CN108034988A - Using porous anodic alumina template as three-dimensional hydrotalcite film of substrate and preparation method thereof - Google Patents
Using porous anodic alumina template as three-dimensional hydrotalcite film of substrate and preparation method thereof Download PDFInfo
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- CN108034988A CN108034988A CN201711297900.7A CN201711297900A CN108034988A CN 108034988 A CN108034988 A CN 108034988A CN 201711297900 A CN201711297900 A CN 201711297900A CN 108034988 A CN108034988 A CN 108034988A
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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
- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/12—Liquid-phase epitaxial-layer growth characterised by the substrate
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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
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Abstract
The invention belongs to inorganic functional material technical field, and in particular to a kind of using porous anodic alumina template as three-dimensional hydrotalcite film of substrate and preparation method thereof.The three-dimensional hydrotalcite film using porous anodic alumina template as substrate is in the presence of strong acidic condition and cadmium ion, by homoepitaxial goes out nickel aluminium in the outer surface of porous anodic alumina template and duct or zinc-aluminum gavite crystal obtains.The houghite crystal that the homoepitaxial in the surface of porous anodic alumina template and duct is prepared in the present invention is tightly combined with substrate, not easily to fall off.The present invention obtain using porous anodic alumina template be substrate three-dimensional hydrotalcite film in use it is possible to prevente effectively from be lost in, be easily isolated and reuse, catalysis, absorption, separation etc. there is excellent application prospect.Preparation condition of the present invention is gentle, technical process is simple, success rate is high.
Description
Technical field
The invention belongs to inorganic functional material technical field, and in particular to one kind is using porous anodic alumina template as substrate
Three-dimensional hydrotalcite film and preparation method thereof.
Background technology
Houghite is a kind of complex metal hydroxide with hydrotalcite laminar crystalline structure, by positively charged gold
Belong to hydroxide layer and interlayer charge balance anion is formed.Its laminate chemical composition can be adjusted as needed, and then
Cause the respective changes such as laminate chemical property, laminate charge density；Interlayer anion can be needed according to application using intercalation or
The mode of ion exchange carries out ionic species and the modulation of quantity, improves the overall performance of hydrotalcite-like materials.By houghite
It is fixed in particular substrate and forms film and to carry out application study be research hotspot nearly ten years.Houghite after immobilization
The shortcomings that film can not only overcome powder body material easily to reunite, hardly possible separation so that it should absorption, catalysis, separation etc.
With more convenient, the new fields such as anti-corrosion of metal, surface infiltration, electrochemistry, sensor can also be extended to.Due to zinc,
Nickel and its hydroxide and oxide are in the excellent properties of catalysis, anti-corrosion of metal, electrochemistry etc., related hydrotalcite film
Preparation research also get the attention.
It is substrate that the preparation of hydrotalcite film, which generally selects certain material, and precipitating reagent or buffering are added in reaction solution
System by solution adjust to faintly acid to alkalescence so that houghite crystal deposition or directly in substrate in-situ chemical give birth to
It is long, form corresponding hydrotalcite film.Chen etc. is successively in Adv.Mater.2006,18 (23):3089-3093 and
Angew.Chem.Int.Ed.2008,47:Report is using anodised aluminium/aluminium as substrate in 2466-2469, using ammonium nitrate-ammonia
The control of water buffer system contains Ni2+Or Zn2+Reaction solution pH value be 6.5, two dimension is prepared for by in-situ chemical growth method
Nickel aluminium and zinc-aluminum gavite film.Guo etc. is in Langmuir 2009,25 (17):Reported in 9894-9897 using aluminium as substrate,
Using same reaction solution and buffer system, it is 6.5 to adjust pH value, and in-situ chemical growth method is successfully prepared zinc-aluminium class neatly
Stone film, and investigated its influence to aluminium substrate antiseptic property.
Chinese patent CN1986419A discloses a kind of vertically oriented hydrotalcite film in nano and micron composite structure and its preparation side
Method, Chinese patent CN1923363A disclose a kind of preparation method for synthesizing hydrotalcite thin film by alcohol oxidation reaction catalyst, on
Two patents are stated using anodised aluminium/aluminium as substrate, it is molten containing bivalent metal ion using ammonium nitrate-ammonium hydroxide buffer system control
The pH value of liquid is respectively 4.5~10 and 6.3~7.3, and carries out follow-up film in-situ chemical growth response in this solution.In
State patent CN106868483A discloses a kind of aluminium and aluminum alloy surface prepares the preparation method of ternary houghite film, will be by urinating
The precipitating reagent stirring and dissolving that element is formed with ammonium fluoride grows legal system in the solution containing bivalent metal ion by in-situ chemical
The ternary houghite film anticorrosion layer of standby metal surface.Xue etc. (Chem.Commun., 2014,50:2301-2303.) innovation
Property under strongly acidic conditions (reaction solution initial pH value as low as 2), it is thin to be successfully prepared NiAl-HTLcs on aluminum substrates
Film, concurrently houghite growth is relatively slow under acid condition now, and the size that it is crystallized is smaller, is tightly combined with substrate, no
It is easy to fall off.
In recent ten years, porous anodic alumina template is received significant attention as the effective template for preparing nano material.
It has regular three-dimensional open-framework, good chemical stability and heat endurance, higher hardness and larger specific surface area.
Can be not only aluminized hydrotalcite film if using growth substrate of the porous anodic alumina template for hydrotalcite film
Growth provides abundant silicon source, can also be class by regulating and controlling its aperture and duct state, such as orifice throat length, pore wall thickness
The growth of hydrotalcite provides more spaces, hydrotalcite film is created on the outer surface and hole of porous anodic alumina template
In road (inner surface), three-dimension film is formed.How rationally to control reaction condition or aided in using instrument, make houghite crystal
It is equably to realize the key of three-dimensional hydrotalcite film preparation in the surfaces externally and internally growth at the same time of porous anodic alumina template
Problem.
Yang etc. is in Mater.Lett.2008,68:Report uses hexa as precipitating reagent in 1302-1304,
It is successfully prepared zinc-aluminum gavite film on the outer surface of porous anodic alumina template, but in template duct and is not present zinc
Aluminium houghite crystal.Ding etc. is in Mater.Lett.2012,77:Report will be dissolved with metal nitrate and hexa-methylene in 1-3
The mixed solution of tetramine flows through the solution after heating by molecular sieve filtration Posterior circle after 90 DEG C of heating, with constant flow pump porous
Anodic oxidation aluminium formwork, the NiAl-HTLcs that can be prepared in porous anodic aluminium oxide surfaces externally and internally dense growth are thin
Film, the hydrotalcite films of other compositions fail preparation, it is to be issued to its in instrument auxiliary diffusion to prepare purpose.
Above result of study is analyzed to find：For the substrate with pore passage structure, since houghite crystal is in weakly acidic pH
Or formed and grown soon under alkaline condition, the blocking of porous anodic aluminium oxide substrate opening of the channel is easily caused, is caused on inner surface
It is difficult to form houghite crystal；Diffusion method is aided in using instrument, some houghite crystal can be realized by forced circulation
Nucleation and growth in inner surface.Up to the present, other easier methods be yet there are no and realize three-dimensional hydrotalcite film
The report of preparation.
The content of the invention
The object of the present invention is to provide a kind of three-dimensional hydrotalcite film using porous anodic alumina template as substrate, its
Homoepitaxial goes out nickel aluminium or zinc-aluminum gavite crystal in the outer surface and duct of porous anodic alumina template；The present invention is at the same time
Its preparation method is provided, reaction condition is gentle, technical process is simple, success rate is high.
Three-dimensional hydrotalcite film of the present invention using porous anodic alumina template as substrate：Strong acidic condition and
In the presence of cadmium ion, homoepitaxial goes out nickel aluminium or zinc-aluminum gavite in the outer surface and duct of porous anodic alumina template
Crystal, obtains the three-dimensional hydrotalcite film using porous anodic alumina template as substrate；
Wherein：
The strong acidic condition is that pH value is 1~2.5, preferably 1.8~2.5.
The houghite is formed by positively charged laminate and interlayer anion ordered arrangement, its chemical general formula is generally
[M1-xAlx(OH)2]x+(NO3 -)x·mH2O, wherein M are Zn or Ni, 0.2≤x≤0.4,0≤m≤2.
Preparation method of the present invention using porous anodic alumina template as the three-dimensional hydrotalcite film of substrate is
Cadmium nitrate is dissolved in the aqueous solution of nickel nitrate or zinc nitrate, forms mixed solution, add porous anodic alumina template, instead
Should, obtain the three-dimensional hydrotalcite film using porous anodic alumina template as substrate.
Wherein：
In the mixed solution, the molar concentration of cadmium ion is 0.1~1.0mol/L, preferably 0.5~1.0mol/L.
In the mixed solution, the molar concentration of nickel ion is 0.1~1.0mol/L, preferably 0.5~1.0mol/L；Zinc from
The molar concentration of son is 0.1~1.0mol/L, preferably 0.1~0.5mol/L.
The pH value of the mixed solution is 1~2.5, preferably 1.8~2.5.Since houghite is in the highly acid of the present invention
Under the conditions of, it is impossible to grow, three-dimensional nickel aluminium or zinc-aluminum gavite film can not be obtained.Therefore, the present invention under strongly acidic conditions,
Using in situ synthesis, three-dimensional nickel aluminium or zinc-aluminum gavite is prepared on porous anodic alumina template using cadmium ion
Film.
The reaction temperature is 60~90 DEG C, preferably 70~85 DEG C；Reaction time is 1~48h, preferably 6~12h.
Any precipitating reagent need not be added in the mixed solution.
The present invention by experimental studies have found that, when cadmium ion individualism, can promote vigorous on porous anodic alumina template
The formation of nurse stone (AlOOH).According to document Chem.Mater.2012,24:81-87 reports that boehmite is to form the neatly of class containing aluminium
One of presoma of stone crystal, nickel, zinc metal ion absorption on boehmite after can gradate as houghite crystal, this can
Can be the reason for successfully preparing three-dimensional nickel aluminium or zinc-aluminum hydrotalcite film under strongly acidic conditions.
Beneficial effects of the present invention are as follows：
The present invention is by adding cadmium ion, in the case where pH value is 1~2.5 strong acidic condition so that porous anodic aluminium oxide
Homoepitaxial goes out nickel aluminium or zinc-aluminum gavite crystal in the outer surface and duct of template.The present invention expands without instrument assisting ion
Dissipate, without any precipitating reagent is added, only by simply controlling reaction condition to may be implemented in porous anodic alumina template
Outer surface homoepitaxial three-dimensional nickel aluminium or zinc-aluminum gavite film.
Preparation condition of the present invention is gentle, technical process is simple, success rate is high, and houghite crystal is prepared in porous sun
The three-dimensional hydrotalcite film of homoepitaxial, these crystal are tightly combined with substrate in the surface and duct of pole alumina formwork,
It is not easily to fall off.The present invention obtain using porous anodic alumina template as substrate three-dimensional hydrotalcite film in use
It is possible to prevente effectively from being lost in, it is easily isolated and reuses, there is excellent application prospect in catalysis, absorption, separation etc..
Brief description of the drawings
Fig. 1 is the thin as the three-dimensional houghite of substrate using porous anodic alumina template of the preparation of the embodiment of the present invention 1~5
X-ray diffraction (XRD) figure of film；
Wherein：A, film prepared by embodiment 1；B, film prepared by embodiment 2；C, film prepared by embodiment 3；D, reality
Apply the film of the preparation of example 4；E, film prepared by embodiment 5；
Fig. 2 is the XRD diagram of film prepared by comparative example 1~3；
Wherein：A, film prepared by comparative example 1；B, film prepared by comparative example 2；C, film prepared by comparative example 3；
Fig. 3 is sweeping using porous anodic alumina template as substrate three-dimensional NiAl-HTLcs film prepared by embodiment 1
Retouch electron microscope (SEM) figure；
Fig. 4 is the SEM figures of film prepared by comparative example 1.
Embodiment
The present invention is described further with reference to embodiments.
Embodiment 1
By 8.90g Ni (NO3)2·6H2O is added in 30ml deionized waters, and ultrasound makes it fully dissolve；Weigh 9.35g Cd
(NO3)2·4H2O is added in solution, and the pH value of solution is about 1.8, then porous anodic alumina template is immersed in the solution, and
Solution is warming up to 80 DEG C, isothermal reaction 12h, takes out porous anodic alumina template, and is cleaned with deionized water, room temperature is done
It is dry, obtain the three-dimensional NiAl-HTLcs film using porous anodic alumina template as substrate.XRD detections, knot are carried out to film
Fruit is as shown in a in Fig. 1；SEM detections are carried out to film, the results are shown in Figure 3.
Embodiment 2
By 0.90g Zn (NO3)2·6H2O is added in 30ml deionized waters, and ultrasound makes it fully dissolve；Weigh 9.35g Cd
(NO3)2·4H2O is added in solution, and the pH value of solution is about 2.3, then porous anodic alumina template is immersed in the solution, and
Solution is warming up to 80 DEG C, isothermal reaction 12h, takes out porous anodic alumina template, and is cleaned with deionized water, room temperature is done
It is dry, obtain the three-dimensional zinc-aluminum gavite film using porous anodic alumina template as substrate.XRD detections, knot are carried out to film
Fruit is as shown in b in Fig. 1.
Embodiment 3
By 4.50g Zn (NO3)2·6H2O is added in 30ml deionized waters, and ultrasound makes it fully dissolve；Weigh 4.67g Cd
(NO3)2·4H2O is added in solution, and the pH value using aqueous solution of nitric acid adjustment solution is about 2.3, then by porous anodic aluminium oxide
Template is immersed in the solution, and solution is warming up to 80 DEG C, isothermal reaction 12h, takes out porous anodic alumina template, and spend
Ionized water cleans, and drying at room temperature, obtains the three-dimensional zinc-aluminum gavite film using porous anodic alumina template as substrate.To thin
Film carries out XRD detections, as a result as shown in c in Fig. 1.
Embodiment 4
By 4.45g Ni (NO3)2·6H2O is added in 30ml deionized waters, and ultrasound makes it fully dissolve；Weigh 4.67g Cd
(NO3)2·4H2O is added in solution, and the pH value using aqueous solution of nitric acid adjustment solution is about 2.3, then by porous anodic aluminium oxide
Template is immersed in the solution, and solution is warming up to 85 DEG C, isothermal reaction 12h, takes out porous anodic alumina template, and spend
Ionized water cleans, and drying at room temperature, obtains the three-dimensional NiAl-HTLcs film using porous anodic alumina template as substrate.To thin
Film carries out XRD detections, as a result as shown in d in Fig. 1.
Embodiment 5
By 8.90g Ni (NO3)2·6H2O is added in 30ml deionized waters, and ultrasound makes it fully dissolve；Weigh 9.35g Cd
(NO3)2·4H2O is added in solution, and the pH value of solution is about 1.8, then porous anodic alumina template is immersed in the solution, and
Solution is warming up to 80 DEG C, isothermal reaction 6h, takes out porous anodic alumina template, and is cleaned with deionized water, drying at room temperature,
Obtain the three-dimensional NiAl-HTLcs film using porous anodic alumina template as substrate.XRD detections are carried out to film, as a result such as
In Fig. 1 shown in e.
Comparative example 1
By 8.90g Ni (NO3)2·6H2O is added in 30ml deionized waters, and ultrasound makes it fully dissolve；It is water-soluble using nitric acid
The pH value of liquid adjustment solution is about 2.0, then porous anodic alumina template is immersed in the solution, and solution is warming up to 80
DEG C, isothermal reaction 12h, takes out porous anodic alumina template, and is cleaned with deionized water, and drying at room temperature, obtains film.To thin
Film carries out XRD detections, as a result as shown in a in Fig. 2；SEM detections are carried out to film, the results are shown in Figure 4.
Comparative example 2
By 0.90g Zn (NO3)2·6H2O is added in 30ml deionized waters, and ultrasound makes it fully dissolve；It is water-soluble using nitric acid
The pH value of liquid adjustment solution is about 2.3, then porous anodic alumina template is immersed in the solution, and solution is warming up to 80
DEG C, isothermal reaction 12h, takes out porous anodic alumina template, and is cleaned with deionized water, and drying at room temperature, obtains film.To thin
Film carries out XRD detections, as a result as shown in b in Fig. 2.
Comparative example 3
By 9.35g Cd (NO3)2·4H2O is added in 30ml deionized waters, and ultrasound makes it fully dissolve；The pH value of solution is about
For 2.4, then porous anodic alumina template immersed in the solution, and solution is warming up to 80 DEG C, isothermal reaction 12h, taken out
Porous anodic alumina template, and cleaned with deionized water, drying at room temperature, obtains film.XRD detections are carried out to film, as a result
As shown in c in Fig. 2.
By the porous anodic alumina template prepared in embodiment 1~5 for substrate three-dimensional NiAl-HTLcs film into
Row XRD analysis, as a result such as Fig. 1.Curve a~e corresponds to the film in embodiment 1~5 respectively in Fig. 1.It can be seen by XRD data
Go out, 2 θ=10 ° of houghite crystal and 2 θ=20 ° diffraction maximums occur, d crystallization situation it is slightly poor, 2 θ=20 ° diffraction maximums compared with
Weak, which illustrates that preparation method using the present invention can successfully prepare houghite crystal.
Film prepared by comparative example 1~3 is subjected to XRD analysis, the results are shown in Figure 2, it can be found that using single
Nickel ion, zinc ion or cadmium-ion solution, under the conditions of similar solution ph, 2 θ=10 ° and 2 θ=20 ° diffraction maximums do not go out
It is existing, then it can not generate houghite crystal.
Fig. 3 is that the SEM that embodiment 1 is prepared using porous anodic alumina template as substrate three-dimensional hydrotalcite film schemes；Fig. 4
The SEM figures of the film prepared for comparative example 1.Compare Fig. 3 and Fig. 4 it can be found that preparation method using the present invention can obtain
Three-dimensional hydrotalcite film using porous anodic alumina template as substrate, and under similar solution ph, single nickel from
Crystallization and growth of the houghite crystal in template surface can not be realized in sub- solution.
By above experimental result it can be found that the addition of cadmium ion is for strongly acidic solution bar in preparation method of the present invention
The generation of hydrotalcite crystal has important facilitation under part.It can promote vigorous nurse on alumina formwork during cadmium ion individualism
The formation of stone (AlOOH).Boehmite is one of presoma to form aluminized hydrotalcite crystal, and nickel, zinc metal ion absorption exist
It can be gradated after on boehmite as houghite crystal.Therefore preparation method using the present invention can be realized successfully in strong acid
Property solution in prepare three-dimensional houghite crystal film.
Claims (10)
- A kind of 1. three-dimensional hydrotalcite film using porous anodic alumina template as substrate, it is characterised in that：Strong acidic condition In the presence of cadmium ion, homoepitaxial goes out nickel aluminium or zinc-aluminium class neatly in the outer surface and duct of porous anodic alumina template Stone crystal, obtains the three-dimensional hydrotalcite film using porous anodic alumina template as substrate.
- 2. the three-dimensional hydrotalcite film according to claim 1 using porous anodic alumina template as substrate, its feature It is：The strong acidic condition is that pH value is 1~2.5.
- 3. the three-dimensional hydrotalcite film according to claim 2 using porous anodic alumina template as substrate, its feature It is：The strong acidic condition is that pH value is 1.8~2.5.
- 4. the three-dimensional hydrotalcite film according to claim 1 using porous anodic alumina template as substrate, its feature It is：The houghite is formed by positively charged laminate and interlayer anion ordered arrangement, its chemical general formula is [M1-xAlx (OH)2]x+(NO3 -)x·mH2O, wherein M are Zn or Ni.
- A kind of 5. preparation side using porous anodic alumina template as the three-dimensional hydrotalcite film of substrate described in claim 1 Method, it is characterised in that：Cadmium nitrate is dissolved in the aqueous solution of nickel nitrate or zinc nitrate, forms mixed solution, add porous anode Alumina formwork, reaction, obtains the three-dimensional hydrotalcite film using porous anodic alumina template as substrate.
- 6. the preparation side according to claim 5 using porous anodic alumina template as the three-dimensional hydrotalcite film of substrate Method, it is characterised in that：In the mixed solution, the molar concentration of cadmium ion is 0.1~1.0mol/L.
- 7. the preparation side according to claim 5 using porous anodic alumina template as the three-dimensional hydrotalcite film of substrate Method, it is characterised in that：In the mixed solution, the molar concentration of nickel ion is 0.1~1.0mol/L；The molar concentration of zinc ion For 0.1~1.0mol/L.
- 8. the preparation side according to claim 7 using porous anodic alumina template as the three-dimensional hydrotalcite film of substrate Method, it is characterised in that：In the mixed solution, the molar concentration of nickel ion is 0.5~1.0mol/L；The molar concentration of zinc ion For 0.1~0.5mol/L.
- 9. the preparation side according to claim 5 using porous anodic alumina template as the three-dimensional hydrotalcite film of substrate Method, it is characterised in that：The reaction temperature is 60~90 DEG C, and the reaction time is 1~48h.
- 10. the preparation according to claim 9 using porous anodic alumina template as the three-dimensional hydrotalcite film of substrate Method, it is characterised in that：The reaction temperature is 70~85 DEG C, and the reaction time is 6~12h.
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| CN112354513A (en) * | 2020-11-09 | 2021-02-12 | 榆林学院 | Zn2+-Al3+-CO32-LDHs @ Al adsorbing material and application thereof in adsorbing fluorine ions by recycling |
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| CN112354513A (en) * | 2020-11-09 | 2021-02-12 | 榆林学院 | Zn2+-Al3+-CO32-LDHs @ Al adsorbing material and application thereof in adsorbing fluorine ions by recycling |
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