CN105858721A - Preparation method of monoatomic layer titanium oxide nanosheet colloidal solution - Google Patents
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Abstract
The present invention discloses a preparation method of a monoatomic layer titanium oxide nanosheet colloidal solution. A titanium source, a potassium source and a lithium source as the original reactants are subjected to high-temperature calcination, ion exchange and intercalation peeling process to obtain the monoatomic layer titanium oxide nanosheet colloidal solution. The method specifically includes the following steps: 1) high-temperature calcination: mixing the original reactants of titanium source, potassium source and lithium source, conducting high-temperature calcination, and cooling to room temperature to obtain a mixed initial product; 2) ion exchange: dispersing the mixed initial product in a solution of hydrochloric acid to form a dispersion liquid, aging the dispersion liquid at room temperature for some time, and conducting filtration, washing and drying to obtain a powder product; and 3) intercalation peeling: dispersing the powder product in an aqueous solution, adding a certain amount of an organic ammonium salt, mixing evenly, shocking for in a period of time in a horizontal shaking table to obtain the homogeneous and stable monoatomic layer titanium oxide nanosheet colloidal solution. The method has the advantages of simpleness, low cost, little pollution and suitability for batch production.
Description
Technical field
The present invention relates to new chemical materials synthesis, light-catalysed technical field, be related specifically to a kind of single former
The preparation method of sublayer TiOx nano sheet colloid solution.
Background technology
Since professor An Deliehaimu of Univ Manchester UK waits the research about Graphene to be awarded
Since Nobel prizes for physics in 2010, Graphene has the structure of single or multiple carbon atomic layer thickness with it
Feature, high electron mobility, good mechanical flexibility, chemical stability and optical transparence, with
And the conduction of excellence, heat conductivility, at lithium ion battery, ultracapacitor, solaode, heat conducting film
Etc. aspect show wide application prospect.As there is the Two-dimensional Inorganic material of similar graphene-structured, also
Receive concern and pay attention to, such as two dimension sulfide (MoS2,WS2Deng), have for relative Graphene suitably
Quasiconductor band gap, has the highest research and using value at electronics approach.
Titanium oxide is as important semiconductor functional material, green non-poisonous with it, chemism is high, photocatalysis
The advantages such as excellent performance, have obtained widely in fields such as self-cleaning coating, light degradation coating, energy storage
Application.Prepare the TiOx nano structure of different dimensions and pattern at present, as zero dimension titanium oxide is received
Rice grain, one-dimensional nanotube, nano wire etc., present the physicochemical characteristics made new advances.This kind of new structure
In the middle of design, there is the two-dimentional monoatomic layer ultra-thin TiOx nano sheet of similar graphene-structured, there is atom
The flat surface of level and the ultrathin of a nanometer, thus possess high Optical Electro-Chemistry activity and excellent colloid
Solution dispersion, has huge using value at aspects such as automatically cleaning, photocatalysis coating and electrochemical energy storages.
The existing technical literature about above-mentioned two dimension monoatomic layer ultra-thin TiOx nano sheet is less, Chinese patent
Document number CN104085920A open (bulletin) day 2014.10.28, disclose a kind of two-dimensional sheet titanium oxide
The preparation method of nanometer sheet material, this technology is with three-dimensional Ti2AlC2Powder is raw material, is immersed in HF and works as
In to remove Al atom, thus obtain retain two-dimensional structure TiO2Nanometer sheet, but there is reaction in this technique
System has the HF of severe corrosive and contaminative, and the thickness distribution of product is uneven, and major part is received 10
More than meter, do not reach the thickness of monolayer.Chinese patent literature CN104628030A open (bulletin) day
2015.05.20, disclosing the preparation method of a kind of floride-free two dimensional oxidation titanium sheet layer material, the method uses solvent
Thermal process is hydrolyzed by concentrated hydrochloric acid suppression isopropyl titanate, obtains the titanium oxide powder of similar graphene-structured.Should
Technique reduces contaminative, and the nanometer sheet thickness obtained still reaches to less than mono-layer oxidized titanium on 2-5nm, purity
Standard, and be not easy to large-scale mass production.Therefore, a kind of new method is developed high-purity for obtaining
The monoatomic layer titanium oxide thin slice of degree, and there is good stability and can be mass, important by having
Meaning.
Summary of the invention
It is an object of the invention to propose the preparation method of a kind of monoatomic layer TiOx nano sheet colloid solution,
Exchanged by high-temperature calcination, ion and intercalation is peeled off, obtained the monatomic of the purity stable homogeneous more than 95%
Layer TiOx nano sheet colloid solution, and method is easy and simple to handle, environmental pollution is little, can produce in batches.
To this end, the present invention is by the following technical solutions:
A kind of preparation method of monoatomic layer TiOx nano sheet colloid solution, with titanium source, potassium source, lithium source be
Primitive reaction thing, through high-temperature calcination, ion exchange and intercalation stripping technology, obtains monoatomic layer titanium oxide
Nanometer sheet colloid solution, specifically includes following steps:
1) high-temperature calcination: with titanium source, potassium source, lithium source be primitive reaction thing, mix by a certain percentage through too high
Temperature calcining, naturally cools to room temperature, obtains mixing head product；
2) ion exchange: mixing head product is dispersed in formation dispersion liquid in the middle of hydrochloric acid solution, dispersion liquid is existed
It is aged a period of time under room temperature, collects obtain powder body product by filtration, cleaning, baking step subsequently；
3) intercalation is peeled off: is dispersed in the middle of aqueous solution by powder body product, is subsequently added a certain amount of organic ammonium salt,
Mix homogeneously, shakes a period of time on horizontal shaker, and the monoatomic layer titanium oxide i.e. obtaining stable homogeneous is received
Rice sheet colloid solution solution.
Preferably, the purity of described monoatomic layer TiOx nano sheet colloid solution is more than 95%, described monatomic
The length of side of layer TiOx nano sheet is 100-1000nm, thickness is 1.5-1.7nm, wherein titanium elements and oxygen element
Mass ratio be 0.87:1 0.91:1.
Preferably, described titanium source, potassium source, the mixed proportion in lithium source be elemental lithium content, Determination of Potassium,
The mol ratio of titanium elements content is: 1:(2～10): (5～30).
Preferably, described titanium source is the arbitrary proportion mixture of one or more in industrial oxidation titanium；Described
Potassium source be the one in industrial potassium chloride, potassium nitrate, potassium carbonate, potassium sulfate, potassium phosphate or potassium bromide or
Several arbitrary proportion mixture；Described lithium source be industrial chlorinations lithium, lithium nitrate, lithium carbonate, lithium sulfate,
The arbitrary proportion mixture of one or more in lithium phosphate or lithium bromide.
Preferably, described high-temperature calcination comprises the steps:
1) just burn: primitive reaction thing is ground 10-50 minute in mortar, puts in platinum crucible, at 600 DEG C
900 DEG C are placed down in chamber type electric resistance furnace interior calcining 1-5 hour, and heating rate is 10 DEG C/min of 1 DEG C/min, with
After from chamber type electric resistance furnace thorax, directly take out quenching, and grind 10-50 minute in mortar；
2) burn eventually: the first burning product after grinding is put in platinum crucible, is placed at 900 DEG C 1800 DEG C
Calcining 10-72 hour in chamber type electric resistance furnace.
Preferably, the concentration of described hydrochloric acid solution is 0.1mol/L 10mol/L, and the concentration of described dispersion liquid is
1g/L—20g/L；
Preferably, described digestion time is 1-8 days, and changes the hydrochloric acid solution of same concentrations in each interval of one day
Once.
Preferably, described filtration, cleaning, drying steps include the following:
1) filter: by the dispersion liquid after ageing, through filtering, obtain aqueous powder body product；
2) clean: mix with one or several the arbitrary proportion in deionized water, dehydrated alcohol or acetone
Bonding solvent cleans above-mentioned aqueous powder body product, until pH value is between 7.0-9.0；
3) it is dried: the aqueous powder body product after cleaning is dried 5-24 hour with 50 DEG C 150 DEG C in an oven,
Obtain the powder body product being dried.
Preferably, the mass percent concentration in the middle of aqueous solution of described organic ammonium salt is 0.1% 5%, institute
Stating organic ammonium salt is Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH or the tetrabutyl
The arbitrary proportion mixture of one or more in ammonium hydroxide.
Preferably, the described time shaken on horizontal shaker is 2 40 days, and concussion speed is 100 300
rpm。
The present invention uses above technical scheme, has following technical effect that 1) present invention use calcining and insert
Layer stripping technology, simple process, is prone to mass industrialized production；And use the system of solvent thermal process,
Exist and be difficult to the deficiency such as batch production and process costs costliness；2) the titanium oxide colloid solution that the present invention obtains,
Wherein the thickness of TiOx nano thin slice is between 1.5-1.7nm, relatively for other techniques, has less
Thickness, has reached the theoretical value of monoatomic layer；2) the titanium oxide colloid solution that the present invention obtains, wherein single former
The high purity 95% of sublayer TiOx nano sheet, its productivity is significantly larger than other technique, photocatalytic degradation,
Automatic cleaning coating, lithium ion battery, ultracapacitor field have huge application prospect.
Accompanying drawing explanation
Fig. 1 is the TEM transmission electron microscope of the embodiment of the present invention one monoatomic layer TiOx nano sheet colloid solution
Figure.
Fig. 2 is the atomic force microscope figure of the embodiment of the present invention one monoatomic layer TiOx nano sheet colloid solution
Figure is compareed with the size of monoatomic layer TiOx nano sheet.
Detailed description of the invention
In order to make objects, features and advantages of the present invention more clear, below in conjunction with drawings and Examples,
The detailed description of the invention of the present invention is made more detailed description, in the following description, elaborates a lot
Concrete details is so that sufficiently understanding the present invention, but the present invention can be to be much different from its of description
He implements mode.Therefore, the present invention not by following discloses be embodied as limited.
A kind of preparation method of monoatomic layer TiOx nano sheet colloid solution, with titanium source, potassium source, lithium source be
Primitive reaction thing, through high-temperature calcination, ion exchange and intercalation stripping technology, obtains monoatomic layer titanium oxide
Nanometer sheet colloid solution, specifically includes following steps:
1) high-temperature calcination: with titanium source, potassium source, lithium source be primitive reaction thing, mix by a certain percentage through too high
Temperature calcining, naturally cools to room temperature, obtains mixing head product；
2) ion exchange: mixing head product is dispersed in formation dispersion liquid in the middle of hydrochloric acid solution, dispersion liquid is existed
It is aged a period of time under room temperature, collects obtain powder body product by filtration, cleaning, baking step subsequently；
3) intercalation is peeled off: is dispersed in the middle of aqueous solution by powder body product, is subsequently added a certain amount of organic ammonium salt,
Mix homogeneously, shakes a period of time on horizontal shaker, and the monoatomic layer titanium oxide i.e. obtaining stable homogeneous is received
Rice sheet colloid solution.
Wherein, the purity of described monoatomic layer TiOx nano sheet colloid solution is more than 95%, described monoatomic layer
The length of side of TiOx nano sheet is 100-1000nm, thickness is 1.5-1.7nm, wherein titanium elements and oxygen element
Mass ratio is 0.87:1 0.91:1.
Wherein, described titanium source, potassium source, the mixed proportion in lithium source are elemental lithium content, Determination of Potassium, titanium
The mol ratio of constituent content is: 1:(2～10): (5～30).
Wherein, described titanium source is the arbitrary proportion mixture of one or more in industrial oxidation titanium；Described potassium
Source is the one in industrial potassium chloride, potassium nitrate, potassium carbonate, potassium sulfate, potassium phosphate or potassium bromide or several
The arbitrary proportion mixture planted；Described lithium source is industrial chlorinations lithium, lithium nitrate, lithium carbonate, lithium sulfate, phosphorus
The arbitrary proportion mixture of one or more in acid lithium or lithium bromide.
Wherein, described high-temperature calcination comprises the steps:
1) just burn: primitive reaction thing is ground 10-50 minute in mortar, puts in platinum crucible, at 600 DEG C
900 DEG C are placed down in chamber type electric resistance furnace interior calcining 1-5 hour, and heating rate is 10 DEG C/min of 1 DEG C/min, with
After from chamber type electric resistance furnace thorax, directly take out quenching, and grind 10-50 minute in mortar；
2) burn eventually: the first burning product after grinding is put in platinum crucible, is placed at 900 DEG C 1800 DEG C
Calcining 10-72 hour in chamber type electric resistance furnace.
Wherein, the concentration of described hydrochloric acid solution is 0.1mol/L 10mol/L, and the concentration of described dispersion liquid is
1g/L—20g/L；
Wherein, described digestion time is 1-8 days.
Wherein, described filtration, cleaning, drying steps include the following:
1) filter: by the dispersion liquid after ageing, through filtering, obtain aqueous powder body product；
2) clean: mix with one or several the arbitrary proportion in deionized water, dehydrated alcohol or acetone
Bonding solvent cleans above-mentioned aqueous powder body product, until pH value is between 7.0-9.0；
3) it is dried: the aqueous powder body product after cleaning is dried 5-24 hour with 50 DEG C 150 DEG C in an oven,
Obtain the powder body product being dried.
Wherein, the mass percent concentration in the middle of aqueous solution of described organic ammonium salt is 0.1% 5%, described
Organic ammonium salt is Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH or tetrabutylammonium hydrogen
The arbitrary proportion mixture of one or more in amine-oxides.
Wherein, the described time shaken on horizontal shaker is 2 40 days, and concussion speed is 100 300rpm.
Embodiment one
Lithium nitrate, potassium bromide, titanium oxide are mixed with molar ratio 1:4:25, puts in mortar and grind 30 points
Clock, puts in platinum crucible, calcines 1 hour in 900 DEG C are placed down in chamber type electric resistance furnace, and heating rate is 10 DEG C
/ min, directly takes out quenching subsequently from chamber type electric resistance furnace thorax, and grinds 30 minutes in mortar.
First burning product after grinding is put in platinum crucible, calcines in being placed in chamber type electric resistance furnace at 1200 DEG C
40 hours, naturally cool to room temperature.
It is in the middle of 9mol/L hydrochloric acid solution that high-temperature calcinations step products therefrom is dispersed in concentration, dispersion liquid dense
Degree is 20g/L.Dispersion liquid is at room temperature aged 7 days, and changes the hydrochloric acid of same concentrations in each interval of one day
Solution once, filters subsequently, with washes of absolute alcohol, until the pH value of product is 7.0, dries and is contained by gained
Pigment body is dried 5 hours with 140 DEG C in an oven, collects powder body product；
Being dispersed in by powdered product in the middle of aqueous solution, dispersion concentration is 20g/L；It is subsequently added tetramethyl hydroxide
Ammonium (TMAOH), this organic amine salt mass percent concentration in the middle of aqueous solution is 5%, uniformly mixes,
Shaking 30 days on horizontal shaker, concussion speed is 100rpm, i.e. obtains stable homogeneous monoatomic layer titanium oxide and receives
Rice sheet colloid solution, its productivity is 95%.Gained colloid solution is characterized, as follows:
Fig. 1 is the TEM transmission electron microscope picture of monoatomic layer TiOx nano sheet colloid solution of the present invention, can
To find out, the TiOx nano sheet in colloid solution peels off into monolayer lamellar, and TiOx nano sheet thickness is thin,
Monolayer rate is high；
Fig. 2 is the atomic force microscope figure of monoatomic layer TiOx nano sheet colloid solution of the present invention and monatomic
The size comparison figure of layer TiOx nano sheet, show, the TiOx nano sheet length of side is about 500nm, thickness is
1.0-2.0nm, for monoatomic layer thickness.
Embodiment two
Lithium chloride, potassium chloride, titanium oxide are mixed with molar ratio 1:4:10, put in mortar and grind 12 minutes,
Putting in platinum crucible, calcine 5 hours in 650 DEG C are placed down in chamber type electric resistance furnace, heating rate is 2 DEG C/min,
From chamber type electric resistance furnace thorax, directly take out quenching subsequently, and grind 20 minutes in mortar.
First burning product after grinding is put in platinum crucible, calcines in being placed in chamber type electric resistance furnace at 1400 DEG C
20 hours, naturally cool to room temperature.
It is in the middle of 0.5mol/L hydrochloric acid solution that high-temperature calcinations step products therefrom is dispersed in concentration, dispersion liquid
Concentration is 2g/L.Dispersion liquid is at room temperature aged 2 days, and changes the hydrochloric acid of same concentrations in each interval of one day
Solution once, filters subsequently, cleans with deionized water, until the pH value of product is 9.0, dries and is contained by gained
Pigment body is dried 24 hours with 60 DEG C in an oven, collects powder body product.
Being dispersed in by powdered product in the middle of aqueous solution, dispersion concentration is 1g/L；It is subsequently added Tetramethylammonium hydroxide
(TMAOH) and the mixture of tetraethyl ammonium hydroxide 1:1), mixture mass percent in the middle of aqueous solution
Concentration is 0.5%, uniformly mixes, and shakes 5 days on horizontal shaker, and concussion speed is 300rpm, obtains all
One stablizes monoatomic layer TiOx nano sheet colloid solution, and its productivity is 95%, and in colloid solution, monoatomic layer is thin
The sheet titanium oxide length of side is 300nm-1000nm, thickness is 1.0-2.0nm.
Embodiment three
Lithium sulfate, potassium nitrate, titanium oxide are mixed with molar ratio 1:5:10, put in mortar and grind 30 minutes,
Putting in platinum crucible, calcine 1 hour in 900 DEG C are placed down in chamber type electric resistance furnace, heating rate is 10 DEG C
/ min, directly takes out quenching subsequently from chamber type electric resistance furnace thorax, and grinds 30 minutes in mortar.
First burning product after grinding is put in platinum crucible, calcines in being placed in chamber type electric resistance furnace at 1200 DEG C
40 hours, naturally cool to room temperature.
It is in the middle of 9mol/L hydrochloric acid solution that high-temperature calcinations step products therefrom is dispersed in concentration, dispersion liquid dense
Degree is 20g/L.Dispersion liquid is at room temperature aged 7 days, and changes the hydrochloric acid of same concentrations in each interval of one day
Solution once, filters subsequently, with washes of absolute alcohol, until the pH value of product is 7.0, dries and is contained by gained
Pigment body is dried 5 hours with 140 DEG C in an oven, collects powder body product.
Being dispersed in by powdered product in the middle of aqueous solution, dispersion concentration is 20g/L；It is subsequently added (tetramethyl hydrogen-oxygen
Change ammonium (TMAOH) and TBAH (TBAOH) with ratio 2:1 mixture), mixture is at aqueous solution
Central mass percent concentration is 5%, uniformly mixes, and shakes 30 days on horizontal shaker, and concussion speed is
100rpm, obtains stable homogeneous monoatomic layer TiOx nano sheet colloid solution, and its productivity is 96%, colloid
In solution the monoatomic layer flake oxidized titanium length of side be 100nm-700nm, thickness be 1.0-2.0nm.
Embodiment four
Lithium chloride, potassium sulfate, titanium oxide are mixed with molar ratio 1:4:25, puts in mortar and grind 50 points
Clock, puts in platinum crucible, calcines 3 hours in 750 DEG C are placed down in chamber type electric resistance furnace, and heating rate is 5 DEG C
/ min, directly takes out quenching subsequently from chamber type electric resistance furnace thorax, and grinds 40 minutes in mortar.
First burning product after grinding is put in platinum crucible, calcines in being placed in chamber type electric resistance furnace at 1000 DEG C
65 hours, naturally cool to room temperature.
It is that high-temperature calcinations step products therefrom is dispersed in concentration is in the middle of 1mol/L hydrochloric acid solution, dispersion liquid
Concentration is 5g/L.Dispersion liquid is at room temperature aged 5 days, and changes the hydrochloric acid of same concentrations in each interval of one day
Solution once, filters subsequently, and acetone cleans, until the pH value of product is 7.0, dries aqueous for gained powder body
Dry 20 hours with 80 DEG C in an oven, collect powder body product；
Being dispersed in by powdered product in the middle of aqueous solution, dispersion concentration is 10g/L；It is subsequently added tetraethyl hydroxide
Ammonium and TPAOH with ratio 2:1 mixture, mixture mass percent concentration in the middle of aqueous solution
Being 3%, uniformly mix, shaking 10 days on horizontal shaker, concussion speed is 200rpm, obtains stable homogeneous
Monoatomic layer TiOx nano sheet colloid solution, its productivity is 96%, and in colloid solution, monoatomic layer is flake oxidized
The titanium length of side is 200nm-800nm, thickness is 1.0-2.0nm.
Embodiment five
Lithium phosphate, potassium bromide, titanium oxide are closed with molar ratio 1:9:15 mixing, puts into and mortar grinds 12
Minute, to put in platinum crucible, calcine 5 hours in 650 DEG C are placed down in chamber type electric resistance furnace, heating rate is
2 DEG C/min, from chamber type electric resistance furnace thorax, directly take out quenching subsequently, and grind 20 minutes in mortar.
First burning product after grinding is put in platinum crucible, calcines in being placed in chamber type electric resistance furnace at 1400 DEG C
20 hours, naturally cool to room temperature.
It is that high-temperature calcinations step products therefrom is dispersed in concentration is in the middle of 0.5mol/L hydrochloric acid solution, dispersion liquid
Concentration be 2g/L.Dispersion liquid is at room temperature aged 2 days, and changes the salt of same concentrations in each interval of one day
Acid solution once, filters subsequently, cleans with deionized water and ethanol 1:1 mixed solution, until the pH value of product
It is 9.0, dries and aqueous for gained powder body is dried 24 hours with 60 DEG C in an oven, collect powder body product.
Being dispersed in by powdered product in the middle of aqueous solution, dispersion concentration is 1g/L；It is subsequently added TPAOH
(TMAOH), this organic amine salt mass percent concentration in the middle of aqueous solution is 5%, uniformly mixes, at water
Shaking 14 days on yawing bed, concussion speed is 100rpm, i.e. obtains stable monoatomic layer flake oxidized titanium colloid
Solution, in colloid solution the monoatomic layer flake oxidized titanium length of side be 200nm-700nm, thickness be 1.0-2.0nm,
Productivity 97%.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all at this
Any amendment, equivalent and the improvement etc. made within bright spirit and principle, should be included in the present invention
Protection domain within.
Claims (10)
1. the preparation method of a monoatomic layer TiOx nano sheet colloid solution, it is characterized in that, with titanium source, potassium source, lithium source be primitive reaction thing, through high-temperature calcination, ion exchange and intercalation stripping technology, obtain monoatomic layer TiOx nano sheet colloid solution, specifically include following steps:
1) high-temperature calcination: with titanium source, potassium source, lithium source be primitive reaction thing, mix by a certain percentage through high-temperature calcination, naturally cool to room temperature, obtain mixing head product；
2) ion exchange: mixing head product is dispersed in formation dispersion liquid in the middle of hydrochloric acid solution, is at room temperature aged dispersion liquid a period of time, is collected obtained powder body product by filtration, cleaning, baking step subsequently；
3) intercalation is peeled off: be dispersed in the middle of aqueous solution by powder body product, is subsequently added a certain amount of organic ammonium salt, mix homogeneously, shakes a period of time, i.e. obtain the monoatomic layer TiOx nano sheet colloid solution of stable homogeneous on horizontal shaker.
The preparation method of a kind of monoatomic layer TiOx nano sheet colloid solution the most according to claim 1, it is characterized in that, the purity of described monoatomic layer TiOx nano sheet colloid solution is more than 95%, the length of side of described monoatomic layer TiOx nano sheet is 100-1000nm, thickness is 1.5-1.7nm, and wherein the mass ratio of titanium elements and oxygen element is 0.87:1 0.91:1.
The preparation method of a kind of monoatomic layer TiOx nano sheet colloid solution the most according to claim 1, it is characterized in that, described titanium source, potassium source, the mixed proportion in lithium source are that elemental lithium content, Determination of Potassium, the mol ratio of titanium elements content are: 1:(2～10): (5～30).
4. according to the preparation method of a kind of monoatomic layer TiOx nano sheet colloid solution described in claim 1 or 3, it is characterised in that described titanium source is the arbitrary proportion mixture of one or more in industrial oxidation titanium；Described potassium source is the arbitrary proportion mixture of one or more in industrial potassium chloride, potassium nitrate, potassium carbonate, potassium sulfate, potassium phosphate or potassium bromide；Described lithium source is the arbitrary proportion mixture of one or more in industrial chlorinations lithium, lithium nitrate, lithium carbonate, lithium sulfate, lithium phosphate or lithium bromide.
The preparation method of a kind of monoatomic layer TiOx nano sheet colloid solution the most according to claim 1, it is characterised in that described high-temperature calcination comprises the steps:
1) just burn: primitive reaction thing is ground 10-50 minute in mortar, put in platinum crucible, calcine 1-5 hour in 600 DEG C 900 DEG C are placed down in chamber type electric resistance furnace, heating rate is 10 DEG C/min of 1 DEG C/min, from chamber type electric resistance furnace thorax, directly take out quenching subsequently, and grind 10-50 minute in mortar；
2) burn eventually: the first burning product after grinding is put in platinum crucible, calcine 10-72 hour in being placed in chamber type electric resistance furnace at 900 DEG C 1800 DEG C.
The preparation method of a kind of monoatomic layer TiOx nano sheet colloid solution the most according to claim 1, it is characterised in that the concentration of described hydrochloric acid solution is 0.1mol/L 10mol/L, and the concentration of described dispersion liquid is 1g/L 20g/L.
The preparation method of a kind of monoatomic layer TiOx nano sheet colloid solution the most according to claim 1, it is characterised in that described digestion time is 1-8 days, and changes the hydrochloric acid solution of same concentrations in each interval of one day once.
The preparation method of a kind of monoatomic layer TiOx nano sheet colloid solution the most according to claim 1, it is characterised in that described filtration, cleaning, drying steps include the following:
1) filter: by the dispersion liquid after ageing, through filtering, obtain aqueous powder body product；
2) clean: clean above-mentioned aqueous powder body product, until pH value is between 7.0-9.0 with the arbitrary proportion mixed solvent of one or several in deionized water, dehydrated alcohol or acetone；
3) it is dried: the aqueous powder body product after cleaning is dried 5-24 hour with 50 DEG C 150 DEG C in an oven, obtains the powder body product being dried.
The preparation method of a kind of monoatomic layer TiOx nano sheet colloid solution the most according to claim 1, it is characterized in that, the mass percent concentration in the middle of aqueous solution of described organic ammonium salt is 0.1% 5%, and described organic ammonium salt is the arbitrary proportion mixture of one or more in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH or TBAH.
The preparation method of a kind of monoatomic layer TiOx nano sheet colloid solution the most according to claim 1, it is characterised in that the described time shaken on horizontal shaker is 2 40 days, concussion speed is 100 300rpm.
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| CN112079384A (en) * | 2020-09-18 | 2020-12-15 | 武汉理工大学 | Method for ultrasonically stripping oxide nanosheets |
| CN113307306A (en) * | 2021-05-06 | 2021-08-27 | 中广核研究院有限公司 | Composite silica aerogel material and preparation method and application thereof |
| CN113353976A (en) * | 2021-06-11 | 2021-09-07 | 清华-伯克利深圳学院筹备办公室 | Two-dimensional material, preparation and assembly method thereof and application of two-dimensional material in artificial nerve component |
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| CN116081583B (en) * | 2023-02-15 | 2023-09-19 | 浙江大学 | Preparation method of ultrathin titanium nitride nanosheets and ultrathin titanium nitride nanosheets |
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