CN106637414A - Metal-organic framework DMMnF/strontium formate heterojunction single crystal optical material and preparation method thereof - Google Patents
Metal-organic framework DMMnF/strontium formate heterojunction single crystal optical material and preparation method thereof Download PDFInfo
- Publication number
- CN106637414A CN106637414A CN201611160645.7A CN201611160645A CN106637414A CN 106637414 A CN106637414 A CN 106637414A CN 201611160645 A CN201611160645 A CN 201611160645A CN 106637414 A CN106637414 A CN 106637414A
- Authority
- CN
- China
- Prior art keywords
- dmmnf
- strontium
- metal
- single crystal
- beaker
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C30B7/08—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by cooling of the solution
-
- 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
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/35—Non-linear optics
- G02F1/355—Non-linear optics characterised by the materials used
- G02F1/3551—Crystals
Abstract
The invention discloses a metal-organic framework DMMnF/strontium formate heterojunction single crystal optical material and a preparation method of the metal-organic framework DMMnF/strontium formate heterojunction single crystal optical material. The metal-organic framework DMMnF/strontium formate heterojunction single crystal optical material comprises a DMMnF single crystal substrate and a strontium formate epitaxial single crystal, wherein the size of the DMNnF single crystal substrate is 2.3*2.3*2.3-2.6*2.6*2.6* mm<3>, the size of the strontium formate epitaxial single crystal is 2.6*2.6*2.6*-3.0*3.0*3.0 mm<3>, and the thickness of the strontium formate epitaxial single crystal is 0.2-0.25 mm. In the preparation process, the used agent is a commercial product and does not need to be prepared complicatedly; a hydrothermal method and a liquid phase method are combined to acquire the large-size single crystal; and the process is high in controllability and is easy to operate, and the purity of the prepared product is high. The prepared heterojunction single crystal material is expected to be widely applied to novel metal-organic framework semiconductors, information storage and optical devices.
Description
Technical field
The present invention relates to a kind of heterojunction material of metal-organic framework single crystal epitaxial growth and preparation method thereof, specifically
Refer to a kind of monocrystalline [(CH3)2NH2]Mn(HCOO)3/Sr(CHOO)2·2H2O heterojunction materials (are abbreviated as DMMnF/Sr
(CHOO)2·2H2O, DM are [(CH3)2NH2]+1, F is for [(HCOO)3]-3) and preparation method thereof.
Technical background
Metal-organic framework (Metal-Organic Frameworks, MOFs) material is because in catalysis, hydrogen storage and optics unit
The aspects such as part have potential using value and receive significant attention, and are a focuses in current New function investigation of materials field.
Flexible, flexible skeleton, easy cutting and easy formation high anisotropy and low lattice are prepared because organic compound has
The advantage of the aspects such as symmetrical structure, people are attempted ferroelectricity organic matter and magnetic transition metal ions binding in recent years, if
Count out based on the new multi-ferroic material of metal-organic hybrid.
In recent years, device for non-linear optical becomes a focus in novel optical investigation of materials field.Nonlinear optics
Material refers to that its optical property depends on the material of incident intensity, nonlinear optical property to be also referred to as the light under high light effect
Property is learned, these properties is primarily due to and is just showed under strong relevant light action only as laser.Using nonlinear optical
Learning the non-linear process such as the frequency multiplication and frequency, difference frequency, optically erasing and Multiphoton Absorbtion of crystal can obtain frequency and incident light
The different laser of frequency, so as to reach the purpose of light frequency conversion.This crystalloid is widely used in laser frequency conversion, four ripples to be mixed
Frequently, light beam steering, image amplification, optical information processing, optical storage, optical-fibre communications, underwater communication, laser countermeasure (s) and nuclear fusion etc. grind
Study carefully field.
Formic acid strontium crystal is a kind of water white transparency, the good potential nonlinear optical material of optical property.Strontium formate and
The preparation method of DMMnF mainly has hydro-thermal method, liquid phase method and double decomposition etc..Hydro-thermal method refer to sealing pressure vessel in,
Using water as solvent, in 100～400 DEG C of temperature, pressure is more than 0.1MPa until under conditions of tens to hundreds of MPa, making forerunner
Thing (raw material) reacts and crystallizes.A special physicochemical environment that cannot be obtained in atmospheric conditions is provided, before making
Drive thing sufficiently to be dissolved in reaction system, form atom or molecular growth primitive, nucleation is simultaneously crystallized.Hydro-thermal method has anti-
Answer speed fast, product purity height, better crystallinity degree, reunite the advantages of lacking.At present, the Sr (CHOO) for being synthesized by hydro-thermal method2·2H2O
With DMMnF materials more based on powder crystallite and small monocrystalline, but, it is extremely restricted as device application, therefore how
Better control over Sr (CHOO)2·2H2The growth of O and DMMnF monocrystalline so that the size of monocrystalline reaches and is easy to wanting for making devices
Ask, and widen its industry application and have very important significance.
As people go deep into metal-organic framework materials research, people are just making great efforts to epitaxial growth metal-organic bone
Frame monocrystalline is sufficiently studied, it is desirable to the size of monocrystalline can be improved by epitaxial growth metal-organic framework monocrystalline, and
Some new heterojunction materials are obtained, so as to expand the using value of metal-organic framework significantly.At present, a kind of metal-have
Machine frame DMMnF/ strontium formate hetero-junctions monocrystalline optical materials and preparation method thereof are not yet reported that.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art, there is provided a kind of metal-organic framework DMMnF/ strontium formates
Hetero-junctions monocrystalline optical material and preparation method thereof.While the preparation method of the DMMnF/ strontium formate hetero-junctions monocrystalline optical materials
Simply, conveniently.
The technical scheme is that：
It by size is 2.3 × 2.3 × 2.3 that a kind of heterogeneous monocrystalline optical material of metal-organic framework DMMnF/ strontium formates is
～2.6 × 2.6 × 2.6mm3DMMnF single crystalline substrates and size be 2.6 × 2.6 × 2.6～3.0 × 3.0 × 3.0mm3, thickness
Strontium formate epitaxy single-crystal for 0.2～0.25mm is constituted.
Described DMMnF monocrystalline is water white transparency cube monocrystalline, and chemical formula is [(CH3)2NH2]Mn(HCOO)3, it is described
Strontium formate epitaxy single-crystal be water white transparency cube monocrystalline, chemical formula be Sr (CHOO)2·2H2O。
The preparation method of the heterogeneous monocrystalline optical material of the metal-organic framework metal-organic framework DMMnF/ strontium formates
Comprise the steps：
(1) concentrated sulfuric acid, acetone, absolute ethyl alcohol and deionized water are sequentially added in beaker, are cleaned by ultrasonic 15 minutes respectively,
Residual metal ions and organic matter in remove beaker, the beaker after cleaning is saved backup；
(2) manganese chloride, DMF are dissolved in distilled water, stirring makes it fully dissolve；Wherein per mole
Manganese chloride correspondence distillation water consumption is 7.5L, and DMF is 1 with the volume ratio of distilled water：1；
(3) step (2) gained mixed solution is loaded in reactor, 135～145 DEG C are heated to after sealing is carried out instead
Should, and 60～72 hours are incubated, then naturally cool to room temperature；
(4) the reacted manganese saturation clear liquid of step (3) is taken out and is loaded the beaker that step (1) was cleaned with pipette
In, then beaker is put into climatic chamber；30 sections of temperature lowering curves of setting, temperature range is 29～21 DEG C, every section of temperature difference 0.3
DEG C, every section of temperature range is incubated 2.5～3 hours, and humidity is 50～55%；
(5) after question response is complete, water white DMMnF cubic crystals can be obtained in beaker bottom, it is standby；
(6) manganese chloride in step (2), implementation steps (2) and step (3) is replaced to obtain reacted strontium and satisfy with strontium chloride
And clear liquid, the water white DMMnF cubic crystals obtained by step (5) are put into strontium saturation clear liquid, according to the side of step (4)
Method sets 30 sections of temperature lowering curves, and temperature range is 35～26 DEG C, every section of 0.3 DEG C of temperature difference, and every section of temperature range insulation 2.5～3 is little
When, humidity is 40～45%；
(7) water white metal-organic framework DMMnF/ strontium formates hetero-junctions monocrystalline is obtained according to step (6) condition
Optical material.
Beneficial effect：
In preparation process of the present invention, agents useful for same is commercial product, without the need for loaded down with trivial details preparation；Using hydro-thermal method and liquid phase method phase
With reference to the bigger monocrystalline of acquisition size and novel metal-organic frame heterojunction material；Process controllability is strong, easy to operate, system
The product purity for obtaining is high.
DMMnF/ strontium formate heterojunction materials obtained by the present invention, are expected in novel metal-organic frame semiconductor, information
Storage and optics aspect are widely used.
Description of the drawings
Fig. 1 is DMMnF/ strontium formates hetero-junctions schematic diagram of the present invention；
Fig. 2 is with the obtained DMMnF monocrystalline digital photographs of the present invention；
Fig. 3 is with the obtained DMMnF/ strontium formate hetero-junctions monocrystalline digital photographs of the present invention；
Fig. 4 is the X-ray diffraction spectrogram (XRD) with the obtained DMMnF of the present invention and strontium formate monocrystalline；
Fig. 5 is the infrared spectrogram (IR) with the obtained DMMnF substrate monocrystals of the present invention；
Fig. 6 is the infrared spectrogram (IR) with the obtained strontium formate epitaxy single-crystal of the present invention.
Specific embodiment
The present invention is further illustrated below in conjunction with example.
The present invention prepares DMMnF/ strontium formate hetero-junctions monocrystal materials to be combined method using hydro-thermal method and liquid phase method.
The concentrated sulfuric acid, acetone, absolute ethyl alcohol and deionized water are sequentially added in beaker, respectively be cleaned by ultrasonic 15 minutes, to remove beaker in
The impurity such as residual metal ions, organic matter, the beaker after cleaning is saved backup.By 2.5mmol manganese chlorides, 15mL N, N- bis-
NMF (DMF) is dissolved in 15mL distilled water, and stirring makes it fully dissolve；Wherein DMF is 1 with the volume ratio of distilled water：
1.Manganese chloride solution is loaded in reactor, 135～145 DEG C is heated to after sealing and is reacted, and it is little to be incubated 60～72
When, then naturally cool to room temperature.Reacted manganese saturation clear liquid pipette is taken out and is fitted into the beaker that cleaned, so
Beaker is put into climatic chamber afterwards, sets 30 sections of temperature lowering curves, temperature range is 29～21 DEG C, every section of 0.3 DEG C of temperature difference, often
Section temperature range is incubated 2.5～3 hours, and humidity is 50～55%.After question response is complete, obtain water white in beaker bottom
DMMnF cubic crystals.2.5mmol strontium chlorides are replaced into manganese chloride, reacted strontium saturation clear liquid are as above obtained described in step,
The water white transparency DMMnF cubic crystals obtained in above-mentioned steps are put into the saturation clear liquid, 30 are set in climatic chamber
Section temperature lowering curve, temperature range is 35～26 DEG C, every section of 0.3 DEG C of temperature difference, and every section of temperature range is incubated 2.5～3 hours, and humidity is
40～45%, finally obtain the heterogeneous crystalline solid of epitaxially grown water white transparency DMMnF/ strontium formates, its structural representation such as Fig. 1 institutes
Show.
Embodiment 1
2.5mmol manganese chlorides, 15mL DMFs (DMF) are dissolved in 15mL distilled water, stirring fills it
Divide dissolving；Wherein DMF is 1 with the volume ratio of distilled water：1.Manganese chloride solution is loaded in reactor, is heated to after sealing
140 DEG C are reacted, and are incubated 60 hours, then naturally cool to room temperature.Reacted manganese saturation clear liquid is taken with pipette
In going out and being fitted into the beaker for cleaning, then beaker is put into climatic chamber, sets 30 sections of temperature lowering curves, temperature range is
29～21 DEG C, every section of 0.3 DEG C of temperature difference, every section of temperature range is incubated 2.5 hours, and humidity is 50%.After question response is complete, in beaker
Bottom obtains water white DMMnF cubic crystals.2.5mmol strontium chlorides are replaced into manganese chloride, is as above obtained described in step
Reacted strontium saturation clear liquid, by the water white transparency DMMnF cubic crystals obtained in above-mentioned steps the saturation clear liquid is put into,
30 sections of temperature lowering curves are set in climatic chamber, temperature range is 35～26 DEG C, and every section of 0.3 DEG C of temperature difference, every section of temperature range is protected
Temperature 3 hours, humidity is 40%, finally obtains the heterogeneous crystalline solid of epitaxially grown water white transparency DMMnF/ strontium formates.
Gained DMMnF crystal is directly observed (such as Fig. 2) under digital camera, it can be found that crystal is in water white transparency, chi
Very little is 2.3 × 2.3 × 2.3～2.6 × 2.6 × 2.6mm3Cubic crystal.The XRD analysis of Fig. 4 show that product is three prismatic crystals
The DMMnF of system (corresponds to CCDC：246991, Cambridge crystal data center), and along 012 direction oriented growth, form single
It is brilliant.Find out from Fig. 3 digital photographs, in the successful epitaxial growth of DMMnF planes of crystal water white transparency Sr (CHOO)2·2H2O is mono-
Crystalline substance, its size is 3.0 × 3.0 × 3.0mm3Cubic crystal, thickness is 0.25mm, and the XRD results of Fig. 4 show epitaxial growth
Crystal be Sr (CHOO)2·2H2O (corresponds to PDF cards：14-0824), and along (012) direction oriented growth, formed
Extension hetero-junctions monocrystalline.Fig. 5 is the IR collection of illustrative plates of DMMnF, in 750-850cm in figure-1、1250-1500cm-1、1500-1750cm-1
And 2250-3250cm-1The absworption peak at place represents respectively the vibration absorption peak of manganese, methyl, secondary ammonium salt and carboxyl, further card
Bright gained crystal is [(CH3)2NH2]Mn(HCOO)3.In the same manner, find out that wave number is 1596cm from the IR collection of illustrative plates (Fig. 6) of strontium formate-1、1363cm-1、873cm-1Pair and 3128cm-1Absworption peak corresponded to C=O bond, C-O singly-bounds, Sr-O keys and O- respectively
The vibration of H keys, shows that, containing strontium, carboxyl and the crystallization water in gained formic acid strontium crystal, its chemical formula is Sr (CHOO)2·2H2O。
Embodiment 2
Such as embodiment 1,2.5mmol manganese chlorides, 15mL DMFs (DMF) are dissolved in into 15mL distilled water
In, stirring makes it fully dissolve；Wherein DMF is 1 with the volume ratio of distilled water：1.Manganese chloride solution is loaded in reactor, it is close
It is honored as a queen and is heated to 140 DEG C and is reacted, and be incubated 60 hours, then naturally cools to room temperature.By reacted manganese saturation
Clear liquid pipette takes out and is fitted into the beaker that cleaned, and then beaker is put into climatic chamber, sets 30 sections of coolings
Curve, temperature range is 29～21 DEG C, every section of 0.3 DEG C of temperature difference, and every section of temperature range is incubated 2.5 hours, and humidity is 55%.Treat anti-
After answering completely, in beaker bottom water white DMMnF cubic crystals are obtained.2.5mmol strontium chlorides are replaced into manganese chloride, such as
Reacted strontium saturation clear liquid is obtained described in upper step, the water white transparency DMMnF cubic crystals obtained in above-mentioned steps are put
Enter the saturation clear liquid, 30 sections of temperature lowering curves set in climatic chamber, temperature range is 35～26 DEG C, every section of 0.3 DEG C of temperature difference,
Every section of temperature range is incubated 3 hours, and humidity is 40%, finally obtains epitaxially grown water white transparency strontium formate cubic crystal.
The pattern and structure of product is same as Example 1.
Embodiment 3
Such as embodiment 1,2.5mmol manganese chlorides, 15mL DMFs (DMF) are dissolved in into 15mL distilled water
In, stirring makes it fully dissolve；Wherein DMF is 1 with the volume ratio of distilled water：1.Manganese chloride solution is loaded in reactor, it is close
It is honored as a queen and is heated to 145 DEG C and is reacted, and be incubated 60 hours, then naturally cools to room temperature.By reacted manganese saturation
Clear liquid pipette takes out and is fitted into the beaker that cleaned, and then beaker is put into climatic chamber, sets 30 sections of coolings
Curve, temperature range is 29～21 DEG C, every section of 0.3 DEG C of temperature difference, and every section of temperature range is incubated 2.5 hours, and humidity is 50%.Treat anti-
After answering completely, in beaker bottom water white DMMnF cubic crystals are obtained.2.5mmol strontium chlorides are replaced into manganese chloride, such as
Reacted strontium saturation clear liquid is obtained described in upper step, the water white transparency DMMnF cubic crystals obtained in above-mentioned steps are put
Enter the saturation clear liquid, 30 sections of temperature lowering curves set in climatic chamber, temperature range is 35～26 DEG C, every section of 0.3 DEG C of temperature difference,
Every section of temperature range is incubated 3 hours, and humidity is 40%, finally obtains epitaxially grown water white transparency strontium formate cubic crystal.
The pattern and structure of product is same as Example 1.Embodiment 4
Such as embodiment 1,2.5mmol manganese chlorides, 15mL DMFs (DMF) are dissolved in into 15mL distilled water
In, stirring makes it fully dissolve；Wherein DMF is 1 with the volume ratio of distilled water：1.Manganese chloride solution is loaded in reactor, it is close
It is honored as a queen and is heated to 140 DEG C and is reacted, and be incubated 60 hours, then naturally cools to room temperature.By reacted manganese saturation
Clear liquid pipette takes out and is fitted into the beaker that cleaned, and then beaker is put into climatic chamber, sets 30 sections of coolings
Curve, temperature range is 29～21 DEG C, every section of 0.3 DEG C of temperature difference, and every section of temperature range is incubated 32.5 hours, and humidity is 55%.Treat
After reaction completely, in beaker bottom water white DMMnF cubic crystals are obtained.2.5mmol strontium chlorides are replaced into manganese chloride,
As above reacted strontium saturation clear liquid is obtained described in step, by the water white transparency DMMnF cubic crystals obtained in above-mentioned steps
The saturation clear liquid is put into, 30 sections of temperature lowering curves are set in climatic chamber, temperature range is 35～26 DEG C, every section of temperature difference 0.3
DEG C, every section of temperature range is incubated 2.5 hours, and humidity is 45%, finally obtains epitaxially grown water white transparency strontium formate cube
Crystal.The pattern and structure of product is same as Example 1.Embodiment 5
Such as embodiment 1,2.5mmol manganese chlorides, 15mL DMFs (DMF) are dissolved in into 15mL distilled water
In, stirring makes it fully dissolve；Wherein DMF is 1 with the volume ratio of distilled water：1.Manganese chloride solution is loaded in reactor, it is close
It is honored as a queen and is heated to 135 DEG C and is reacted, and be incubated 60 hours, then naturally cools to room temperature.By reacted manganese saturation
Clear liquid pipette takes out and is fitted into the beaker that cleaned, and then beaker is put into climatic chamber, sets 30 sections of coolings
Curve, temperature range is 29～21 DEG C, every section of 0.3 DEG C of temperature difference, and every section of temperature range is incubated 3 hours, and humidity is 50%.Question response
After completely, in beaker bottom water white DMMnF cubic crystals are obtained.2.5mmol strontium chlorides are replaced into manganese chloride, as above
Reacted strontium saturation clear liquid is obtained described in step, the water white transparency DMMnF cubic crystals obtained in above-mentioned steps are put into
The saturation clear liquid, sets 30 sections of temperature lowering curves in climatic chamber, and temperature range is 35～26 DEG C, every section of 0.3 DEG C of temperature difference, often
Section temperature range is incubated 3 hours, and humidity is 40%, finally obtains epitaxially grown water white transparency strontium formate cubic crystal.Produce
The pattern and structure of thing is same as Example 1.
Claims (3)
1. a kind of metal-organic framework DMMnF/ strontium formates hetero-junctions monocrystalline optical material, it is characterised in that be to be by size
2.3 × 2.3 × 2.3～2.6 × 2.6 × 2.6mm3DMMnF single crystalline substrates and size be 2.6 × 2.6 × 2.6～3.0 × 3.0
×3.0mm3, thickness is the strontium formate epitaxy single-crystal composition of 0.2～0.25mm.
2. metal-organic framework DMMnF/ strontium formates hetero-junctions monocrystalline optical material according to claim 1, its feature exists
It is water white transparency cube monocrystalline in described DMMnF monocrystalline, chemical formula is [(CH3)2NH2]Mn(HCOO)3, described formic acid
Strontium epitaxy single-crystal is water white transparency cube monocrystalline, and chemical formula is Sr (CHOO)2·2H2O。
3. a kind of preparation side of metal-organic framework DMMnF/ strontium formates hetero-junctions monocrystalline optical material as claimed in claim 1
Method, it is characterised in that comprise the steps：
(1) concentrated sulfuric acid, acetone, absolute ethyl alcohol and deionized water are sequentially added in beaker, is cleaned by ultrasonic 15 minutes respectively, to go
Except residual metal ions and organic matter in beaker, the beaker after cleaning is saved backup；
(2) manganese chloride, DMF are dissolved in distilled water, stirring makes it fully dissolve；Wherein every mole chlorination
Manganese correspondence distillation water consumption is 7.5L, and DMF is 1 with the volume ratio of distilled water：1；
(3) step (2) gained mixed solution is loaded in reactor, 135～145 DEG C is heated to after sealing and is reacted,
And 60～72 hours are incubated, then naturally cool to room temperature；
(4) the reacted manganese saturation clear liquid pipette of step (3) is taken out and is fitted into the beaker that step (1) was cleaned, so
Beaker is put into climatic chamber afterwards；30 sections of temperature lowering curves of setting, temperature range is 29～21 DEG C, every section of 0.3 DEG C of temperature difference, often
Section temperature range is incubated 2.5～3 hours, and humidity is 50～55%；
(5) after question response is complete, water white DMMnF cubic crystals are obtained in beaker bottom, it is standby；
(6) manganese chloride in step (2) is replaced with strontium chloride, it is clear that implementation steps (2) and step (3) obtain reacted strontium saturation
Liquid, by the water white DMMnF cubic crystals obtained by step (5) strontium saturation clear liquid is put into, and is set according to the method for step (4)
Fixed 30 sections of temperature lowering curves, temperature range is 35～26 DEG C, every section of 0.3 DEG C of temperature difference, and every section of temperature range is incubated 2.5～3 hours, wet
Spend for 40～45%；
(7) water white metal-organic framework DMMnF/ strontium formates hetero-junctions monocrystalline optics is obtained according to step (6) condition
Material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611160645.7A CN106637414A (en) | 2016-12-15 | 2016-12-15 | Metal-organic framework DMMnF/strontium formate heterojunction single crystal optical material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611160645.7A CN106637414A (en) | 2016-12-15 | 2016-12-15 | Metal-organic framework DMMnF/strontium formate heterojunction single crystal optical material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106637414A true CN106637414A (en) | 2017-05-10 |
Family
ID=58823747
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611160645.7A Pending CN106637414A (en) | 2016-12-15 | 2016-12-15 | Metal-organic framework DMMnF/strontium formate heterojunction single crystal optical material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106637414A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104726937A (en) * | 2015-03-09 | 2015-06-24 | 张香丽 | Calcium formate single crystal optical material and preparation method thereof |
| CN104762661A (en) * | 2015-03-09 | 2015-07-08 | 浙江理工大学 | A copper-doped metal-organic framework DMMnF single crystal material and a preparing method thereof |
| CN104788476A (en) * | 2015-03-09 | 2015-07-22 | 浙江理工大学 | Metal-organic framework DMCaF monocrystalline material and preparation method thereof |
| CN104788505A (en) * | 2015-03-09 | 2015-07-22 | 浙江理工大学 | Metal-organic framework single crystal epitaxially grown DMCoF/DMMnF heterojunction material and preparation method thereof |
| CN104788504A (en) * | 2015-03-09 | 2015-07-22 | 陈谦 | Component controllable cobalt doped metal-organic framework DMMnF monocrystalline material and preparation method thereof |
| CN104788506A (en) * | 2015-03-09 | 2015-07-22 | 浙江理工大学 | Metal-organic framework single crystal epitaxially grown DMMnF/DMCoF heterojunction material and preparation method thereof |
-
2016
- 2016-12-15 CN CN201611160645.7A patent/CN106637414A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104726937A (en) * | 2015-03-09 | 2015-06-24 | 张香丽 | Calcium formate single crystal optical material and preparation method thereof |
| CN104762661A (en) * | 2015-03-09 | 2015-07-08 | 浙江理工大学 | A copper-doped metal-organic framework DMMnF single crystal material and a preparing method thereof |
| CN104788476A (en) * | 2015-03-09 | 2015-07-22 | 浙江理工大学 | Metal-organic framework DMCaF monocrystalline material and preparation method thereof |
| CN104788505A (en) * | 2015-03-09 | 2015-07-22 | 浙江理工大学 | Metal-organic framework single crystal epitaxially grown DMCoF/DMMnF heterojunction material and preparation method thereof |
| CN104788504A (en) * | 2015-03-09 | 2015-07-22 | 陈谦 | Component controllable cobalt doped metal-organic framework DMMnF monocrystalline material and preparation method thereof |
| CN104788506A (en) * | 2015-03-09 | 2015-07-22 | 浙江理工大学 | Metal-organic framework single crystal epitaxially grown DMMnF/DMCoF heterojunction material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| S. MUTHUPOONGODI等: "Growth and characterization of strontium formate dehydrate (Sr(HCOO)2•2H2O) single crystals doped strongly with glycine", 《OPTIK》 * |
| 朱建国等: "《电子与光电子材料》", 31 August 2007, 国防工业出版社 * |
| 林景臻等: "非线性光学晶体二水甲酸锶的生长", 《人工晶体学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105384188A (en) | Cesium lead bromide powder preparation method | |
| Liu et al. | Bulk crystal growth and characterization of semi-organic nonlinear optical crystal tri-diethylammonium hexachlorobismuthate (TDCB) | |
| CN104788505B (en) | A kind of DMCoF/DMMnF heterojunction materials of metal organic frame single crystal epitaxial growth and preparation method thereof | |
| CN112960660A (en) | Black phosphorus nanobelt material and preparation method thereof | |
| CN102417206B (en) | Preparation method of NaV2O5 crystal material with right angle morphology | |
| CN113186590B (en) | Preparation method of centimeter-level molybdenum trioxide single crystal | |
| CN106637414A (en) | Metal-organic framework DMMnF/strontium formate heterojunction single crystal optical material and preparation method thereof | |
| CN104674334B (en) | A kind of formiate LiMg (COOH)3Monocrystalline optical material and preparation method thereof | |
| CN101654408B (en) | Anhydrous zinc tartrate ferroelectric function material and preparation method thereof | |
| CN104726937B (en) | Calcium formate single crystal optical material and preparation method thereof | |
| CN101560218B (en) | Organometallic complex of nonlinear optical and ferroelectric material, synthesis and application thereof | |
| CN104674351B (en) | A kind of formiate LiCa (COOH)3Monocrystalline optical material and preparation method thereof | |
| CN111730063B (en) | Preparation method of lead nanowire | |
| CN109898137A (en) | A kind of preparation method of sodium tantalate monocrystal thin films | |
| CN104788506B (en) | A kind of DMMnF/DMCoF heterojunction materials of metal organic frame single crystal epitaxial growth and preparation method thereof | |
| CN104788504B (en) | A kind of controllable cobalt doped metal organic frame DMMnF monocrystal materials of composition and preparation method thereof | |
| CN104674350A (en) | Multiferroic formate LiCo(COOH)3 single-crystal materials and preparation method thereof | |
| CN104788476B (en) | A kind of metal organic frame DMCaF monocrystal materials and preparation method thereof | |
| CN109825874A (en) | A kind of preparation method of monocrystalline lead titanate thin film | |
| CN101619491B (en) | Frroelectric material boron potassium ermanate, preparation method and application thereof | |
| CN104788507A (en) | Magnesium doped metal-organic framework DMMg0.5Mn0.5F single crystal material and preparation method thereof | |
| CN104788475B (en) | A kind of metal organic frame DMMgF monocrystal materials and preparation method thereof | |
| CN104762662A (en) | A copper-doped metal-organic framework DMCoF single crystal material and a preparing method thereof | |
| KR20170036231A (en) | Purifying method of dodecanedioic acid | |
| CN104762661A (en) | A copper-doped metal-organic framework DMMnF single crystal material and a preparing method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170510 |
|
| WD01 | Invention patent application deemed withdrawn after publication |