CN101157475A - Even compact and transparent laminated double-metal hydroxide film and preparation method thereof - Google Patents
Even compact and transparent laminated double-metal hydroxide film and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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- C01G9/00—Compounds of zinc
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- C01P2002/22—Two-dimensional structures layered hydroxide-type, e.g. of the hydrotalcite-type
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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- C—CHEMISTRY; METALLURGY
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a uniform, compact and transparent layered double metal hydroxide film and the preparing method thereof, and belongs to the technical field of layered double metal hydroxides. The general chemical formula of the film layer LDHs is [M<2+>1-xM<3+>x (OH) 2]<X+> (A<n->) x/n*mH2O, wherein, M<2+> represents any one of Mg<2+>, Ni<2+> and Zn <2+>; M<3+> represents either one of Al<3+> and Fe<3+>; A<n-> is any one of NO3<->, Cl<-> and SO4<2->; x is larger than or equal to 0.2 and less than or equal to 0.4; m is larger than or equal to 0 and less than or equal to 2. The preparing method needs not a base piece for support, and refers to gas-liquid interface method to prepare the uniform, compact and transparent LDHs film on an air-water interface under the joint effect of surface tension of the solution and pH gradients. The invention has the advantage that the film is formed on a gas-liquid interface without the need of a base piece for support, thereby overcoming influence of the base piece on preparation of the LDHs film; the reaction occurs at normal temperature and has lower energy consumption; the equipment is simple and easy to operate.
Description
Affiliated field
The invention belongs to the layered double hydroxide field, transparent laminated double-metal hydroxide film of a kind of even compact and preparation method thereof is provided especially, prepare the transparent laminated double-metal hydroxide film of even compact at the air-water interface place.
Background technology
Layered double hydroxide also claims houghite (LDHs), is a kind of important inorganic functional material.LDHs has laminate structure, and its body layer plate element composition, interlayer object anion species and quantity etc. all have Modulatory character.These characteristics make LDHs have the physics-chem characteristic of multiple excellence, show very wide application prospect in many fields such as ion-exchange, absorption, catalysis, macromolecule modified, optical material, magnetics material, electricity materials.At present, research and the application to LDHs both at home and abroad generally all is confined to the LDHs powder body material, yet the LDHs powder body material exists shortcomings such as easy loss, recovery difficulty.Mould material more helps device with respect to powder body material, and this will widen it greatly in industrial application, and for the film of orientation, the functional of each side such as its electricity, light, magnetic all can improve a lot.
Different with other stratified material is that LDHs is difficult for being prepared into film, thereby has hindered some application and developments and the device of LDHs material.The preparation method about the LDHs film of bibliographical information is limited at present, mainly contains one-step synthesis and two step synthesis method two big classes.The example of one-step synthesis such as document Chem.Lett., in 2005,34,1610, Lei etc. at first carry out sulfonation with the polystyrene substrate with the vitriol oil to be handled, and utilizes Wyler's process to obtain the Mg-Al hydrotalcite film of vertical orientated densification in its surface preparation afterwards; Document Adv.Mater., in 2006,18,3089, people such as Duan are substrate with anodised aluminium/aluminium, adopt the growth in situ method to prepare the Ni-Al hydrotalcite film with ultra-hydrophobicity.Two the step synthesis method such as document Adv.Mater., in 2001,13,1263, people such as 6andner at first prepare the colloid of LDHs, afterwards its casting are deposited on the magnalium LDHs film that has obtained the alkoxyl group intercalation on the glass substrate; Document Thin Solid Films, 2001,397, in 255, the method that people such as Akihiko utilize LB at first on the mica substrate load electronegative ruthenium metal complexes, utilize itself and the interparticle electrostatic interaction of positively charged LDHs to prepare the hybrid film of Ni-Al hydrotalcite and ruthenium containing metal title complex afterwards; Document Chem.commun., in 2007,2,123, people such as Wang at first prepare equal dispersive LDHs nanoparticle, adopt " solvent evaporated method " with its assembling preparation LDHs film in order then.
Summary of the invention
The objective of the invention is to: transparent laminated double-metal hydroxide film of a kind of even compact and preparation method thereof is provided, need not the preparation method-liquid-gas interface method of substrate support, double-metal hydroxide film that even compact is transparent, under the surface tension of solution and the acting in conjunction of pH gradient, prepare the transparent LDHs film of even compact, to realize the device of multifunctional material LDHs at the air-water interface place.
The laminated double-metal hydroxide film that even compact provided by the invention is transparent, film are the forming at the interface of air-water, need not the support of substrate in the film process, have overcome the influence of substrate to the LDHs film preparation.The chemical general formula of rete is
[M
2+ 1-xM
3+ x(OH)
2]
x+(A
n-)
x/n·mH
2O，
M wherein
2+Represent Mg
2+, Ni
2+, Zn
2+In any, M
3+Represent Al
3+, Fe
3+In any, A
N-Be NO
3 -, Cl
-, SO
4 2-In any, 0.2≤x≤0.33,0≤m≤2.
This LDHs film is even, fine and close, smooth, and the thickness of film increases along with the prolongation in reaction times at micron order.
The concrete synthesis step of laminated double-metal hydroxide film of the present invention is as follows:
A, preparation solubility divalence inorganic salt M
2+Y and solubility trivalent inorganic salt M
3+The mixed solution of Y, total concentration of metal ions is 0.1-0.3mol/L in the solution, divalence trivalent metal cation molar concentration rate (M
2+/ M
3+) be 2-4: 1;
B, preparation mass percent concentration are the dilute ammonia solution of 0.5-2%;
C, measure isopyknic salts solution and alkaline solution in culture dish, be placed in the moisture eliminator of sealing, 20-30 ℃ of reaction 4-24h down.Reaction is transferred to CO with the film at air-water interface place after finishing
2The unreacted mixing salt that adheres to flush away in the water is transferred to it after washing 1-5 time and is carried out drying on the clean substrate under 10～40 ℃.Described substrate is slide glass, silicon chip or silicon-dioxide etc.
Divalent metal M in the steps A
2+Be Ni
2+, Zn
2+In a kind of, trivalent metal cation M
3+Be Al
3+, Fe
3+In a kind of.Negatively charged ion Y can be Cl
-, NO
3 -, SO
4 2-Deng the inorganic acid radical negatively charged ion, that preferable is NO
3 -
With above-mentioned materials carry out XRD, IR, TG-DTA, ultimate analysis, FESEM characterizes proof and utilizes this method successfully to prepare the transparent LDHs film of even compact.The IR of the powder after film grinds proof interlayer anion is a nitrate radical, has also occurred LDHs material distinctive 001 serial diffraction peak in the XRD spectra, and this shows that obtain is typical nitrate radical type LDHs.The SEM photo of film shows that the smooth densification of LDHs film surface is smooth, and particle diameter is nanometer scale and high-sequential, uniform distribution.
The invention has the advantages that: room temperature reaction, energy consumption is low; The liquid-gas interface film forming need not the support of substrate in the film process, overcome the influence of substrate to the LDHs film preparation, can transfer to silicon chip, glass etc. after the film forming arbitrarily on the substrate; The film smooth surface is smooth, all is the nanostructure of high-sequential on the both macro and micro; Can regulate and control the kind and the composition of LDHs laminate metallic element and interlayer anion as required, obtain multi-functional LDHs film; Single step reaction, equipment is simple, processing ease.
Description of drawings
Fig. 1 is the synoptic diagram of liquid-gas interface reaction.
The Ni that Fig. 2 is obtained for embodiment 1
2AlNO
3The LDHs film grinds the XRD spectra of back powder, and X-coordinate is 2 θ, unit: degree; Ordinate zou is an intensity.
The Ni that Fig. 3 is obtained for embodiment 1
2AlNO
3The LDHs film grinds the FT-IR spectrogram of back powder, and X-coordinate is a wave number, unit: cm
-1Ordinate zou is a transmitance.
The Ni that Fig. 4 is obtained for embodiment 1
2AlNO
3The LDHs film amplifies 10,000 field emission electron scanning electronic microscope (FESEM) photo.
The Ni that Fig. 5 is obtained for embodiment 1
2AlNO
3The LDHs film amplifies 100,000 field emission electron scanning electronic microscope (FESEM) photo.
Embodiment
Embodiment 1
Steps A: with the solid Ni (NO of 1.1604g (0.004mol)
3)
2.6H
2Solid Al (the NO of O and 0.7503g (0.002mol)
3)
3.9H
2O is dissolved in the CO that goes of 20ml
2In the water.
Step B: measure the 0.54ml mass percent concentration and be 28% strong aqua, being diluted to 20ml is 0.68% weak ammonia to obtain mass percent concentration.
Step C: mixing salt and alkali lye are placed different culture dish respectively, in the moisture eliminator of sealing, react, 25 ℃ of temperature of reaction, the reaction times is 24h, the film on part salts solution surface spends CO after taking out
2Water washing three times is transferred to afterwards on the silicon substrate of washes clean and is carried out drying under the low temperature, obtains membrane sample.Remain membrane sample and take out the back centrifuge washing, 60 ℃ of dry 24h and grindings down obtain Ni
2AlNO
3The LDHs powder.
In the IR spectrogram of film powder at 1384cm
-1Strong and the sharp-pointed charateristic avsorption band that occurs is the v of nitrate radical
3The antisymmetric stretching vibration peak, and the distinctive serial diffraction peak of LDHs has appearred in 2 θ near 10 °, 20 ° and 61 ° in XRD spectra, the particle diameter of product shows that the densification of film smooth surface is smooth, particle diameter result and the basically identical that is calculated by XRD for the 4.75nm.FESEM photo.
Embodiment 2
Steps A: with the solid Zn (NO of 4.3360g (0.016mol)
3)
2.6H
2Solid Al (the NO of O and 3.0012g (0.008mol)
3)
3.9H
2O is dissolved in the CO that goes of 80ml
2In the water.
Step B: measure the 2.16ml mass percent concentration and be 28% strong aqua, being diluted to 80ml is 0.68% weak ammonia to obtain mass percent concentration.
Step C: mixing salt and alkali lye are placed different culture dish respectively, in the moisture eliminator of sealing, react, 25 ℃ of temperature of reaction, the reaction times is 24h, the film on part salts solution surface spends CO after taking out
2Water washing three times is transferred to afterwards on the silicon substrate of washes clean and is carried out drying under the low temperature, obtains membrane sample.Remain membrane sample and take out the back centrifuge washing, 60 ℃ of dry 24h and grindings down obtain Zn
2AlNO
3The LDHs powder.
In the IR spectrogram of film powder at 1384cm
-1Strong and the sharp-pointed charateristic avsorption band that occurs is the v of nitrate radical
3The antisymmetric stretching vibration peak, and the distinctive serial diffraction peak of LDHs has appearred in 2 θ near 10 °, 20 ° and 61 ° in XRD spectra.FESEM photo demonstration film is made up of nano level particle, and the smooth surface densification is smooth.
Embodiment 3
Steps A: with the solid Ni (NO of 1.1604g (0.004mol)
3)
2.6H
2Solid Fe (the NO of O and 0.8080g (0.002mol)
3)
3.9H
2O is dissolved in the CO that goes of 80ml
2In the water.
Step B: measure the 1.25ml mass percent concentration and be 28% strong aqua, being diluted to 20ml is 1.57% weak ammonia to obtain mass percent concentration.
Step C: mixing salt and alkali lye are placed different culture dish respectively, in the moisture eliminator of sealing, react, 25 ℃ of temperature of reaction, the reaction times is 24h, the film on part salts solution surface spends CO after taking out
2Water washing three times is transferred to afterwards on the silicon substrate of washes clean and is carried out drying under the low temperature, obtains membrane sample.Remain membrane sample and take out the back centrifuge washing, 60 ℃ of dry 24h and grindings down obtain Ni
2FeNO
3The LDHs powder.
In the IR spectrogram of film powder at 1384cm
-1Strong and the sharp-pointed charateristic avsorption band that occurs is the v of nitrate radical
3The antisymmetric stretching vibration peak, and the distinctive serial diffraction peak of LDHs has appearred in 2 θ near 10 °, 20 ° and 61 ° in XRD spectra.FESEM photo demonstration film is made up of nano level particle, and the smooth surface densification is smooth.
Claims (3)
1. the laminated double-metal hydroxide film that even compact is transparent is characterized in that, the chemical general formula of rete LDHs is: [M
2+ 1-xM
3+ x(OH)
2]
X+(A
N-)
X/nMH
2O;
Wherein, M
2+Represent Mg
2+, Ni
2+, Zn
2+In any, M
3+Represent Al
3+, Fe
3+In any, A
N-Be NO
3 -, Cl
-, SO
4 2-Any, 0.2≤x≤0.4,0≤m≤2.
2. method for preparing the transparent laminated double-metal hydroxide film of the described even compact of claim 1 is characterized in that technology is:
A, preparation solubility divalence inorganic salt M
2+Y and solubility trivalent inorganic salt M
3+The mixed solution of Y, total concentration of metal ions is 0.1-0.3mol/L in the solution, divalence trivalent metal cation molar concentration rate is 2-4: 1, Y is NO
3 -, Cl
-, SO
4 2-The inorganic acid radical negatively charged ion;
B, preparation mass percent concentration are the dilute ammonia solution of 0.5-2%;
C, measure isopyknic salts solution and alkaline solution in culture dish, be placed in the moisture eliminator of sealing, 20-30 ℃ of reaction 4-24h down; Reaction is transferred to CO with the film at air-water interface place after finishing
2In the water, with the unreacted mixing salt that flush away adheres to, it is transferred to after washing 1-5 time and carry out drying on the clean substrate under 10～40 ℃, described substrate is slide glass, silicon chip or silicon-dioxide.
3. method according to claim 2 is characterized in that, the M in the steps A
2+Be Ni
2+, Zn
2+In a kind of; M
3+Be Al
3+Or Fe
3+In a kind of; Y is NO
3 -
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710122132 CN100560502C (en) | 2007-09-21 | 2007-09-21 | Laminated double-metal hydroxide film that a kind of even compact is transparent and preparation method thereof |
| PCT/CN2008/070857 WO2009036660A1 (en) | 2007-09-21 | 2008-04-30 | A method for preparing film of layered double hydroxides |
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|---|---|---|---|
| CN 200710122132 CN100560502C (en) | 2007-09-21 | 2007-09-21 | Laminated double-metal hydroxide film that a kind of even compact is transparent and preparation method thereof |
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|---|---|
| CN101157475A true CN101157475A (en) | 2008-04-09 |
| CN100560502C CN100560502C (en) | 2009-11-18 |
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| WO (1) | WO2009036660A1 (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009036660A1 (en) * | 2007-09-21 | 2009-03-26 | Beijing University Of Chemical Technology | A method for preparing film of layered double hydroxides |
| CN101818346A (en) * | 2010-04-15 | 2010-09-01 | 北京化工大学 | Oriented ZnO nano-rod film and preparation method thereof |
| CN101550547B (en) * | 2009-04-14 | 2010-11-03 | 北京化工大学 | A method to prepare nano iron membrane |
| TWI414483B (en) * | 2009-09-22 | 2013-11-11 | Univ Nat Chunghsing | Method for preparing layered double hydroxides |
| CN105334251A (en) * | 2015-11-16 | 2016-02-17 | 安徽师范大学 | Tremella-like Fe-Ni layered double hydroxides, oxygen evolution electrode as well as preparation methods and applications thereof |
| CN107001061A (en) * | 2014-12-17 | 2017-08-01 | 日本碍子株式会社 | Layered double-hydroxide film and the composite containing layered double-hydroxide |
| CN108034988A (en) * | 2017-12-08 | 2018-05-15 | 山东理工大学 | Using porous anodic alumina template as three-dimensional hydrotalcite film of substrate and preparation method thereof |
| CN108046298A (en) * | 2017-12-20 | 2018-05-18 | 国标（北京）检验认证有限公司 | Concentrate the purification process of magnesium isotope oxide |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113278986B (en) * | 2021-04-08 | 2022-04-01 | 深圳大学 | C-axis oriented NiFe-LDH film electrocatalyst and preparation method thereof |
| CN115124061A (en) * | 2022-06-07 | 2022-09-30 | 秦迎 | Polymer modified hydrotalcite-like nano composite material and preparation method thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2003901788A0 (en) * | 2003-04-15 | 2003-05-01 | Commonwealth Scientific And Industrial Research Organisation | Production of layered double hydroxides |
| CN1222467C (en) * | 2003-10-23 | 2005-10-12 | 浙江大学 | Method of preparing bimetal oxide and hydrotalcite |
| CN100427401C (en) * | 2005-12-29 | 2008-10-22 | 北京化工大学 | Preparation method of highly oriented transparent dihydroxy metal oxide film |
| CN100390066C (en) * | 2006-10-12 | 2008-05-28 | 北京化工大学 | Manganese dioxide/hydrotalcite inorganic nanometer piece composite superthin film and its preparation method |
| CN100560502C (en) * | 2007-09-21 | 2009-11-18 | 北京化工大学 | Laminated double-metal hydroxide film that a kind of even compact is transparent and preparation method thereof |
-
2007
- 2007-09-21 CN CN 200710122132 patent/CN100560502C/en not_active Expired - Fee Related
-
2008
- 2008-04-30 WO PCT/CN2008/070857 patent/WO2009036660A1/en active Application Filing
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009036660A1 (en) * | 2007-09-21 | 2009-03-26 | Beijing University Of Chemical Technology | A method for preparing film of layered double hydroxides |
| CN101550547B (en) * | 2009-04-14 | 2010-11-03 | 北京化工大学 | A method to prepare nano iron membrane |
| TWI414483B (en) * | 2009-09-22 | 2013-11-11 | Univ Nat Chunghsing | Method for preparing layered double hydroxides |
| CN101818346A (en) * | 2010-04-15 | 2010-09-01 | 北京化工大学 | Oriented ZnO nano-rod film and preparation method thereof |
| CN107001061A (en) * | 2014-12-17 | 2017-08-01 | 日本碍子株式会社 | Layered double-hydroxide film and the composite containing layered double-hydroxide |
| CN105334251A (en) * | 2015-11-16 | 2016-02-17 | 安徽师范大学 | Tremella-like Fe-Ni layered double hydroxides, oxygen evolution electrode as well as preparation methods and applications thereof |
| CN105334251B (en) * | 2015-11-16 | 2018-05-25 | 安徽师范大学 | The Fe-Ni double-metal hydroxides of class tremelliform analyse oxygen electrode and its preparation method and application |
| CN108034988A (en) * | 2017-12-08 | 2018-05-15 | 山东理工大学 | Using porous anodic alumina template as three-dimensional hydrotalcite film of substrate and preparation method thereof |
| CN108034988B (en) * | 2017-12-08 | 2019-09-06 | 山东理工大学 | Using porous anodic alumina template as three-dimensional hydrotalcite film of substrate and preparation method thereof |
| CN108046298A (en) * | 2017-12-20 | 2018-05-18 | 国标（北京）检验认证有限公司 | Concentrate the purification process of magnesium isotope oxide |
| CN108046298B (en) * | 2017-12-20 | 2021-05-25 | 国标（北京）检验认证有限公司 | Method for purifying concentrated magnesium isotope oxide |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2009036660A1 (en) | 2009-03-26 |
| CN100560502C (en) | 2009-11-18 |
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