.0-2.0:0.5:2.0-3.0 sodium hydroxide, argent, binary solid solution orpiment and elemental sulfur for raw material；With volume ratio be 0.5-1.0:2.0-3.0 85wt% hydrazine hydrate and Polyethylene Glycol for solvent；Every 0.334-0.513 gram of raw material is added in the above-mentioned mixed solvent of 2.5-4.0mL, and reacts 5-8 days in 120-140 DEG C of baking oven, after deionized water and washing with alcohol, obtain quaternary sulfide semiconductor material NaAg2AsS3·H2O。
3. a quaternary sulfide compound semiconductor material, it is characterised in that its chemical constitution formula is KAg2AsS3, belong to anorthic system, P-1 space group, cell parameter α=91.205 (9) °, β=92.884 (9) °, γ=90.335 (8) °, Z=4, Dc=4.590g/cm3, monocrystal is yellow lamellar, and energy gap is 2.21eV。
4. the preparation method of a quaternary sulfide semiconductor material as claimed in claim 3, it is characterised in that with mol ratio be 1.0-2.0:1.0-2.0:0.5:2.0-3.0 potassium hydroxide, argent, binary solid solution orpiment and elemental sulfur for raw material；With volume ratio be 0.5-1.0:0.5-1.0:2.0-3.0 85wt% hydrazine hydrate, ethylenediamine and Polyethylene Glycol for solvent；Every 0.35-0.545 gram of raw material is added in the above-mentioned mixed solvent of 3.0-5.0mL, reacts 5-8 days in 120-140 DEG C of baking oven, after deionized water and washing with alcohol, obtain quaternary sulfide semiconductor material KAg2AsS3。
5. the purposes of the quaternary sulfide compound semiconductor material as described in claim 1 or 3, it is characterised in that: it is used for preparing Optical Electro-Chemistry semiconductor device or solaode buffer layer material。
CN201610063977.7A 2016-01-29 2016-01-29 Quaternary chalcogenide semiconductor material, and preparation method and application thereof Pending CN105696080A (en)

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CN111573631A (en) * 2020-05-25 2020-08-25 安阳师范学院 Quaternary copper-containing chalcogenide and preparation method and application thereof

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