CN104911665A - Lithium aluminate porous template and preparation method thereof - Google Patents
Lithium aluminate porous template and preparation method thereof Download PDFInfo
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- CN104911665A CN104911665A CN201510176217.2A CN201510176217A CN104911665A CN 104911665 A CN104911665 A CN 104911665A CN 201510176217 A CN201510176217 A CN 201510176217A CN 104911665 A CN104911665 A CN 104911665A
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Abstract
The invention discloses a lithium aluminate porous template and a preparation method thereof. The method comprises the following steps: 1) preparation of an anodic alumina template; and 2) hydrothermal synthesis preparation of a lithium aluminate porous template by using the anodic alumina template as the aluminum source. The invention also provides the lithium aluminate porous template obtained by the above preparation method. The method controls the preparation conditions of anodic alumina; anodic alumina is used both as a template and as an aluminum source for preparing LiAlO2; the hydrothermal method is employed for the preparation of a fast ion conductor LiAlO2 porous template. The method has the advantages of simple process, easily controlled process, low cost and high yield; compared with other template methods for preparing porous materials, the method uses the template as a starting material to inherit its morphology; and the prepared lithium aluminate porous template with special morphology provides a novel method for the preparation of a nano porous material.
Description
Technical field
The present invention relates to inorganic porous material preparing technical field, particularly a kind of lithium aluminate foraminous die plate and preparation method thereof.
Background technology
The preparation method of inorganic porous ceramic material is a lot, according to the difference of material, structure, pore size and porosity, is suitable for different preparation methods.According to preparation technology, be divided into template and without template.Mainly contain solvent-thermal method and sol-gel method etc. without template, wherein solvent-thermal method is applied widely, but the particle diameter of wayward reaction product.Sol-gel method preparation process is complicated, the particle diameter of same wayward product, and reaction time is longer, there is more by product after reaction, also higher to equipment requirements.Template synthesis porous material, by structure and the size of the accurate control punch of template, but finally needs just can obtain product by certain means removal template.
At present, utilize anodised aluminium for Template preparation Application of micron more and more extensive, technique is more and more ripe.Patent of invention publication number is CN 102274976 A, the Chinese patent that name is called " a kind of anodic oxidation aluminium formwork prepares the method for nano material ", describes with the method for anodised aluminium AAO for Template preparation nano material, simple and practical, easily implements.Be in this way numerous template of representative, the process of its synthesizing nano-porous material, be all only using AAO as a template, by control AAO (Anodic Aluminum Oxide, anodised aluminium) preparation condition, the pattern of regulation and control product and pore size, AAO template is removed by certain means the most at last, thus obtains product.
Summary of the invention
Provide hereinafter about brief overview of the present invention, to provide about the basic comprehension in some of the present invention.Should be appreciated that this general introduction is not summarize about exhaustive of the present invention.It is not that intention determines key of the present invention or integral part, and nor is it intended to limit the scope of the present invention.Its object is only provide some concept in simplified form, in this, as the preorder in greater detail discussed after a while.
The object of the embodiment of the present invention is the defect for above-mentioned prior art, provides lithium aluminate foraminous die plate that a kind of preparation cost is low, productive rate is high and preparation method thereof.
To achieve these goals, the technical scheme that the present invention takes is:
A preparation method for lithium aluminate foraminous die plate, comprises the steps:
1) anodic oxidation aluminium formwork is prepared;
2) take anodic oxidation aluminium formwork as aluminium source, hydrothermal method prepares lithium aluminate foraminous die plate.
The present invention also provides a kind of lithium aluminate foraminous die plate, prepares according to above-mentioned preparation method.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention is by the preparation condition of control AAO, and using AAO both as template, LiAlO is prepared in conduct again
2aluminium source, hydro-thermal prepares fast-ionic conductor LiAlO
2foraminous die plate, there is the advantage that technique is simple, process is easily controlled, cost is low, productive rate is high, compared with the method for other template synthesis porous materials, utilize template as raw material, inherit its shape characteristic, preparing the lithium aluminate foraminous die plate with special microscopic appearance, providing novel method for preparing nano-porous materials.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is LiAlO in embodiment 1
2the XRD figure of foraminous die plate;
Fig. 2 is LiAlO in embodiment 1
2sEM (Scanning Electron Microscope, the scanning electronic microscope) figure of foraminous die plate;
Fig. 3 is XRD (X-ray diffract ion, the X-ray diffraction) figure of LiAlO2 foraminous die plate in embodiment 2;
Fig. 4 is LiAlO in embodiment 2
2the SEM figure of foraminous die plate;
Fig. 5 is LiAlO in embodiment 3
2the XRD figure of foraminous die plate;
Fig. 6 is LiAlO in embodiment 3
2the SEM figure of foraminous die plate;
Fig. 7 is LiAlO in embodiment 4
2the XRD figure of foraminous die plate;
Fig. 8 is LiAlO in embodiment 4
2the SEM figure of foraminous die plate;
Fig. 9 is LiAlO in embodiment 5
2the XRD figure of foraminous die plate;
Figure 10 is LiAlO in embodiment 5
2the SEM figure of foraminous die plate.
Embodiment
For making the object of the embodiment of the present invention, technical scheme and advantage clearly, below in conjunction with the accompanying drawing in the embodiment of the present invention, technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.The element described in an accompanying drawing of the present invention or a kind of embodiment and feature can combine with the element shown in one or more other accompanying drawing or embodiment and feature.It should be noted that for purposes of clarity, accompanying drawing and eliminate expression and the description of unrelated to the invention, parts known to persons of ordinary skill in the art and process in illustrating.Based on the embodiment in the present invention, those of ordinary skill in the art, not paying the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The invention provides a kind of preparation method of lithium aluminate foraminous die plate, comprise the steps:
1) AAO template is prepared:
Anonizing is adopted to prepare AAO template, specifically aluminium foil is through annealing, degrease, polishing, the aluminium foil handled well is clipped in DC power anode as anode, using nickel sheet as negative electrode, put into the phosphoric acid electrolyte of certain temperature, add oxidation voltage, carry out anodic oxidation, after certain electrolysis time, cleaning, drying, obtain prefabricated AAO template.
Described anodic oxidation be with concentration be the phosphoric acid solution of 0.3 ~ 0.5mol/L for electrolytic solution, oxidation voltage 40 ~ 80V, electrolysis temperature 15 ~ 25 DEG C, electrolysis time 1 ~ 3h.
2) with AAO template for aluminium source, Li2CO3 is lithium source, and hydrothermal method prepares lithium aluminate foraminous die plate:
Take the aluminium source of mol ratio 1:2 ~ 1:3 and lithium source to move into and have in anticorrosive PTFE lining autoclave, add the deionized water of reactor volume 80%, after sealing, reactor is heated to 200 ~ 220 DEG C of hydro-thermal reaction 48 ~ 72h; Reaction terminates, and takes out reactor, naturally cools to room temperature, to open after kettle cover through filtering, deionized water and washes of absolute alcohol, drying, the hydrothermal product obtained is 650-750 DEG C of calcining 6h in atmosphere, namely obtains lithium aluminate foraminous die plate.
Preparation method of the present invention is compared to existing general porous material preparation method, and existing method all will consume other materials, as pore former, and method of the present invention, materials used are self raw material.In-situ corrosion pore-forming, its success ratio is high.
The present invention also provides a kind of lithium aluminate foraminous die plate, prepares according to above-mentioned preparation method.
Below by specific embodiment, the present invention is further illustrated:
Embodiment 1
Aluminium foil is through annealing, degrease, polished finish, pre-treatment aluminium foil is clipped in DC power anode as anode, using the nickel sheet to electrode area ratio of 1:1 as negative electrode, according to anodic oxidation condition: the electrolytic solution of concentration 0.3mol/L phosphoric acid solution, 80V oxidation voltage, under the condition that electrolysis temperature is 25 DEG C, anodic oxidation 1h, wash, dry, obtain prefabricated AAO template.
AAO template and the Li of above preparation is taken by the mol ratio of n (Al): n (Li)=1:2
2cO
3put into the autoclave with anticorrosive PTFE lining, add the deionized water of reactor volume 80%, reactor is heated to 220 DEG C of hydro-thermal reaction 72h after sealing, reaction terminates, naturally cool to room temperature, to open after kettle cover through filtering, deionized water and washes of absolute alcohol, drying, in box-type furnace air, 700 DEG C of calcining 6h, obtain white lithium aluminate foraminous die plate.
See Fig. 1 and Fig. 2, be the LiAlO of the present embodiment
2the XRD figure of foraminous die plate and LiAlO
2the SEM figure of foraminous die plate.That XRD spectra obtains is LiAlO
2thing phase, can LiAlO be seen from SEM figure
2it is vesicular structure.
Embodiment 2
Aluminium foil is through annealing, degrease, polished finish, pre-treatment aluminium foil is clipped in DC power anode as anode, using the nickel sheet to electrode area ratio of 1:1 as negative electrode, according to anodic oxidation condition: the electrolytic solution of concentration 0.35mol/L phosphoric acid solution, 70V oxidation voltage, under the condition that electrolysis temperature is 20 DEG C, anodic oxidation 2h, wash, dry, obtain prefabricated AAO template.
AAO template and the Li of above preparation is taken by n (Al): n (Li)=1:2.2
2cO
3put into the reactor with anticorrosive PTFE lining, pour the deionized water accounting for reactor volume 75% into, the well heater after sealing, reactor being placed in 215 DEG C carries out hydro-thermal reaction 66h.Reaction terminates, and naturally cools to room temperature, through filtering, first spending deionized water rinse after opening kettle cover, then uses washes of absolute alcohol, drying, and in box-type furnace air, 750 DEG C of calcining 6h, obtain white lithium aluminate foraminous die plate.
See Fig. 3 and Fig. 4, be the LiAlO of the present embodiment
2the XRD figure of foraminous die plate and LiAlO
2the SEM figure of foraminous die plate.That XRD spectra obtains is LiAlO
2thing phase, can LiAlO be seen from SEM figure
2it is vesicular structure.
Embodiment 3
Aluminium foil is through annealing, degrease, polished finish, pre-treatment aluminium foil is clipped in DC power anode as anode, using the nickel sheet to electrode area ratio of 1:1 as negative electrode, according to anodic oxidation condition: the electrolytic solution of concentration 0.4mol/L phosphoric acid solution, 60V oxidation voltage, under the condition that electrolysis temperature is 22 DEG C, anodic oxidation 3h, wash, dry, obtain prefabricated AAO template.
AAO template and the Li of above preparation is taken by n (Al): n (Li)=1:2.5
2cO
3put into the reactor with anticorrosive PTFE lining, pour the deionized water accounting for reactor volume 70% into, the well heater after sealing, reactor being placed in 210 DEG C carries out hydro-thermal reaction 60h.Reaction terminates, and naturally cools to room temperature, after opening kettle cover through filtering, deionized water and dehydrated alcohol cleans respectively, dry, in box-type furnace air, 650 DEG C of calcining 6h, obtain white lithium aluminate foraminous die plate.
See Fig. 5 and Fig. 6, be the LiAlO of the present embodiment
2the XRD figure of foraminous die plate and LiAlO
2the SEM figure of foraminous die plate.That XRD spectra obtains is LiAlO
2thing phase, can LiAlO be seen from SEM figure
2it is vesicular structure.
Embodiment 4
Aluminium foil is through annealing, degrease, polished finish, pre-treatment aluminium foil is clipped in DC power anode as anode, using the nickel sheet to electrode area ratio of 1:1 as negative electrode, according to anodic oxidation condition: the electrolytic solution of concentration 0.45mol/L phosphoric acid solution, 50V oxidation voltage, under the condition that electrolysis temperature is 18 DEG C, anodic oxidation 2.5h, wash, dry, obtain prefabricated AAO template.
AAO template and the Li of above preparation is taken by n (Al): n (Li)=1:2.8
2cO
3put into reactor, pour the deionized water accounting for reactor volume 90% into, after sealing, reactor is heated to 205 DEG C of hydro-thermal reaction 54h.After reaction terminates, naturally cool to room temperature, after opening kettle cover through filtering, deionized water and dehydrated alcohol cleans respectively, dry, in box-type furnace air, 700 DEG C of calcining 6h, obtain white lithium aluminate foraminous die plate.
See Fig. 7 and Fig. 8, be the LiAlO of the present embodiment
2the XRD figure of foraminous die plate and LiAlO
2the SEM figure of foraminous die plate.That XRD spectra obtains is LiAlO
2thing phase, can LiAlO be seen from SEM figure
2it is vesicular structure.
Embodiment 5
Aluminium foil is through annealing, degrease, polished finish, pre-treatment aluminium foil is clipped in DC power anode as anode, using the nickel sheet to electrode area ratio of 1:1 as negative electrode, according to anodic oxidation condition: the electrolytic solution of concentration 0.5mol/L phosphoric acid solution, 40V oxidation voltage, under the condition that electrolysis temperature is 15 DEG C, anodic oxidation 1.5h, wash, dry, obtain prefabricated AAO template.
AAO template and the Li of above preparation is taken by n (Al): n (Li)=1:3
2cO
3put into reactor, pour the deionized water accounting for reactor volume 85% into, after sealing, reactor is heated to 200 DEG C of hydro-thermal reaction 48h.After reaction terminates, naturally cool to room temperature, after opening kettle cover through filtering, deionized water and dehydrated alcohol cleans respectively, dry, in box-type furnace air, 700 DEG C of calcining 6h, obtain white lithium aluminate foraminous die plate.
See Fig. 9 and Figure 10, be the LiAlO of the present embodiment
2the XRD figure of foraminous die plate and LiAlO
2the SEM figure of foraminous die plate.That XRD spectra obtains is LiAlO
2thing phase, can LiAlO be seen from SEM figure
2it is vesicular structure.
State in each embodiment on the invention, the sequence number of embodiment is only convenient to describe, and does not represent the quality of embodiment.The description of each embodiment is all emphasized particularly on different fields, in certain embodiment, there is no the part described in detail, can see the associated description of other embodiments.
In the embodiments such as apparatus and method of the present invention, obviously, each parts or each step reconfigure after can decomposing, combine and/or decomposing.These decompose and/or reconfigure and should be considered as equivalents of the present invention.Simultaneously, above in the description of the specific embodiment of the invention, the feature described for a kind of embodiment and/or illustrate can use in one or more other embodiment in same or similar mode, combined with the feature in other embodiment, or substitute the feature in other embodiment.
Should emphasize, term " comprises/comprises " existence referring to feature, key element, step or assembly when using herein, but does not get rid of the existence or additional of one or more further feature, key element, step or assembly.
Although last it is noted that described the present invention and advantage thereof in detail above, be to be understood that and can carry out various change when not exceeding the spirit and scope of the present invention limited by appended claim, substituting and converting.And scope of the present invention is not limited only to the specific embodiment of process, equipment, means, method and step described by specification sheets.One of ordinary skilled in the art will readily appreciate that from disclosure of the present invention, can use perform the function substantially identical with corresponding embodiment described herein or obtain and its substantially identical result, existing and that will be developed in the future process, equipment, means, method or step according to the present invention.Therefore, appended claim is intended to comprise such process, equipment, means, method or step in their scope.
Claims (10)
1. a preparation method for lithium aluminate foraminous die plate, is characterized in that, comprises the steps:
1) anodic oxidation aluminium formwork is prepared;
2) take anodic oxidation aluminium formwork as aluminium source, hydrothermal method prepares lithium aluminate foraminous die plate.
2. the preparation method of lithium aluminate foraminous die plate according to claim 1, is characterized in that:
Described step 1) comprising:
Anonizing is adopted to prepare anodic oxidation aluminium formwork, specifically aluminium foil is through annealing, degrease, polishing, the aluminium foil handled well is clipped in DC power anode as anode, using nickel sheet as negative electrode, put into the phosphoric acid electrolyte of certain temperature, add oxidation voltage, carry out anodic oxidation, after certain electrolysis time, cleaning, drying, obtain prefabricated anodic oxidation aluminium formwork.
3. the preparation method of lithium aluminate foraminous die plate according to claim 2, is characterized in that, described anodic oxidation be with concentration be the phosphoric acid solution of 0.3 ~ 0.5mol/L for electrolytic solution, oxidation voltage 40 ~ 80V, electrolysis temperature 15 ~ 25 DEG C, electrolysis time 1 ~ 3h.
4. the preparation method of the lithium aluminate foraminous die plate according to claim 1,2 or 3, is characterized in that:
Described step 2) comprising: aluminium source and lithium source are moved in autoclave, adds deionized water; After sealing, hydro-thermal reaction is carried out in reactor heating; Reaction terminates, and takes out reactor, naturally cools to room temperature, to open after kettle cover through filtering, cleaning, dry, and the hydrothermal product obtained is calcined in atmosphere, namely obtains lithium aluminate foraminous die plate.
5. the preparation method of a kind of nanometer lithium aluminate foraminous die plate according to claim 4, it is characterized in that, described lithium source is Li
2cO
3; The add-on of described deionized water is the 70-90% of reactor volume.
6. the preparation method of lithium aluminate foraminous die plate according to claim 4, is characterized in that, be provided with anticorrosive PTFE lining in described autoclave.
7. the preparation method of lithium aluminate foraminous die plate according to claim 4, it is characterized in that, described aluminium source and lithium source mol ratio are 1:2 ~ 3, described cleaning deionized water and dehydrated alcohol lotion.
8. the preparation method of lithium aluminate foraminous die plate according to claim 4, is characterized in that, hydro-thermal reaction 48 ~ 72h is carried out in described reactor heating 200 ~ 220 DEG C.
9. the preparation method of lithium aluminate foraminous die plate according to claim 4, it is characterized in that, the temperature of described calcining is 650-750 DEG C, and calcination time is 6h.
10. a lithium aluminate foraminous die plate, is characterized in that, prepares according to the preparation method described in any one of claim 1-9.
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Cited By (1)
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| CN107082439A (en) * | 2017-05-09 | 2017-08-22 | 东北大学 | A kind of preparation method of nanoscale lithium aluminate |
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