CN104762661A - A copper-doped metal-organic framework DMMnF single crystal material and a preparing method thereof - Google Patents
A copper-doped metal-organic framework DMMnF single crystal material and a preparing method thereof Download PDFInfo
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- CN104762661A CN104762661A CN201510101491.3A CN201510101491A CN104762661A CN 104762661 A CN104762661 A CN 104762661A CN 201510101491 A CN201510101491 A CN 201510101491A CN 104762661 A CN104762661 A CN 104762661A
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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
- C30B29/54—Organic 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
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
-
- 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
Abstract
A copper-doped metal-organic framework DMMnF single crystal material and a preparing method thereof are disclosed. The material is formed by a DMCu<0.2>Mn<0.8>F single crystal having a dimension of 2.5*2.5*1.5-3.5*3.5*2.0 mm<3>, wherein the mole ratio of copper ions and manganese ions in the compound is 1:4. Agents used are commercial products and free of tedious and complex preparation. By combination of a hydrothermal method and a liquid phase method, the novel metal-organic framework single crystal material is obtained and the single crystal with a larger dimension is obtained. A process is high in controllability and easy in operation. A prepared product is high in purity. The copper-doped DMMnF single crystal material is expected to achieve wide application in the fields of novel metal-organic framework semiconductors, information storage and optical devices.
Description
Technical field
The present invention relates to a kind of magnesium doping metals-organic frame monocrystal material and preparation method thereof, specifically refer to a kind of Cu doping [(CH
3)
2nH
2] Mn (HCOO)
3monocrystal material (is abbreviated as DMCu
0.2mn
0.8f, DM are [(CH
3)
2nH
2]
+ 1, F is [(HCOO)
3]
-3) and preparation method thereof.
Technical background
Metal-organic framework (Metal-Organic Frameworks, MOFs) material is subject to extensive concern because having potential using value in catalysis, Chu Qing and optical element etc., is a focus in current New function investigation of materials field.Due to organic compound have preparation flexibly, the advantage of flexible, the easy cutting of skeleton and the easy aspect such as height of formation anisotropy and low lattice symmetry structure, people attempt, by ferroelectricity organism and magnetic transition metal ionic bond, designing the novel multi-ferroic material based on metal-organic hybrid in recent years.
The discovery of magnetoelectric effect in DMMnF material, shows ferroelectricly to combine organic with magnetic metal ion, greatly will expand the exploration space of multi-ferroic material and magnetoelectric effect.The preparation method of DMMnF mainly contains hydrothermal method, liquid phase method etc.Hydrothermal method refer to sealing pressurized vessel in, using water as solvent, at temperature 100 ~ 400 ° of C, pressure be greater than 0.1MPa until tens to hundreds of MPa condition under, make precursor (raw material) react and crystallization.Namely a special physicochemical environment that cannot obtain in atmospheric conditions is provided, precursor is dissolved fully in reactive system, form atom or molecular growth primitive, nucleation crystallization.The advantages such as it is fast that hydrothermal method has speed of response, and product purity is high, better crystallinity degree, reunion are few.At present, be main by the DMMnF material of water heat transfer mainly with powder crystallite and small monocrystalline, but, be extremely restricted as device application, therefore the growth of how better control DMMnF monocrystalline, make the size of monocrystalline reach the requirement being easy to making devices, and widen its industry application have very important significance.
That studies metal-organic framework materials along with people gos deep into, people are just making great efforts to study fully the magneto-electric coupled mechanism of multiferroic MOFs base monocrystal material, wish magnetic structure and the electronic structure that can be changed Mn position in DMMnF by compound, some metallic elements that adulterate, and Effective Regulation is carried out to its magnetoelectric effect, thus greatly widen the using value of MOFs material.At present, a kind of Cu doping [(CH
3)
2nH
2] Mn (HCOO)
3monocrystal material and preparation method thereof is not also reported.
Summary of the invention
The object of the invention is to adulterate DMMnF monocrystal material and the larger DMCu of size for obtaining novel C u
0.2mn
0.8f monocrystalline, simultaneously this DMCu
0.2mn
0.8the preparation method of F monocrystalline is simple, convenient, provides a kind of Copper-cladding Aluminum Bar metal-organic framework DMMnF monocrystal material and preparation method thereof.
Technical scheme of the present invention is:
A kind of Copper-cladding Aluminum Bar metal-organic framework DMMnF monocrystal material is by being of a size of 2.5 × 2.5 × 1.5 ~ 3.5 × 3.5 × 2.0 mm
3, and in compound, the molar percentage of cupric ion and mn ion is the DMCu of 1:4
0.2mn
0.8f monocrystalline forms.
Described DMCu
0.2mn
0.8f monocrystalline is white translucent crystal, and its chemical formula is [(CH
3)
2nH
2] Cu
0.2mn
0.8(HCOO)
3.
The preparation method of described Copper-cladding Aluminum Bar metal-organic framework DMMnF monocrystal material comprises the steps:
(1) in beaker, add the vitriol oil, acetone, dehydrated alcohol and deionized water successively, respectively ultrasonic cleaning 15 minutes, to remove residual metal ions and organism in beaker, the beaker after cleaning is saved backup;
(2) cupric chloride and Manganous chloride tetrahydrate are taken mixing according to the mol ratio of 1:4, be dissolved in distilled water with DMF, stir and make it fully dissolve; Wherein the volume ratio of DMF and distilled water is 1:1; Needed for every mole of cupric chloride and Manganous chloride tetrahydrate mixture, distilled water consumption is 6mL;
(3) step (2) gained mixing solutions is loaded in reactor, be heated to 135 ~ 145 ° of C after sealing and react, and be incubated 60 ~ 72 hours, then naturally cool to room temperature;
(4) reacted for step (3) saturated clear liquid transfer pipet taken out and load in the cleaned beaker of step (1), then beaker being put into climatic chamber; Set 30 sections of temperature lowering curves, temperature range is 28 ~ 22 ° of C, every section of temperature difference 0.5 ° of C, and every section of temperature range is incubated 2.5 ~ 3 hours, and humidity is 45 ~ 55%;
(5) by the crystal grain of beaker bottom absolute ethanol washing 3 times, Copper-cladding Aluminum Bar metal-organic framework DMMnF monocrystal material within 10 minutes, is obtained in 60 ° of C vacuum-dryings.
The model of described climatic chamber is WHS-70B model.Humidity in described step (4) is controlled by humidifier and climatic chamber.
Beneficial effect:
In preparation process of the present invention, agents useful for same is commerical prod, without the need to loaded down with trivial details preparation; Utilize hydrothermal method and liquid phase method to combine and obtain the larger monocrystalline of size and new copper doping metals-organic frame monocrystal material; Process controllability is strong, easy to operate, and obtained product purity is high.
The DMCu of gained of the present invention
0.2mn
0.8f material, is expected to store in novel metal-organic frame semi-conductor, information and be widely used in optics.
Accompanying drawing explanation
Fig. 1 is the DMCu obtained with the present invention
0.2mn
0.8f monocrystalline digital photograph;
Fig. 2 is the DMCu obtained with the present invention
0.2mn
0.8x-ray diffraction (XRD) spectrogram of F monocrystalline;
Fig. 3 is the DMCu obtained with the present invention
0.2mn
0.8f monocrystalline spectrogram, wherein (a) is the DMCu obtained with the present invention
0.2mn
0.8f monocrystalline XPS composes entirely, and (b) is the DMCu obtained with the present invention
0.2mn
0.8the XPS spectrum figure of F monocrystalline Mn2p; C () is the DMCu obtained with the present invention
0.2mn
0.8the XPS spectrum figure of F monocrystalline Cu2p.
Embodiment
The present invention is further illustrated below in conjunction with example.
The present invention prepares DMCu
0.2mn
0.8f monocrystal material adopts hydrothermal method and liquid phase method to combine method.In beaker, add the vitriol oil, acetone, dehydrated alcohol and deionized water successively, have children outside the state plan cleaning 15 minutes respectively, to remove the impurity such as residual metal ions, organism in beaker, the beaker after cleaning is saved backup.Cupric chloride and Manganous chloride tetrahydrate are taken 2.5 mmol according to the mol ratio of 1:4, is dissolved in 15 mL distilled water with 15 mL DMFs (DMF), stir and make it fully dissolve; Wherein the volume ratio of DMF and distilled water is 1:1.This mixing solutions is loaded in reactor, is heated to 135 ~ 145 ° of C after sealing and reacts, and be incubated 60 ~ 72 hours, then naturally cool to room temperature.Reacted saturated clear liquid transfer pipet taken out and loads in the cleaned beaker of step (1), then beaker being put into climatic chamber; Set 30 sections of temperature lowering curves, temperature range is 28 ~ 22 ° of C, every section of temperature difference 0.5 ° of C, and every section of temperature range is incubated 2.5 ~ 3 hours, and humidity is 45 ~ 55%.By the crystal grain of beaker bottom absolute ethanol washing 3 times, within 10 minutes, obtain the DMCu of white translucent in 60 ° of C vacuum-dryings
0.2mn
0.8f cubic crystal.
Embodiment 1
Cupric chloride and Manganous chloride tetrahydrate are taken 2.5 mmol according to the mol ratio of 1:4, is dissolved in 15 mL distilled water with 15 mL DMFs (DMF), stir and make it fully dissolve; Wherein the volume ratio of DMF and distilled water is 1:1.This mixing solutions is loaded in reactor, is heated to 140 ° of C after sealing and reacts, and be incubated 60 hours, then naturally cool to room temperature.Reacted saturated clear liquid transfer pipet taken out and loads in the cleaned beaker of step (1), then beaker being put into climatic chamber; Set 30 sections of temperature lowering curves, temperature range is 28 ~ 22 ° of C, and every section of temperature difference 0.5 ° of C, every section of temperature range is incubated 2.5 hours, and humidity is 50%.By the crystal grain of beaker bottom absolute ethanol washing 3 times, within 10 minutes, obtain the DMCu of white translucent in 60 ° of C vacuum-dryings
0.2mn
0.8f cubic crystal.
Gained crystal is directly observed (as Fig. 1) under digital camera, can find that crystal is white translucent, be of a size of 2.5 × 2.5 × 1.5 ~ 3.5 × 3.5 × 2.0 mm
3cubic crystal.The XRD analysis of Fig. 2 shows product D MCu
0.2mn
0.8f and the DMMnF basically identical (corresponding to CCDC:246991, crystal data center, Cambridge) that do not adulterate, crystal, along (012) direction oriented growth, forms monocrystalline.In XRD figure spectrum, do not find the diffraction peak of Tubercuprose and other impurity, show that copper is successfully adulterated and enter in the lattice of DMMnF crystal.DMCu can be found out during the XPS of Fig. 3 a composes entirely
0.2mn
0.8containing N, Cu, Mn in F monocrystalline, O, C element, calculates the atomic ratio of product close to 1:0.2:0.8:6:5 through XPS integrating peak areas, and the valent state of Cu, Mn is+divalent (Fig. 3 b, c), shows that the chemical formula of products therefrom is [(CH
3)
2nH
2] Cu
0.2mn
0.8(HCOO)
3.
Embodiment 2
As embodiment 1, cupric chloride and Manganous chloride tetrahydrate are taken 2.5 mmol according to the mol ratio of 1:4, be dissolved in 15 mL distilled water with 15 mL DMFs (DMF), stir and make it fully dissolve; Wherein the volume ratio of DMF and distilled water is 1:1.This mixing solutions is loaded in reactor, is heated to 140 ° of C after sealing and reacts, and be incubated 65 hours, then naturally cool to room temperature.Reacted saturated clear liquid transfer pipet taken out and loads in the cleaned beaker of step (1), then beaker being put into climatic chamber; Set 30 sections of temperature lowering curves, temperature range is 28 ~ 22 ° of C, and every section of temperature difference 0.5 ° of C, every section of temperature range is incubated 2.5 hours, and humidity is 55%.By the crystal grain of beaker bottom absolute ethanol washing 3 times, within 10 minutes, obtain the DMCu of white translucent in 60 ° of C vacuum-dryings
0.2mn
0.8f cubic crystal.The pattern of product is all identical with embodiment 1 with structure.
Embodiment 3
As embodiment 1, cupric chloride and Manganous chloride tetrahydrate are taken 2.5 mmol according to the mol ratio of 1:4, be dissolved in 15 mL distilled water with 15 mL DMFs (DMF), stir and make it fully dissolve; Wherein the volume ratio of DMF and distilled water is 1:1.This mixing solutions is loaded in reactor, is heated to 135 ° of C after sealing and reacts, and be incubated 65 hours, then naturally cool to room temperature.Reacted saturated clear liquid transfer pipet taken out and loads in the cleaned beaker of step (1), then beaker being put into climatic chamber; Set 30 sections of temperature lowering curves, temperature range is 28 ~ 22 ° of C, and every section of temperature difference 0.5 ° of C, every section of temperature range is incubated 3 hours, and humidity is 45%.By the crystal grain of beaker bottom absolute ethanol washing 3 times, within 10 minutes, obtain the DMCu of white translucent in 60 ° of C vacuum-dryings
0.2mn
0.8f cubic crystal.The pattern of product is all identical with embodiment 1 with structure.
Embodiment 4
As embodiment 1, cupric chloride and Manganous chloride tetrahydrate are taken 2.5 mmol according to the mol ratio of 1:4, be dissolved in 15 mL distilled water with 15 mL DMFs (DMF), stir and make it fully dissolve; Wherein the volume ratio of DMF and distilled water is 1:1.This mixing solutions is loaded in reactor, is heated to 135 ° of C after sealing and reacts, and be incubated 70 hours, then naturally cool to room temperature.Reacted saturated clear liquid transfer pipet taken out and loads in the cleaned beaker of step (1), then beaker being put into climatic chamber; Set 30 sections of temperature lowering curves, temperature range is 28 ~ 22 ° of C, and every section of temperature difference 0.5 ° of C, every section of temperature range is incubated 2.5 hours, and humidity is 45%.By the crystal grain of beaker bottom absolute ethanol washing 3 times, within 10 minutes, obtain the DMCu of white translucent in 60 ° of C vacuum-dryings
0.2mn
0.8f cubic crystal.The pattern of product is all identical with embodiment 1 with structure.
Embodiment 5
As embodiment 1, cupric chloride and Manganous chloride tetrahydrate are taken 2.5 mmol according to the mol ratio of 1:4, be dissolved in 15 mL distilled water with 15 mL DMFs (DMF), stir and make it fully dissolve; Wherein the volume ratio of DMF and distilled water is 1:1.This mixing solutions is loaded in reactor, is heated to 145 ° of C after sealing and reacts, and be incubated 60 hours, then naturally cool to room temperature.Reacted saturated clear liquid transfer pipet taken out and loads in the cleaned beaker of step (1), then beaker being put into climatic chamber; Set 30 sections of temperature lowering curves, temperature range is 28 ~ 22 ° of C, and every section of temperature difference 0.5 ° of C, every section of temperature range is incubated 3 hours, and humidity is 55%.By the crystal grain of beaker bottom absolute ethanol washing 3 times, within 10 minutes, obtain the DMCu of white translucent in 60 ° of C vacuum-dryings
0.2mn
0.8f cubic crystal.The pattern of product is all identical with embodiment 1 with structure.
Claims (5)
1. a Copper-cladding Aluminum Bar metal-organic framework DMMnF monocrystal material, is characterized in that, is by being of a size of 2.5 × 2.5 × 1.5 ~ 3.5 × 3.5 × 2.0 mm
3, and in compound, the molar percentage of cupric ion and mn ion is the DMCu of 1:4
0.2mn
0.8f monocrystalline forms.
2. Copper-cladding Aluminum Bar metal-organic framework DMMnF monocrystal material according to claim 1, is characterized in that described DMCu
0.2mn
0.8f monocrystalline is white translucent crystal, and its chemical formula is [(CH
3)
2nH
2] Cu
0.2mn
0.8(HCOO)
3.
3. a preparation method for Copper-cladding Aluminum Bar metal-organic framework DMMnF monocrystal material as claimed in claim 1, is characterized in that, comprise the steps:
(1) in beaker, add the vitriol oil, acetone, dehydrated alcohol and deionized water successively, respectively ultrasonic cleaning 15 minutes, to remove residual metal ions and organism in beaker, the beaker after cleaning is saved backup;
(2) cupric chloride and Manganous chloride tetrahydrate are taken mixing according to the mol ratio of 1:4, be dissolved in distilled water with DMF, stir and make it fully dissolve; Wherein the volume ratio of DMF and distilled water is 1:1; Needed for every mole of cupric chloride and Manganous chloride tetrahydrate mixture, distilled water consumption is 6mL;
(3) step (2) gained mixing solutions is loaded in reactor, be heated to 135 ~ 145 ° of C after sealing and react, and be incubated 60 ~ 72 hours, then naturally cool to room temperature;
(4) reacted for step (3) saturated clear liquid transfer pipet taken out and load in the cleaned beaker of step (1), then beaker being put into climatic chamber; Set 30 sections of temperature lowering curves, temperature range is 28 ~ 22 ° of C, every section of temperature difference 0.5 ° of C, and every section of temperature range is incubated 2.5 ~ 3 hours, and humidity is 45 ~ 55%;
(5) by the crystal grain of beaker bottom absolute ethanol washing 3 times, Copper-cladding Aluminum Bar metal-organic framework DMMnF monocrystal material within 10 minutes, is obtained in 60 ° of C vacuum-dryings.
4. the preparation method of Copper-cladding Aluminum Bar metal-organic framework DMMnF monocrystal material according to claim 3, is characterized in that the model of described climatic chamber is WHS-70B model.
5. the preparation method of Copper-cladding Aluminum Bar metal-organic framework DMMnF monocrystal material according to claim 3, is characterized in that the humidity in described step (4) is controlled by humidifier and climatic chamber.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106637414A (en) * | 2016-12-15 | 2017-05-10 | 浙江理工大学 | Metal-organic framework DMMnF/strontium formate heterojunction single crystal optical material and preparation method thereof |
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| CN106637414A (en) * | 2016-12-15 | 2017-05-10 | 浙江理工大学 | Metal-organic framework DMMnF/strontium formate heterojunction single crystal optical material and preparation method thereof |
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Application publication date: 20150708 |