CN108796613B - Preparation method of W/S/Cu cluster-metal crystal material with third-order nonlinear optical performance and crystal material - Google Patents
Preparation method of W/S/Cu cluster-metal crystal material with third-order nonlinear optical performance and crystal material Download PDFInfo
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Abstract
The invention discloses a preparation method of a W/S/Cu cluster-metal crystal material with third-order nonlinear optical performance and the crystal material. Adding ammonium trithiotungstate and cuprous cyanide into a pyridine solvent, and stirring to obtain an orange solution; adding a pyridine buffer layer on the upper layer of the solution, and then adding an organic solution of calcium nitrate tetrahydrate above the buffer layer; and sealing, crystallizing, filtering, washing and drying to obtain the crystal material. The invention obtains a W/S/Cu cluster-metal crystal material { [ Ca (Py) ]with third-order nonlinear optical performance2(H2O)2][Ca(Py)2][WOS3Cu3(Py)3(CN)3]2·4Py}n. The invention has simple synthesis, mild condition and easy control, and the synthesized raw materials are cheap and easy to obtain; the obtained product has high yield, good chemical and optical stability of the material and good three-order nonlinear optical performance of the material.
Description
Technical Field
The invention belongs to the technical field of nonlinear optical materials, and particularly relates to a preparation method of a W/S/Cu cluster-metal crystal material with third-order nonlinear optical performance and a crystal material.
Background
Researchers have discovered nonlinear optical phenomena such as photoelectric effect, frequency doubling effect, two-photon absorption and the like by using laser excitation materials, and nonlinear optical devices developed by utilizing the effects are widely applied to many aspects such as optical information processing, optical storage, optical computing and laser instruments, laser medical treatment, distance measurement and directional energy weapons and the like. The development of nonlinear optical materials has been targeting high nonlinear optical coefficients, strong nonlinear response, good environmental stability and high quality material properties, and has been extensively and deeply studied in the fields of inorganic nonlinear optical materials, organic small molecule nonlinear optical materials, etc.
Factors influencing the nonlinear optical properties of the W/S/Cu cluster-based coordination polymer include the configuration of a cluster structural unit, the structure of an organic ligand, the connection mode of a cluster metal framework and the like.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above-mentioned technical drawbacks.
Therefore, in one aspect of the invention, the invention overcomes the defects in the prior art and provides a preparation method of a W/S/Cu cluster-metal crystal material with third-order nonlinear optical performance.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of a W/S/Cu cluster-metal crystal material with third-order nonlinear optical performance comprises the following steps,
adding ammonium trithiotungstate and cuprous cyanide into a pyridine solvent, and stirring to form an orange solution;
adding calcium nitrate tetrahydrate into an organic solvent, and stirring to prepare a colorless solution;
and (3) placing the orange solution into a reaction tube, adding a proper amount of pyridine as a buffer layer on the orange solution, slowly adding the colorless solution above the buffer layer, sealing, crystallizing, filtering, washing and drying to obtain the crystal material.
As a preferred scheme of the preparation method of the W/S/Cu cluster-metal crystal material with the third-order nonlinear optical performance, the method comprises the following steps: the molar ratio of the ammonium trithiotungstate to the cuprous cyanide to the calcium nitrate tetrahydrate is 1: 2.5-4: 2-4.
As a preferred scheme of the preparation method of the W/S/Cu cluster-metal crystal material with the third-order nonlinear optical performance, the method comprises the following steps: and adding ammonium trithiotungstate and cuprous cyanide into a pyridine solvent, wherein the volume of the pyridine solvent required by 0.4 mmol of ammonium trithiotungstate is 3-5 ml.
As a preferred scheme of the preparation method of the W/S/Cu cluster-metal crystal material with the third-order nonlinear optical performance, the method comprises the following steps: the calcium nitrate tetrahydrate is added into an organic solvent, wherein the volume of the organic solvent for dissolving 0.8 mmol of calcium nitrate tetrahydrate is 6-10 ml.
As a preferred scheme of the preparation method of the W/S/Cu cluster-metal crystal material with the third-order nonlinear optical performance, the method comprises the following steps: the orange solution is placed in a reaction test tube, a proper amount of pyridine is added to the upper layer of the orange solution to serve as a buffer layer, and the volume ratio of the pyridine buffer layer to the orange solution is 1: 6-10.
As a preferred scheme of the preparation method of the W/S/Cu cluster-metal crystal material with the third-order nonlinear optical performance, the method comprises the following steps: the method comprises the following steps of adding calcium nitrate tetrahydrate into an organic solvent, and stirring to obtain a colorless solution, wherein the organic solvent comprises one or more of methanol, ethanol, isopropanol and acetonitrile.
As a preferred scheme of the preparation method of the W/S/Cu cluster-metal crystal material with the third-order nonlinear optical performance, the method comprises the following steps: the chemical formula of the crystal material is { [ Ca (Py) ]2(H2O)2][Ca(Py)2][WOS3Cu3(Py)3(CN)3]2·4Py}n。
As another aspect of the invention, the invention overcomes the defects in the prior art and provides a W/S/Cu cluster-metal crystal material with third-order nonlinear optical performance.
In order to solve the technical problems, the invention provides the following technical scheme: a W/S/Cu cluster-metal crystalline material having third-order nonlinear optical properties, wherein: the chemical formula of the crystal material is { [ Ca (Py) ]2(H2O)2][Ca(Py)2][WOS3Cu3(Py)3(CN)3]2·4Py}nThe crystal material is a two-dimensional plane structure with double nodes, wherein the central cluster unit is bird nest shaped [ WOS ]3Cu3]+Clusters are connected with three Ca atoms through cyano groups, the Ca atoms are in hexa-coordination, one is connected with four cluster cores to form a tetraconnection, the other is connected with two cluster cores as a linear bridge, and the other coordination sites are respectively formed by solvent pyridineMolecules and water molecules.
The invention has the beneficial effects that: the invention has simple synthesis, mild condition and easy control, and the synthesized raw materials are cheap and easy to obtain; the obtained product has high yield, good chemical and optical stability of the material and good three-order nonlinear optical performance of the material.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 shows the crystal material of the present invention { [ Ca (Py) ]2(H2O)2][Ca(Py)2][WOS3Cu3(Py)3(CN)3]2·4Py}nThe connection mode and the two-dimensional plane structure diagram.
FIG. 2 shows the crystal material of the present invention { [ Ca (Py) ]2(H2O)2][Ca(Py)2][WOS3Cu3(Py)3(CN)3]2·4Py}nThird order nonlinear optical absorption and refraction patterns.
FIG. 3 shows the crystal material prepared by the present invention { [ Ca (Py) ]2(H2O)2][Ca(Py)2][WOS3Cu3(Py)3(CN)3]2·4Py}nPowder X-ray diffraction pattern of (1).
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1:
the preparation method of the W/S/Cu cluster-metal crystal material with the third-order nonlinear optical performance comprises the following steps:
step one, adding 0.4 mmol of ammonium trithiotungstate and 1.2 mmol of cuprous cyanide into 3 ml of pyridine solvent, and stirring to obtain an orange clear solution;
in the second step, 0.8 mmol of calcium nitrate tetrahydrate was added to 8 ml of an isopropyl alcohol solvent and stirred to dissolve to prepare a colorless solution.
And thirdly, placing the orange red solution obtained in the first step on the lower layer of a reaction test tube, adding 0.5 ml of pyridine as a buffer layer, slowly adding the colorless solution obtained in the second step above the buffer layer, sealing, crystallizing, filtering, washing and drying to obtain the crystal material.
Testing of third-order nonlinear optical properties: the prepared crystalline material was ground into a powder, and 1mg of the powder was sampled in 10 ml of acetonitrile and dissolved by sonication. The obtained solution was subjected to Z-scan test with a laser beam having a pulse width of 4ns and a wavelength of 532 nm.
Example 2:
the preparation method of the W/S/Cu cluster-metal crystal material with the third-order nonlinear optical performance comprises the following steps:
step one, adding 0.4 mmol of ammonium trithiotungstate and 1.4 mmol of cuprous cyanide into 3 ml of pyridine solvent, and stirring to obtain an orange clear solution;
in the second step, 1 mmol of calcium nitrate tetrahydrate was added to 10 ml of isopropyl alcohol solvent and stirred to dissolve to obtain a colorless solution.
And thirdly, placing the orange red solution obtained in the first step on the lower layer of a reaction test tube, adding 0.5 ml of pyridine as a buffer layer, slowly adding the colorless solution obtained in the second step above the buffer layer, sealing, crystallizing, filtering, washing and drying to obtain the crystal material.
Testing of third-order nonlinear optical properties: the prepared crystalline material was ground into a powder, and 1mg of the powder was sampled in 10 ml of acetonitrile and dissolved by sonication. The obtained solution was subjected to Z-scan test with a laser beam having a pulse width of 4ns and a wavelength of 532 nm.
Example 3:
the preparation method of the W/S/Cu cluster-metal crystal material with the third-order nonlinear optical performance comprises the following steps:
step one, adding 0.4 mmol of ammonium trithiotungstate and 1.2 mmol of cuprous cyanide into 3 ml of pyridine solvent, and stirring to obtain an orange clear solution;
in the second step, 1.2 mmol of calcium nitrate tetrahydrate was added to 10 ml of acetonitrile solvent and stirred to dissolve it to obtain a colorless solution.
And thirdly, placing the orange red solution obtained in the first step on the lower layer of a reaction test tube, adding 0.4 ml of pyridine as a buffer layer, slowly adding the colorless solution obtained in the second step above the buffer layer, sealing, crystallizing, filtering, washing and drying to obtain the crystal material.
Testing of third-order nonlinear optical properties: the prepared crystalline material was ground into a powder, and 1mg of the powder was sampled in 10 ml of acetonitrile and dissolved by sonication. The obtained solution was subjected to Z-scan test with a laser beam having a pulse width of 4ns and a wavelength of 532 nm.
Example 4:
the preparation method of the W/S/Cu cluster-metal crystal material with the third-order nonlinear optical performance comprises the following steps:
step one, adding 0.4 mmol of ammonium trithiotungstate and 1.2 mmol of cuprous cyanide into 3 ml of pyridine solvent, and stirring to obtain an orange clear solution;
in the second step, 1.0 mmol of calcium nitrate tetrahydrate was added to 10 ml of an ethanol solvent and stirred to dissolve it to prepare a colorless solution.
And thirdly, placing the orange red solution obtained in the first step on the lower layer of a reaction test tube, adding 0.4 ml of pyridine as a buffer layer, slowly adding the colorless solution obtained in the second step above the buffer layer, sealing, crystallizing, filtering, washing and drying to obtain the crystal material.
Testing of third-order nonlinear optical properties: the prepared crystalline material was ground into a powder, and 1mg of the powder was sampled in 10 ml of acetonitrile and dissolved by sonication. The obtained solution was subjected to Z-scan test with a laser beam having a pulse width of 4ns and a wavelength of 532 nm.
Example 5:
the preparation method of the W/S/Cu cluster-metal crystal material with the third-order nonlinear optical performance comprises the following steps:
step one, adding 0.4 mmol of ammonium trithiotungstate and 1.2 mmol of cuprous cyanide into 4 ml of pyridine solvent, and stirring to obtain an orange clear solution;
in the second step, 1.0 mmol of calcium nitrate tetrahydrate was added to 10 ml of methanol solvent and stirred to dissolve it to obtain a colorless solution.
And thirdly, placing the orange red solution obtained in the first step on the lower layer of a reaction test tube, adding 0.4 ml of pyridine as a buffer layer, slowly adding the colorless solution obtained in the second step above the buffer layer, sealing, crystallizing, filtering, washing and drying to obtain the crystal material.
Testing of third-order nonlinear optical properties: the prepared crystalline material was ground into a powder, and 1mg of the powder was sampled in 10 ml of acetonitrile and dissolved by sonication. The obtained solution was subjected to Z-scan test with a laser beam having a pulse width of 4ns and a wavelength of 532 nm.
Example 6:
the preparation method of the W/S/Cu cluster-metal crystal material with the third-order nonlinear optical performance comprises the following steps:
step one, adding 0.4 mmol of ammonium trithiotungstate and 1.3 mmol of cuprous cyanide into 3 ml of pyridine solvent, and stirring to obtain an orange clear solution;
in the second step, 1.6 mmol of calcium nitrate tetrahydrate was added to 10 ml of acetonitrile solvent and stirred to dissolve it to obtain a colorless solution.
And thirdly, placing the orange red solution obtained in the first step on the lower layer of a reaction test tube, adding 0.4 ml of pyridine as a buffer layer, slowly adding the colorless solution obtained in the second step above the buffer layer, sealing, crystallizing, filtering, washing and drying to obtain the crystal material.
Testing of third-order nonlinear optical properties: the prepared crystalline material was ground into a powder, and 1mg of the powder was sampled in 10 ml of acetonitrile and dissolved by sonication. The obtained solution was subjected to Z-scan test with a laser beam having a pulse width of 4ns and a wavelength of 532 nm.
FIG. 1 shows the crystal material of the present invention { [ Ca (Py) ]2(H2O)2][Ca(Py)2][WOS3Cu3(Py)3(CN)3]2·4Py}nThe connection mode and the two-dimensional plane structure diagram. As shown in figure 1, the crystal material of the invention belongs to a two-dimensional plane structure with double nodes, wherein the central cluster unit is bird nest shaped WOS3Cu3]+The clusters are connected with three Ca atoms through cyano groups, the Ca atoms are in six coordination, one is connected with four cluster cores to form four connection, the other is used as a linear bridge to connect two cluster cores, and the other coordination sites are respectively occupied by solvent pyridine molecules and water molecules.
FIG. 2 shows the crystal material of the present invention { [ Ca (Py) ]2(H2O)2][Ca(Py)2][WOS3Cu3(Py)3(CN)3]2·4Py}nThird order nonlinear optical absorption and refraction patterns. As can be seen from the experimental results shown in FIG. 2, the crystalline material prepared according to the present invention { [ Ca (Py) ]2(H2O)2][Ca(Py)2][WOS3Cu3(Py)3(CN)3]2·4Py}nUnder 532nm laser irradiation, there are obvious three-order non-linear optical absorption and refraction signals with absorption coefficient and refraction coefficient separatelyIs 1.5 × 10-11m W-1And 7.0 × 10-18m2W-1The hyperpolarizability is 3.66 × 10-29esu。
FIG. 3 shows the crystal material prepared by the present invention { [ Ca (Py) ]2(H2O)2][Ca(Py)2][WOS3Cu3(Py)3(CN)3]2·4Py}nPowder X-ray diffraction pattern of (1). As can be seen from the experimental results of FIG. 3, the powder X-ray diffraction pattern of the crystalline material prepared by the present invention is substantially consistent with the X-ray diffraction pattern calculated theoretically, which indicates that the crystalline material prepared by the present invention has a very high purity.
The invention has simple synthesis, mild condition and easy control, and the synthesized raw materials are cheap and easy to obtain; the obtained product has high yield, good chemical and optical stability of the material and good three-order nonlinear optical performance of the material.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (5)
1. A preparation method of a W/S/Cu cluster-metal crystal material with third-order nonlinear optical performance is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
adding ammonium trithiotungstate and cuprous cyanide into a pyridine solvent, and stirring to form an orange solution;
adding calcium nitrate tetrahydrate into an organic solvent, and stirring to prepare a colorless solution;
placing the orange solution into a reaction test tube, adding a proper amount of pyridine on the upper layer of the orange solution to serve as a buffer layer, slowly adding the colorless solution above the buffer layer, sealing, crystallizing, filtering, washing and drying to obtain the crystal material;
wherein the molar ratio of the ammonium trithiotungstate to the cuprous cyanide to the calcium nitrate tetrahydrate is 1: 2.5-4: 2-4;
the orange solution is placed in a reaction test tube, a proper amount of pyridine is added to the upper layer of the orange solution to serve as a buffer layer, and the volume ratio of the pyridine buffer layer to the orange solution is 1: 6-10;
the chemical formula of the crystal material is { [ Ca (Py) ]2(H2O)2][Ca(Py)2][WOS3Cu3(Py)3(CN)3]2·4Py}n。
2. The method of preparing a W/S/Cu cluster-metal crystalline material having third-order nonlinear optical properties as claimed in claim 1, wherein: and adding ammonium trithiotungstate and cuprous cyanide into a pyridine solvent, wherein 0.4 mmol of ammonium trithiotungstate is added into the pyridine solvent with the volume of 3-5 ml.
3. The method of preparing a W/S/Cu cluster-metal crystalline material having third-order nonlinear optical properties as claimed in claim 1, wherein: the calcium nitrate tetrahydrate is added into an organic solvent, wherein 0.8 mmol of calcium nitrate tetrahydrate is dissolved in 6-10 ml of the organic solvent.
4. The method of preparing a W/S/Cu cluster-metal crystalline material having third-order nonlinear optical properties as claimed in claim 1, wherein: the method comprises the following steps of adding calcium nitrate tetrahydrate into an organic solvent, and stirring to obtain a colorless solution, wherein the organic solvent comprises one or more of methanol, ethanol, isopropanol and acetonitrile.
5. The W/S/Cu cluster-metal crystal material with third-order nonlinear optical properties prepared by the preparation method of any one of claims 1 to 4, wherein: the chemical formula of the crystal material is { [ Ca (Py) ]2(H2O)2][Ca(Py)2][WOS3Cu3(Py)3(CN)3]2·4Py}nThe crystal material is a binodal crystalDimensional plane structure in which the central cluster unit is bird's nest shaped [ WOS ]3Cu3]+The clusters are connected with three Ca atoms through cyano groups, the Ca atoms are in six coordination, one is connected with four cluster cores to form four connection, the other is used as a linear bridge to connect two cluster cores, and the other coordination sites are respectively occupied by solvent pyridine molecules and water molecules.
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| JPH02179624A (en) * | 1988-12-30 | 1990-07-12 | Idemitsu Kosan Co Ltd | Organic nonlinear optical material |
| CN101295118A (en) * | 2007-04-26 | 2008-10-29 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal boric acid lutetium lanthanum scandium |
| CN105586639A (en) * | 2016-02-29 | 2016-05-18 | 江南大学 | Preparation method of second-order nonlinear optical crystal material {[Tb(NMP)7][WS4Ag3I4]} |
| CN107761172A (en) * | 2017-10-25 | 2018-03-06 | 江南大学 | The preparation of third-order nonlinear optical Mo/Cu/S cage modle cluster base crystalline materials |
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| JPH02179624A (en) * | 1988-12-30 | 1990-07-12 | Idemitsu Kosan Co Ltd | Organic nonlinear optical material |
| CN101295118A (en) * | 2007-04-26 | 2008-10-29 | 中国科学院福建物质结构研究所 | Nonlinear optical crystal boric acid lutetium lanthanum scandium |
| CN105586639A (en) * | 2016-02-29 | 2016-05-18 | 江南大学 | Preparation method of second-order nonlinear optical crystal material {[Tb(NMP)7][WS4Ag3I4]} |
| CN107761172A (en) * | 2017-10-25 | 2018-03-06 | 江南大学 | The preparation of third-order nonlinear optical Mo/Cu/S cage modle cluster base crystalline materials |
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