CN108862266A - A kind of preparation method of stannic oxide/graphene nano material - Google Patents
A kind of preparation method of stannic oxide/graphene nano material Download PDFInfo
- Publication number
- CN108862266A CN108862266A CN201810858330.2A CN201810858330A CN108862266A CN 108862266 A CN108862266 A CN 108862266A CN 201810858330 A CN201810858330 A CN 201810858330A CN 108862266 A CN108862266 A CN 108862266A
- Authority
- CN
- China
- Prior art keywords
- round
- bottomed flask
- preset
- preparation
- nano material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/6303—Inorganic additives
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
Abstract
The invention discloses a kind of preparation methods of stannic oxide/graphene nano material, including：S1, the ultrasonic treatment that GO powder is carried out to the first preset time in deionized water, obtain GO aqueous solution；S2, it takes the GO aqueous solution of the first preset vol to be put into round-bottomed flask, the butanol of the second preset vol is slowly added into round-bottomed flask, stand 10 minutes；S3, nitrogen or carbon dioxide are slowly introducing from round-bottomed flask bottom by quartz ampoule, while carry out the water bath with thermostatic control of the second preset time, stand 2 hours；S4, the lower liquid that third preset vol is sucked out from round-bottomed flask bottom by glass pipette；S5, it persistently rocks round-bottomed flask 5 minutes, the liquid in round-bottomed flask is transferred in beaker.GO two-dimension nano materials surface modification titanic oxide material may be implemented in preparation method provided by the present invention.GO is not susceptible to coagulation phenomenon during modification process, not will form multilayer GO, inhibits the generation of a large amount of titanium dioxide monomer particle.
Description
Technical field
The present invention relates to technical field of nano material, and in particular to a kind of preparation method of stannic oxide/graphene nano material.
Background technique
Excellent mechanical property is basis and the premise that a kind of material carries out engineer application.The brittleness problems of ceramic material are tight
Recasting about its application：Since ceramic material has the polycrystalline structure characteristic of ionic bond or covalent bond, shortage can promote material to deform
Sliding system, make to be easy to produce crackle after ceramic material is loaded, reduce materials'use service life and stability.
Oxide-graphene oxide (GO) of graphene has high-specific surface area, excellent as two-dimentional carbon nanomaterial
Mechanics and tribological property, be one of intensity and the very high material of toughness, while its two-dimensional shape feature makes itself and ceramics
Substrate contact area is big, is conducive to transmitting stress, improves the fracture toughness of ceramics, improves its brittleness speciality.Therefore, GO is toughening pottery
The ideal toughening phase of porcelain composite material.With Al2O3It, generally can be by GO powder and Al for ceramics2O3Powder ball milling is blended, and adds
Heat pressurization is sintered, and prepares the Al of GO toughening2O3Ceramic material.
In Al2O3Though adding GO toughening material in ceramic material plays certain toughening effect, tough compared to the height of GO
Property for, it is this simply in ceramic powder add GO toughening effect it is unsatisfactory.With regard to current GO toughening Al2O3Ceramics
Status plays the strong need of graphite alkenes toughness of material and further researches and develops.
When ceramic post sintering, solid powder is heated to be pressurized, and powder body material is deformed, flowed, and forms ceramic block.But
GO and Al2O3The interface that ceramic matrix is in contact is unlike material, and two kinds of material wellabilities are poor.The mobility of material between them
Difference is easy to leave gas, makes the internal many stomatas of formation after ceramic post sintering；Also, in stress, stress is from Al2O3Ceramic matrix
When being mutually transmitted to GO phase, since two alternate cohesive forces are very weak, it is not easy to transmit stress, the toughness for keeping GO powerful cannot effectively be sent out
It waves, is easy the crack initiation between two-phase interface instead.
On the one hand the fraction of titanic oxide material of GO molecular surface has preferable stickiness and boundary with GO as transition zone
Face bond strength；On the other hand, titanic oxide material and Al2O3Ceramic material has preferable wellability (therefore, titanium dioxide
It is usually used in Al2O3The additive of ceramics), the Al in sintering2O3Molecular mobility is big between ceramics and titanic oxide material, is conducive to row
Gas forms preferable boundary layer.Therefore, GO surface modification titanium dioxide can enhance GO material and Al2O3Between ceramic matrix phase
Wellability, to prepare the better GO toughening Al of toughening effect2O3Ceramic material provides solid foundation.Existing GO adsorption two
The method of titania meterial is chiefly used in the fields such as optics, catalysis.Different from above-mentioned application field, it to be used for GO toughening Al2O3Ceramics
When, there is its special requirement：To be dispersed in GO in ceramic matrix, when modified GO nano material cannot occur for the surface GO
Agglomeration.Art methods have a disadvantage that：
(1) GO is easy to happen coagulation during surface modification processes.Coagulation is a kind of chemical phenomenon, is directed toward in colloid and adds
When entering electrolyte solution, the cation (or anion) of addition has neutralized the charge of colloidal particle institute band, makes colloidal polyurea particle
Integrated larger particles are precipitated in dispersing agent to form precipitating.GO best dispersion solvent is water, after titanium salt is added in water
Titanium ion is set to be adsorbed on the surface GO, oxidation processes obtain GO surface modification titanic oxide material after drying.But above method meeting
Introduce high-valence cationic Ti4+, and GO adsorbs OH- and negatively charged, Ti in water4+Make GO that coagulation occur rapidly in water, is formed macro
Cotton-shaped reunion is seen, ideal nano-grade GO material can not be obtained, be not readily used for toughening Al2O3Ceramics.
(2) GO poor dispersion in other solvents.To avoid GO coagulation problem, some researchs use organic solvent dispersion
GO is re-introduced into the organic salt of titanium, and the most common are TBT --- butyl titanate.TBT occurs hydrolysis and generates titanium ion in the solution
Or titanium hydroxide (Ti (OH)4), it is dried together with GO, heated oxide, forms the mixture of GO and titanium dioxide.But GO is organic
Poor dispersion in solvent is multilayer GO (10 layers or more) even graphite oxide generally there are form.What is formed is titanium dioxide
Only attract by Van der Waals force between titanium modified multilayer GO, multilayer GO.This material is used as toughening phase in ceramics, and when stress is more
It is easy to happen separation, vibration between layer GO, is cracked, ceramic fracture toughness is reduced.
Summary of the invention
In view of the deficiencies in the prior art, the purpose of the present invention is to provide a kind of stannic oxide/graphene nano materials
GO two-dimension nano materials surface modification titanic oxide material may be implemented in preparation method.GO is not easy to send out during modification process
Raw coagulation phenomenon not will form multilayer GO (10 layers or more or even graphite oxide), inhibit a large amount of titanium dioxide monomer particle
It generates.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of stannic oxide/graphene nano material, including：
S1, the ultrasonic treatment that GO powder is carried out to the first preset time in deionized water, obtain GO aqueous solution；
S2, it takes the GO aqueous solution of the first preset vol to be put into round-bottomed flask, slowly adds into the round-bottomed flask
Enter the butanol of the second preset vol, stands 10 minutes；
S3, nitrogen or carbon dioxide are slowly introducing from the round-bottomed flask bottom by quartz ampoule, while it is pre- to carry out second
If the water bath with thermostatic control of time, 2 hours are stood；
S4, the lower liquid that third preset vol is sucked out from the round-bottomed flask bottom by glass pipette；
S5, it persistently rocks the round-bottomed flask 5 minutes, the liquid in the round-bottomed flask is transferred in beaker, stand 5
Minute；
S6, the mixed solution for preparing butyl titanate and dehydrated alcohol；
S7, the mixed solution is slowly dropped into the beaker by glass dropper, while by glass bar described
It is persistently stirred in beaker；
S8, in the beaker substance carry out centrifuge washing, under the first preset temperature to centrifuge washing after it is remaining
The drying process of sediment progress third preset time；
S9, the heat treatment that the powder obtained after drying process is carried out to the 4th preset time under air environment, obtain
Surface modification has the GO nano material of titanium dioxide.
Further, a kind of preparation method of stannic oxide/graphene nano material as described above, in step S1, described first is pre-
If the time is 30 minutes, the content of GO is 0.5-2mg/mL in the GO aqueous solution.
Further, a kind of preparation method of stannic oxide/graphene nano material as described above, in step S2, described first is pre-
If volume is 300-500mL, second preset vol is 200mL, and the capacity of the round-bottomed flask is 1000mL.
Further, a kind of preparation method of stannic oxide/graphene nano material as described above, in step S3, described second is pre-
If the time is 2 hours, the temperature of water bath with thermostatic control is 50-80 DEG C.
Further, a kind of preparation method of stannic oxide/graphene nano material as described above, in step S4, the third is pre-
If volume=first preset vol-V, V 15-45mL.
Further, a kind of preparation method of stannic oxide/graphene nano material as described above, in step S6, the mixing is molten
The volume ratio of butyl titanate and dehydrated alcohol is 1 in liquid:4-1:20, the content of butyl titanate is in the mixed solution
0.2-1.2mg/mL。
Further, a kind of preparation method of stannic oxide/graphene nano material as described above, in step S8, described first is pre-
If temperature is 80 DEG C, the third preset time is 24-48 hours, and the revolving speed of centrifuge washing is 3000-6000r/min.
Further, a kind of preparation method of stannic oxide/graphene nano material as described above, in step S9, the described 4th is pre-
If the time is 30-45 minutes, heating temperature is 120-300 DEG C.
The beneficial effects of the present invention are：GO two-dimension nano materials table may be implemented in preparation method provided by the present invention
Face modified titanic oxide material.GO is not susceptible to coagulation phenomenon during modification process, not will form (10 layers or more of multilayer GO
Even graphite oxide), inhibit the generation of a large amount of titanium dioxide monomer particle.
1, immiscible fourth alcohol and water is mixed, forms the droplet of a large amount of " water+GO " in butanol.Since butanol is slightly soluble in
Water makes water be adsorbed on GO molecular surface, is partially soluble in butanol solution by the amphipathic of GO.General GO is not easy point in alcoholic solution
It dissipates, can be present in alcoholic solution in the form of multilayer GO or graphite oxide, realize single layer or few layer GO in fourth by step S1-S5
Dispersion in alcohol.
2, realize that TBT is slowly hydrolyzed in GO molecular surface.TBT hydrolysis generates titanium dioxide and (is generally Ti in the solution
(OH)4) be it is most widely used prepare nano-titanium dioxide method, but TBT meets water and hydrolyzes rapidly, not easy to stick in aqueous solution
Invest the surface GO.Processing (step (1~4)) through the technical program forms the droplet of a large amount of " water+GO " in butanol.Due to
Butanol is slightly soluble in water, by the amphipathic of GO, so that water is adsorbed on GO molecular surface, is partially soluble in butanol solution.In butanol solution,
The titanium dioxide near GO molecule occurs for hydrone needed for only capable of providing TBT hydrolysis near GO molecule, TBT hydrolysis
Presoma is adhered to GO molecular surface.
Detailed description of the invention
Fig. 1 is a kind of process signal of the preparation method of the stannic oxide/graphene nano material provided in the embodiment of the present invention
Figure.
Fig. 2 is the scanning of the graphene oxide composite material of a small amount of titanium dioxide of surface modification prepared in the embodiment of the present invention
Electron microscope.
Specific embodiment
The present invention is described in further detail with specific embodiment with reference to the accompanying drawings of the specification.
The technical solution one of the prior art
Molecule construction from part --- it is chemically reacted in aqueous solution, titanium salt or aluminium salt is added in GO aqueous solution, generated
Ti4+Ion or Al3+Ion makes GO adsorption Ti4+Ion or Al3+Ion makes the Ti on the surface GO after heat drying4+Ion or
Al3+Ion is contacted with oxygen in air generates titanium dioxide.
The shortcomings that technical solution one：
Titanium salt or aluminium salt are added in GO aqueous solution, Ti can be generated in water4+Ion or Al3+Ion.In GO aqueous solution
High price (being greater than monovalence) metal ion, which is added, can make GO molecule generate coagulation phenomenon.Its principle is：GO molecule is negatively charged in water,
Metal ion is positively charged, and GO molecular surface can adsorb metal ion；One high volence metal ion adsorbs several GO molecules simultaneously,
It is aggregating nearly all GO molecule all by metal ion.Therefore, technical solution one is easy to cause GO nano material to form group
It is poly-, it cannot disperse well, and then powder to be sintered cannot be uniformly mixed into ceramic particle.Such powder sintering at
Ceramic material, micro components are unevenly distributed, and GO aggregation is easy to produce crackle, reduces ceramic fracture toughness.
The technical solution two of the prior art
Butyl titanate (TBT) is added in organic solvent, mix with GO, slowly plus water, titanium is adsorbed on GO and divides after TBT hydrolysis
Sublist face.
The shortcomings that technical solution two：
GO is not easy to disperse in organic solvent, generally generates multilayer GO (more than 10 layers), or even close to the thickness of graphite oxide
Degree.That formed is titania modified multilayer GO, is only attracted by Van der Waals force between multilayer GO.This material is made in ceramics
For toughening phase, separation, vibration are easy to happen between multilayer GO when stress, cracks, reduces ceramic fracture toughness.
For above-mentioned disadvantage of the existing technology, the embodiment of the invention provides a kind of stannic oxide/graphene nano materials
GO two-dimension nano materials surface modification titanic oxide material may be implemented in preparation method.GO is not easy to send out during modification process
Raw coagulation phenomenon not will form multilayer GO (10 layers or more or even graphite oxide), inhibit a large amount of titanium dioxide monomer particle
It generates.Specific technical solution is as follows：
As shown in Figure 1, a kind of preparation method of stannic oxide/graphene nano material, including：
S1, the ultrasonic treatment that GO powder is carried out to the first preset time in deionized water, obtain GO aqueous solution；
S2, it takes the GO aqueous solution of the first preset vol to be put into round-bottomed flask, it is pre- that second is slowly added into round-bottomed flask
If the butanol of volume, 10 minutes are stood；
S3, nitrogen or carbon dioxide are slowly introducing from round-bottomed flask bottom by quartz ampoule, at the same carry out second it is default when
Between water bath with thermostatic control, stand 2 hours；
S4, the lower liquid that third preset vol is sucked out from round-bottomed flask bottom by glass pipette；
S5, it persistently rocks round-bottomed flask 5 minutes, the liquid in round-bottomed flask is transferred in beaker, stand 5 minutes；
S6, the mixed solution for preparing butyl titanate and dehydrated alcohol；
S7, mixed solution is slowly dropped into beaker by glass dropper, while is persistently stirred in beaker by glass bar
It mixes；
S8, centrifuge washing is carried out to the substance in beaker, under the first preset temperature to centrifuge washing after remaining precipitating
The drying process of object progress third preset time；
S9, the heat treatment that the powder obtained after drying process is carried out to the 4th preset time under air environment, obtain
Surface modification has the GO nano material of titanium dioxide.
In step S1, the first preset time is 30 minutes, and the content of GO is 0.5-2mg/mL in GO aqueous solution.
In step S2, the first preset vol is 300-500mL, and the second preset vol is 200mL, and the capacity of round-bottomed flask is
1000mL。
In step S3, the second preset time is 2 hours, and the temperature of water bath with thermostatic control is 50-80 DEG C.
In step S4, third preset vol=the first preset vol-V, V 15-45mL.
In step S6, the volume ratio of butyl titanate and dehydrated alcohol is 1 in mixed solution:4-1:20, in mixed solution
The content of butyl titanate is 0.2-1.2mg/mL.
In step S8, the first preset temperature is 80 DEG C, and third preset time is 24-48 hours, and the revolving speed of centrifuge washing is
3000-6000r/min。
In step S9, the 4th preset time is 30-45 minutes, and heating temperature is 120-300 DEG C.
Embodiment one
(1) by GO powder, 30 minutes (ultrasonic power 180W) of ultrasound, preparation GO aqueous solution, GO content are in deionized water
0.5-2mg/mL (in this content range, GO can be water-soluble fully dispersed, and there is no multilayer GO or graphite oxides).
(2) above-mentioned GO aqueous solution, volume V1=300-500mL are taken, deposit capacity is to delay in the round-bottomed flask of 1000mL
It is slow that butanol 200mL is added, stand 10 minutes.In this flask, butanol is not soluble in water, can be in solution upper layer；At GO aqueous solution
In lower layer, and the half of the GO aqueous solution volume nearly molten product of flask, the area of both GO solution and butanol layering interfaces are larger.
(3) nitrogen or carbon dioxide are slowly introducing from drag by quartz ampoule, while carry out 50-80 DEG C of thermostatted water
Bath, time are 2 hours.Later, 2 hours are stood.Purpose is that GO molecule in GO aqueous solution is precipitate into layering circle of fourth alcohol and water
Near face.
(4) lower liquid is sucked out from round bottom beaker bottom with glass pipette, sucking liquid volume V is altogether：V=(V1-
15mL)-(V1-45mL)。
(5) it rocks repeatedly round-bottomed flask 5 minutes.Later, liquid is moved in beaker, stands 5 minutes.
(6) mixed solution of TBT and dehydrated alcohol are prepared, the two volume ratio is 1:4-1:20, TBT content is in solution
0.2mL-1.2mL, about 0.2-1.2mg are close with GO mass.
(7) solution in step (6) is slowly dropped into the beaker of step (5) with glass dropper, while is being burnt with glass bar
The lasting stirring of cup.
(8) material in the cup will be burnt through 3000-6000r/min centrifuge washing, 80 DEG C of drying process are carried out to remaining sediment,
Continue 24-48 hours.
(9) 120-300 DEG C will be heated under gained powder air environment, continue 30-45 minutes.Obtain surface modification a small amount of two
The GO material of titanium oxide, microcosmic scanning electron microscope (SEM) photograph are as shown in Figure 2.
It realizes that GO molecule is in the precipitation of aqueous solution upper layer in GO aqueous solution by step (3), then is discharged and is in by step (4)
The water of lower layer only remains 30mL water, and at this moment GO molecule is near the layering face of aqueous solution and butanol.Although butanol is insoluble in water,
But it according to the amphipathic of GO molecule, is rocked repeatedly, the droplet that part GO can wrap up dampening is mixed into be formed in butanol solution and suspend
Liquid.The state of GO material is still single layer or few layer at this time, therefore GO is also single layer in the titania modified GO material generated
Or few layer.TBT dissolves in butanol, then TBT is instilled into butanol suspension through step (6), and TBT meets the water of GO package in butanol
Hydrolysis occurs for drop, generates the presoma Ti (OH) of titanium dioxide in GO molecular surfacex, because water content is very in butanol
Few, only GO surrounding molecules have hydrone, therefore TBT hydrolysis can only occur in GO surrounding molecules, and be attached on GO molecule, water
Molecule is seldom, and has the inhibiting effect of ethyl alcohol and butanol, the Ti (OH) of generationxVery slowly, big titanium dioxide not easily generated
Particle monomer or Ti (OH)4Monomer, i.e. realization overwhelming majority Ti (OH)xIt is attached to GO molecular surface, dries and removes moisture and fourth
After alcohol, ethanol impurity, under high temperature heating conditions, Ti (OH)xTitanium dioxide (TiO can be transformed into2)。
Hydrone is present in butanol with the state of a large amount of droplets, and overall content is seldom, leans on the amphipathic holding water of GO molecule
Stability of the droplet in butanol, the connection between droplet has been isolated in a large amount of butanol molecules, after TBT hydrolysis, GO molecular surface
Though there is high price titanium Ti4+Ion, but due to the buffer action of butanol, GO molecule cannot mutually contact；Also, as more TBT exist
GO surface hydrolysis, the more Ti of GO adsorption (OH)x, prevent the intermolecular contact of GO.Therefore, it is existing to be not susceptible to coagulation by GO
As.
Key Term used herein is defined as follows：
Toughening --- increase the fracture toughness of ceramic matrix.
A kind of ball milling --- technique of common mixed powder particle.
Fracture toughness --- a kind of characteristic of the resistance to fracture energy of fragile material is measured, fracture toughness is bigger, and material is not allowed more
Brittle failure easily occurs.
It is modified --- by improving the surface characteristic of GO in GO surface modification titanium dioxide, make itself and Al2O3 ceramic matrix
Between wellability increase.
Improving wellability --- when ceramic post sintering, solid powder is heated to be pressurized, and powder body material is deformed, flowed, and is formed
Ceramic block.But GO and Al2O3The interface that ceramic matrix is in contact be unlike material, the poor fluidity of material between them,
It is easy to leave gas, makes the internal many stomatas of formation after ceramic post sintering --- i.e.：Two kinds of material wellabilities are poor.GO surface modification two
After titanium oxide, with Al2O3Between wellability be much improved.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technology
Within, then the present invention is also intended to include these modifications and variations.
Claims (8)
1. a kind of preparation method of stannic oxide/graphene nano material, which is characterized in that including：
S1, the ultrasonic treatment that GO powder is carried out to the first preset time in deionized water, obtain GO aqueous solution；
S2, it takes the GO aqueous solution of the first preset vol to be put into round-bottomed flask, is slowly added into the round-bottomed flask
The butanol of two preset vols stands 10 minutes；
S3, nitrogen or carbon dioxide are slowly introducing from the round-bottomed flask bottom by quartz ampoule, at the same carry out second it is default when
Between water bath with thermostatic control, stand 2 hours；
S4, the lower liquid that third preset vol is sucked out from the round-bottomed flask bottom by glass pipette；
S5, it persistently rocks the round-bottomed flask 5 minutes, the liquid in the round-bottomed flask is transferred in beaker, stand 5 points
Clock；
S6, the mixed solution for preparing butyl titanate and dehydrated alcohol；
S7, the mixed solution is slowly dropped into the beaker by glass dropper, while by glass bar in the beaker
Interior lasting stirring；
S8, centrifuge washing is carried out to the substance in the beaker, under the first preset temperature to centrifuge washing after remaining precipitating
The drying process of object progress third preset time；
S9, the heat treatment that the powder obtained after drying process is carried out to the 4th preset time under air environment, obtain surface
It is modified with the GO nano material of titanium dioxide.
2. a kind of preparation method of stannic oxide/graphene nano material according to claim 1, which is characterized in that step S1
In, first preset time is 30 minutes, and the content of GO is 0.5-2mg/mL in the GO aqueous solution.
3. a kind of preparation method of stannic oxide/graphene nano material according to claim 2, which is characterized in that step S2
In, first preset vol is 300-500mL, and second preset vol is 200mL, and the capacity of the round-bottomed flask is
1000mL。
4. a kind of preparation method of stannic oxide/graphene nano material according to claim 3, which is characterized in that step S3
In, second preset time is 2 hours, and the temperature of water bath with thermostatic control is 50-80 DEG C.
5. a kind of preparation method of stannic oxide/graphene nano material according to claim 4, which is characterized in that step S4
In, the third preset vol=first preset vol-V, V 15-45mL.
6. a kind of preparation method of stannic oxide/graphene nano material according to claim 5, which is characterized in that step S6
In, the volume ratio of butyl titanate and dehydrated alcohol is 1 in the mixed solution:4-1:20, metatitanic acid four in the mixed solution
The content of butyl ester is 0.2-1.2mg/mL.
7. a kind of preparation method of stannic oxide/graphene nano material according to claim 6, which is characterized in that step S8
In, first preset temperature is 80 DEG C, and the third preset time is 24-48 hours, and the revolving speed of centrifuge washing is 3000-
6000r/min。
8. a kind of preparation method of stannic oxide/graphene nano material according to claim 7, which is characterized in that step S9
In, the 4th preset time is 30-45 minutes, and heating temperature is 120-300 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810858330.2A CN108862266B (en) | 2018-07-31 | 2018-07-31 | Preparation method of graphene oxide nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810858330.2A CN108862266B (en) | 2018-07-31 | 2018-07-31 | Preparation method of graphene oxide nano material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108862266A true CN108862266A (en) | 2018-11-23 |
| CN108862266B CN108862266B (en) | 2021-11-26 |
Family
ID=64306437
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810858330.2A Active CN108862266B (en) | 2018-07-31 | 2018-07-31 | Preparation method of graphene oxide nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108862266B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110681860A (en) * | 2019-09-09 | 2020-01-14 | 厦门大学 | Graphene oxide coated metal composite nano with Raman signal and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102553560A (en) * | 2012-01-12 | 2012-07-11 | 哈尔滨工业大学 | Preparation method of titanium dioxide/graphene composite photocatalyst |
| CN103337611A (en) * | 2013-07-10 | 2013-10-02 | 厦门大学 | Preparation method of graphene-titanium dioxide composite material |
| CN105688809A (en) * | 2016-01-26 | 2016-06-22 | 西南科技大学 | Preparing method for graphene oxide/titanium dioxide nanometer tube composite material |
| KR20170139953A (en) * | 2016-06-10 | 2017-12-20 | 포항공과대학교 산학협력단 | Titanium dioxide photoelectrode and method for preparing the same |
| CN108178186A (en) * | 2017-12-01 | 2018-06-19 | 中国科学院上海高等研究院 | A kind of titanium dioxide of size tunable and the preparation method of graphene oxide compound |
-
2018
- 2018-07-31 CN CN201810858330.2A patent/CN108862266B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102553560A (en) * | 2012-01-12 | 2012-07-11 | 哈尔滨工业大学 | Preparation method of titanium dioxide/graphene composite photocatalyst |
| CN103337611A (en) * | 2013-07-10 | 2013-10-02 | 厦门大学 | Preparation method of graphene-titanium dioxide composite material |
| CN105688809A (en) * | 2016-01-26 | 2016-06-22 | 西南科技大学 | Preparing method for graphene oxide/titanium dioxide nanometer tube composite material |
| KR20170139953A (en) * | 2016-06-10 | 2017-12-20 | 포항공과대학교 산학협력단 | Titanium dioxide photoelectrode and method for preparing the same |
| CN108178186A (en) * | 2017-12-01 | 2018-06-19 | 中国科学院上海高等研究院 | A kind of titanium dioxide of size tunable and the preparation method of graphene oxide compound |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110681860A (en) * | 2019-09-09 | 2020-01-14 | 厦门大学 | Graphene oxide coated metal composite nano with Raman signal and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108862266B (en) | 2021-11-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105796478B (en) | Assembled by nano-colloid particle, high intensity, selfreparing, injectable composite colloid gel rubber material and its preparation method and application | |
| CN101601986A (en) | A kind of method for making of chitosan-silicon dioxide compound hollow microballoon and application | |
| CN106041112B (en) | A kind of freeze drying process of preparing same of dispersion-strengtherning tungsten powder | |
| CN102923770B (en) | Preparation method of yttrium-stabilized nanometer zirconium dioxide powder | |
| Shi et al. | Preparation and enzymatic application of flower-like hybrid microcapsules through a biomimetic mineralization approach | |
| CN107986777B (en) | Zirconia ceramic matrix composite and preparation method thereof | |
| Kumari et al. | Zirconia-based nanomaterials: recent developments in synthesis and applications | |
| CN109909497A (en) | Powder surface treating agent, titanium or titanium alloy powder ejection forming method and product | |
| CN112190697A (en) | High-phycocyanin-loaded nanoparticle and preparation method and application thereof | |
| CN105709736B (en) | A kind of mosaic Pt@CeO2The preparation method of nano-tube composite catalyst | |
| Chen et al. | Preparation of ZrO2 microspheres by spray granulation | |
| CN108862266A (en) | A kind of preparation method of stannic oxide/graphene nano material | |
| CN1321066C (en) | Zirconium dioxide nano powder material preparation method | |
| CN109865833A (en) | The method for preparing powder metallurgy of titanium or titanium alloy product, titanium or titanium alloy product | |
| CN112773945B (en) | Method for preparing ceramic-magnetofluid composite bracket | |
| CN109971982A (en) | The preparation method and product of in-situ authigenic ceramic phase enhancing titanium composite material | |
| CN107352807B (en) | Preparation method of spherical bioactive glass | |
| CN1587062A (en) | Nano structure yttrium stabilized zirconium oxide aggregated powder and its producing method | |
| CN105969758B (en) | Immobilised enzymes, magnetic carbon material and preparation method thereof | |
| CN104485191A (en) | Magnetic hollow nanometer ball and preparation method thereof | |
| CN115368122B (en) | Modified diatomite porous ceramic slurry and ceramic powder | |
| Tajiri et al. | Manufacturing and characterization of porous ceramic capillary membranes for enzyme functionalization through click chemistry | |
| CN108609627A (en) | A kind of preparation method and applications of the nano silicon dioxide of coralliform network structure | |
| CN1762901A (en) | Nanostructured yttrium stable zirconium oxide agglomerate type powder and its production method | |
| CN114873640A (en) | Method for preparing fibrous zirconium dioxide aerogel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |