CN109293935B - A kind of quaternary chalcogen compound Ba8Zn4Ga2S15 and its preparation method and use - Google Patents
A kind of quaternary chalcogen compound Ba8Zn4Ga2S15 and its preparation method and use Download PDFInfo
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- 150000001786 chalcogen compounds Chemical group 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 33
- 150000004770 chalcogenides Chemical group 0.000 claims abstract description 26
- 230000005284 excitation Effects 0.000 claims abstract description 5
- 238000005286 illumination Methods 0.000 claims abstract description 3
- 239000011701 zinc Substances 0.000 claims description 45
- -1 chalcogenide compound Chemical class 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 16
- 239000005083 Zinc sulfide Substances 0.000 claims description 15
- 229910052733 gallium Inorganic materials 0.000 claims description 15
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 15
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 14
- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical compound [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 claims description 14
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 13
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
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- 238000007796 conventional method Methods 0.000 description 2
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- 229910052723 transition metal Inorganic materials 0.000 description 2
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- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910007609 Zn—S Inorganic materials 0.000 description 1
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- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
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- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供了一种四元硫属化合物Ba8Zn4Ga2S15及其制备方法与用途，所述四元硫属化合物的分子式为Ba8Zn4Ga2S15。所述四元硫属化合物Ba8Zn4Ga2S15为晶体，所述四元硫属化合物Ba8Zn4Ga2S15晶体的晶体结构属于单斜晶系，空间群为P2(1)/n(no.14)。所述四元硫属化合物Ba8Zn4Ga2S15晶体的晶胞参数分别为a＝13.328(2)，b＝9.0097(4)，c＝13.332(2)，α＝γ＝90°，β＝109.520(5)°，V＝1508.8(2)。测试表明，其能隙约为3.7eV。另外，所述化合物或其晶体还具有荧光性能，在波长为340nm的激发光下，化合物能够发射出波长为600nm的光，有望在白光照明中获得应用。
The invention provides a quaternary chalcogen compound Ba 8 Zn 4 Ga 2 S 15 and a preparation method and application thereof, wherein the molecular formula of the quaternary chalcogen compound is Ba 8 Zn 4 Ga 2 S 15 . The quaternary chalcogen compound Ba 8 Zn 4 Ga 2 S 15 is a crystal, the crystal structure of the quaternary chalcogen compound Ba 8 Zn 4 Ga 2 S 15 crystal belongs to the monoclinic system, and the space group is P2(1) /n(no.14). The unit cell parameters of the quaternary chalcogenide Ba 8 Zn 4 Ga 2 S 15 crystal are respectively a=13.328(2), b=9.0097(4), c=13.332(2), α=γ=90°, β=109.520(5)°, V=1508.8(2). Tests show that its energy gap is about 3.7eV. In addition, the compound or its crystal also has fluorescence properties, and under excitation light with a wavelength of 340 nm, the compound can emit light with a wavelength of 600 nm, which is expected to be applied in white light illumination.
Description
Technical Field
The invention relates to a novel quaternary chalcogen compound Ba8Zn4Ga2S15And a preparation method and application thereof, belonging to the technical field of inorganic solid functional materials.
Background
The functional material is a material having a specific function under the action of light, electricity, magnetism, heat, chemistry, biochemistry or the like. In the application of functional materials, inorganic solid functional materials have made great progress and are always in the leading position, and have been applied to a plurality of devices. The fluorescent material is a material capable of re-radiating photons or electromagnetic waves after absorbing the photons or electromagnetic waves. Specifically, when high-energy short-wavelength light is incident on a substance, electrons in the substance absorb energy and transit from a ground state to a high energy level, and the electrons are unstable at the high energy level, and transit from the high energy level to a low energy level, thereby releasing energy to emit fluorescence. With the development of science and technology, people have more and more researches on fluorescent materials, and the application range of the fluorescent materials is wider and wider. At present, besides being used as dye, the fluorescent material also has wide application in the fields of coating, organic pigment, optical brightening agent, photo-oxidant, chemical and biochemical analysis, anti-counterfeiting mark, medicine tracing and the like.
The chalcogen compound is a potential new-generation inorganic solid functional material due to rich structure and various performances, and is widely applied to the fields of infrared nonlinear optics, thermoelectric conversion, fluorescence, photocatalysis and the like. Studies have shown that d is included10Transition metal chalcogenides tend to have attractive fluorescent properties, for example the semiconductor compounds ZnS, CdS, ZnSe, CdSe may show strong and tunable fluorescent properties at certain particle sizes. Compound K2Cd3(1-x)Mn3xS4(x is more than or equal to 0 and less than or equal to 1) shows stronger luminous performance at room temperature, and the introduction of trace Mn causes an interesting photo-induced red-shift phenomenon. More interestingly, d is contained10The emission wavelength of transition metal chalcogenides can change with temperature, i.e., there is a thermochromic behavior. For example, when the temperature is reduced from 285K to 9K, the compound CdGa2Se4From 582nm to 712 nm. In addition, compared with organic coordination polymers, inorganic solid fluorescent materials have relatively few types at present although they have more stable and stronger fluorescent effects. Therefore, searching or exploring the synthesis of novel efficient fluorescent materials is one of the research hotspots of the current inorganic solid functional materials.
Disclosure of Invention
In order to ameliorate the deficiencies of the prior art, it is an object herein to provide a quaternary chalcogenide Ba8Zn4Ga2S15And a preparation method and application thereof. The four elements of Ba, Zn, Ga and S are combined, and the quaternary chalcogen compound Ba with a novel one-dimensional chain structure is successfully designed and synthesized by a high-temperature solid-phase synthesis method8Zn4Ga2S15. Fluorescence property measurements indicate that the quaternary chalcogenizationThe compounds have excellent fluorescent properties.
The following technical scheme is provided:
a quaternary chalcogen compound with molecular formula of Ba8Zn4Ga2S15。
Wherein the quaternary chalcogenides Ba8Zn4Ga2S15Is a pure phase.
Wherein the quaternary chalcogenides Ba8Zn4Ga2S15Being crystalline, said quaternary chalcogenides Ba8Zn4Ga2S15The crystal structure of the crystal belongs to a monoclinic system, and the space group is P2(1)/n (No. 14).
Wherein the quaternary chalcogenides Ba8Zn4Ga2S15The crystal has unit cell parameters a-13.328 (2), b-9.0097 (4), c-13.332 (2), α - γ -90 °, β -109.520 (5) °, and V-1508.8 (2).
Wherein the quaternary chalcogenides Ba8Zn4Ga2S15Or the crystal of the material is an inorganic solid functional material with fluorescent property.
Wherein the quaternary chalcogenide compound or the crystal thereof can emit red light under ultraviolet light irradiation, for example, can emit light with a wavelength of 600nm under excitation light irradiation with a wavelength of 340 nm.
Wherein the quaternary chalcogenide compound or the crystal thereof has an energy gap of about 3.7 eV.
Wherein the quaternary chalcogen compound or the crystal thereof has a one-dimensional chain structure.
Also provided herein is a method of making the quaternary chalcogenide described above, comprising the steps of: and (3) placing a mixture of raw materials of barium sulfide, zinc sulfide and gallium sulfide under a vacuum condition, and preparing the quaternary chalcogenide by a high-temperature solid-phase method.
In one embodiment of the present invention, the preparation method comprises the steps of: the mixture of raw materials of barium sulfide, zinc sulfide and gallium sulfide is placed under vacuum condition, and is heated to 800-.
Wherein, the mixture of barium sulfide, zinc sulfide and gallium sulfide is put into a graphite crucible for high-temperature solid-phase reaction. The purpose of using a graphite crucible is to prevent reactants from corroding the quartz tube at high temperatures.
Wherein the mixture of the raw materials barium sulfide, zinc sulfide and gallium sulfide is prepared by the conventional method known to the technical personnel in the field.
Wherein the vacuum condition is that the vacuum degree reaches 10-2-10-4Of the order of Pa, e.g. up to 10-3Of the order of Pa.
Wherein, when the temperature is reduced to 200-500 ℃, the temperature is naturally reduced to room temperature, such as 15-35 ℃.
Wherein the quaternary chalcogen compound is washed by ethanol and dried.
Wherein, the quaternary chalcogenide compound obtained by the method is pure phase.
Wherein the quaternary chalcogenide compound obtained by the method is a crystal.
Wherein the molar ratio of barium sulfide, zinc sulfide and gallium sulfide in the raw materials is 8:4: 1.
Also provided herein is the use of the quaternary chalcogenides described above in the field of white light illumination.
The invention has the beneficial effects that:
the quaternary chalcogen compound with a novel one-dimensional chain structure and a preparation method and application thereof are provided, and the molecular formula of the quaternary chalcogen compound is Ba8Zn4Ga2S15. Said quaternary chalcogenides Ba8Zn4Ga2S15Being crystalline, said quaternary chalcogenides Ba8Zn4Ga2S15The crystal structure of the crystal belongs toMonoclinic system, space group is P2(1)/n (No. 14). Said quaternary chalcogenides Ba 8Zn4Ga2S15The crystal has unit cell parameters a-13.328 (2), b-9.0097 (4), c-13.332 (2), α - γ -90 °, β -109.520 (5) °, and V-1508.8 (2). The test shows that the energy gap is about 3.7 eV. In addition, the compound or the crystal thereof has fluorescence property, namely, the compound can emit red light under ultraviolet irradiation, for example, under excitation light with the wavelength of 340 nm, the compound can emit light with the wavelength of 600 nm.
Drawings
FIG. 1 is Ba of example 18Zn4Ga2S15A schematic of the crystal structure of (a);
FIG. 2 is Ba of example 18Zn4Ga2S15The powder X-ray diffraction pattern of (a);
FIG. 3 is Ba of example 18Zn4Ga2S15The experimental energy gap of powder of (1);
FIG. 4 is Ba of example 18Zn4Ga2S15Fluorescence spectrum (a) of (a) and known crystalline Ba6Zn7Ga2S16The fluorescence spectrum (b) of (a).
Detailed Description
The preparation process is further described in detail with reference to the following examples. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the present disclosure. Any technique that may be implemented based on the teachings set forth herein is intended to be within the scope of the protection sought herein.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
Wherein, said Ba6Zn7Ga2S16(also denoted as Ba18Zn21Ga6S48) The specific properties and preparation method thereof are disclosed in Chinese patent document CN107022793AThe contents. Reference may also be made to journal articles Yanyan Li, Pengfei Liu, Liming Wu6Zn7Ga2S16:A Wide Band Gap Sulfide with Phase-Matchable Infrared NLO Properties,Chemistry of Materials. 2017,29(12),5259-5266。
Example 1
Raw materials of barium sulfide (BaS), zinc sulfide (ZnS) and gallium sulfide (Ga)2S3) Fully grinding and uniformly mixing barium sulfide, zinc sulfide and gallium sulfide according to a molar ratio of 8:4:1, weighing 0.5 g of the total weight, and placing the mixture in a graphite crucible. Placing the graphite crucible filled with the raw materials in a quartz reaction tube, and vacuumizing to 10 DEG-3Pa, and fusing and sealing the quartz reaction tube by using oxyhydrogen flame. And (3) putting the sealed quartz reaction tube into a tube furnace with a temperature controller, heating to 850 ℃ after 35h, preserving the temperature for 100h, cooling to 300 ℃ after 110h, then cutting off the power supply of the furnace, and naturally cooling to room temperature. To obtain the compound Ba8Zn4Ga2S15The target crystal of (1).
Example 2
Ba prepared in example 18Zn4Ga2S15And carrying out structural characterization on the crystal material.
X-ray single crystal diffraction of the crystalline material was carried out on a Mercury CCD type single crystal diffractometer with Mo target, K α radiation source (λ 0.07107nm) and test temperature 293K. And it is structurally parsed by Shelxtl software. The results of the crystallographic data are shown in table 1, and the schematic diagram of the crystal structure is shown in fig. 1.
TABLE 1 sample Ba8Zn4Ga2S15Crystallographic data of
As shown in FIG. 1, the compound Ba8Zn4Ga2S15One-dimensional infinite chain [ Zn ]4S10]∞Is composed of a repeating unit Zn4S10Extending in the b direction in a co-apical fashion. IsolatedGaS of4The tetrahedron is uniformly suspended on both sides of the one-dimensional chain. The specific connection mode is GaS4Tetrahedron through common vertex and two common edge ZnS4And (4) tetrahedrally connecting. Repeating unit Zn4S10Is formed by alternately connecting two same tetrahedral dimer in a reverse common edge way. The dimer is formed from Zn (1) S4And Zn (2) S4The tetrahedrons are connected in a shared edge. Zn, Ga and S atoms are tetrahedrally coordinated. Distorted Zn (1) S4The average bond length of the tetrahedra is
With the known Ba2ZnS3(Zn–S：
) Close. Tetrahedral Zn (2) S4Has a bond length in the range of
And K10Zn4Ge4S17The data of (a) is similar. Tetrahedral GaS4Middle Ga-S bond length range
And the known RbGaS2(Ga–S: 
) And (4) approaching. The Ba atom and the S atom are in two coordination modes of 7 and 9, and the bond length of the Ba-S is within the range of
X-ray powder diffraction phase analysis (XRD) of the quaternary chalcogenide compound obtained in example 1 was performed on a MiniFlex type II X-ray diffractometer from Rigaku, Cu target, K α radiation source (λ 0.154184 nm). The powder XRD pattern of the sample of example 1 was compared to the XRD pattern fitted to the corresponding single crystal diffraction data, as shown in figure 2. As can be seen from FIG. 2, the samples The XRD spectrogram is consistent with the XRD spectrogram obtained by fitting single crystal diffraction data, which indicates that the sample Ba is obtained8Zn4Ga2S15Has high crystallinity and purity.
Example 3
For the quaternary chalcogenide compound Ba obtained in example 18Zn4Ga2S15The crystals of (4) were subjected to optical property characterization.
The experimental energy gap of the powder of the sample was characterized on a PE Lambda950 ultraviolet visible (near infrared) absorption or diffuse reflectance spectrometer with the results shown in fig. 3. As can be seen from fig. 3, the experimental energy gap of the powder of the quaternary chalcogenide crystal obtained in example 1 was about 3.7 eV.
Example 4
For the quaternary chalcogenide compound Ba obtained in example 18Zn4Ga2S15The crystals of (4) were subjected to optical property characterization.
The fluorescence properties of the samples were characterized on an FLS980 spectrofluorometer, and the results are shown in fig. 4 (a). As can be seen from FIG. 4 (a), the quaternary chalcogenide crystal obtained in example 1 also has fluorescence properties, and the compound emits light with a wavelength of 600nm under excitation light with a wavelength of 340nm, and the fluorescence intensity is approximately the known crystal Ba under the same test conditions6Zn7Ga2S16(as shown in (b) of fig. 4) by a factor of 11.8.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (18)
1. A quaternary chalcogen compound with molecular formula of Ba8Zn4Ga2S15Said quaternary chalcogenides Ba8Zn4Ga2S15Being crystalline, said quaternary chalcogenides Ba8Zn4Ga2S15The crystal structure of the crystal belongs to monoclinicIs a space group ofP2(1)/nSaid quaternary chalcogenides Ba8Zn4Ga2S15The crystal has unit cell parameters ofa = 13.328(2)，b = 9.0097(4)，c= 13.332(2)，α= γ= 90°，β = 109.520(5)°，V = 1508.8(2)。
2. The quaternary chalcogenide compound of claim 1, wherein the quaternary chalcogenide compound Ba8Zn4Ga2S15Is a pure phase.
3. The quaternary chalcogenide compound according to claim 1 or 2, wherein said quaternary chalcogenide compound Ba8Zn4Ga2S15Is an inorganic solid functional material with fluorescent property.
4. The quaternary chalcogenide compound according to claim 1 or 2, wherein the quaternary chalcogenide compound is capable of emitting red light under ultraviolet light irradiation.
5. The quaternary chalcogenide compound according to claim 4, wherein the quaternary chalcogenide compound is capable of emitting light having a wavelength of 600 nm under irradiation of excitation light having a wavelength of 340 nm.
6. The quaternary chalcogenide compound of claim 1 or 2 having an energy gap of 3.7 eV.
7. The quaternary chalcogenide compound according to claim 1 or 2, having a one-dimensional chain-like structure.
8. A method of making the quaternary chalcogenide compound of any of claims 1-7 comprising the steps of: and (3) placing a mixture of raw materials of barium sulfide, zinc sulfide and gallium sulfide under a vacuum condition, and preparing the quaternary chalcogenide by a high-temperature solid-phase method.
9. The method according to claim 8, comprising in particular the steps of: and (3) placing the mixture of the raw materials of barium sulfide, zinc sulfide and gallium sulfide in a vacuum condition, heating to 800-1200 ℃ after 20-80 h, preserving the heat for not less than 30 h, and then cooling to 200-500 ℃ after 30-150 h to obtain the quaternary chalcogenide.
10. The method according to claim 9, comprising in particular the steps of: and (3) placing the mixture of the raw materials of barium sulfide, zinc sulfide and gallium sulfide in a vacuum condition, heating to 800-350 ℃ after 40-60 h, preserving the heat for not less than 90 h, and then cooling to 250-350 ℃ after 70-135 h to obtain the quaternary chalcogenide.
11. The method according to claim 9, comprising in particular the steps of: and (3) placing the mixture of the raw materials of barium sulfide, zinc sulfide and gallium sulfide in a vacuum condition, heating to 850 ℃ after 50 h, preserving the heat for 150 h, and then cooling to 300 ℃ after 110-130 h to obtain the quaternary chalcogenide.
12. The production method according to any one of claims 8 to 11, wherein a mixture of raw materials of barium sulfide, zinc sulfide and gallium sulfide is placed in a graphite crucible to perform a high-temperature solid-phase reaction.
13. The production method according to any one of claims 8 to 11, wherein the vacuum condition is a degree of vacuum of 10-2 -10-4Of the order of Pa.
14. The method according to any one of claims 8-11, wherein the temperature is naturally decreased to room temperature after the temperature is decreased to 200-500 ℃.
15. The production method according to any one of claims 8 to 11, wherein the molar ratio of barium sulfide, zinc sulfide and gallium sulfide in the raw material is 8: 4: 1.
16. The method of any one of claims 8-11, wherein the method produces a quaternary chalcogenide in pure phase.
17. The method of any one of claims 8-11, wherein the quaternary chalcogenide compound obtained by the method is crystalline.
18. Use of a quaternary chalcogenide according to any of claims 1 to 7 in the field of white light illumination.
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| CN102169910A (en) * | 2011-01-14 | 2011-08-31 | 南开大学 | Thin film solar cell based on sulfur compound nanocrystalline |
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| Title |
|---|
| Ba6Zn7Ga2S16: A Wide Band Gap Sulfide with Phase-Matchable Infrared NLO Properties;Yan-Yan Li等;《American Chemical Society》;20170531;第5259-5266页 * |
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