CN106927683A - Wet chemistry method builds the preparation method of controllable nano crystal glass ceramics - Google Patents
Wet chemistry method builds the preparation method of controllable nano crystal glass ceramics Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/16—Halogen containing crystalline phase
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Abstract
The present invention proposes that a kind of wet chemistry method builds the preparation method of controllable nano crystal glass ceramics, it is characterised in that comprise the following steps：(1) it is nanocrystalline using hot injection method synthesis different size；(2) sol-gal process synthetic glass matrix is used；(3) the Na20-B203-Si02 glass colloidal sol obtained by the nanocrystalline and step (2) obtained by step (1) or silicon dioxide gel fusion are bonded together to form into homogeneous, transparent nanocrystalline glass ceramics.Mesh of the invention is to provide a kind of preparation method for realizing controllable nano crystal glass ceramics, the nano particle controllable by synthesizing size, then the serial controllable nano crystal glass ceramics that have embodied tunable characteristic are formed in optical property in glass matrix, and this characteristic is significant in the basic research of optoelectronic areas and application for this kind of material.
Description
Technical field
Controllable nano crystalline substance is built the present invention relates to the preparation method of nanocrystalline glass ceramics, more particularly to a kind of wet chemistry method
The preparation method of glass ceramics with obtain different series, different size be distributed nanocrystalline glass ceramics.
Background technology
Glass ceramics (glass-ceramics), refers to the shape by way of controlling glass crystallization also known as devitrified glass
Into a kind of composite that is combined with glass of crystalline phase.Due to its superior performance, glass ceramics has become material science
One of development material of field emphasis and focus.In particular with manufacturing technology, the hair of nanometer technology, and modern analytical technique
Exhibition, the crystal with nanoscale is incorporated into the nanocrystalline glass ceramics (nano-glass- formed after glass system
Ceramics the performance of more desirable) is often shown.These nanocrystalline introducings can not only improve glass material sheet
The mechanical mechanics property of body, and can assign glass material more novel characteristics.Such as show good nonlinear optics
Property, causes special light transmission, produces ion transport and relaxation phenomena higher etc..That is, nanometer crystal glass is made pottery
Porcelain can not only embody two kinds of components of different shape in a kind of material, and this nanocrystalline covalent and glass between
Combination can play a part of to change glass property, and this undoubtedly pushes nanocrystalline glass ceramics to one and more significantly grinds
Study carefully position, now have become an important branch in Inorganic Non-metallic Materials research field and cause the extensive pass of scholars
Note.
Therefore many scholars are attracted to study the synthesis of nanocrystalline glass ceramics, and efficiently control it is nanocrystalline in glass
The target even more pursued always of growth.Because nanocrystalline Size Distribution and pattern knot in glass cannot be efficiently controlled
Structure, can cause the defect or unstable on this kind of material property so that the practical application of this kind of material is very limited.Than
Such as, obtain a kind of nanocrystalline glass ceramics with high light quality and generally require and possess two kinds of conditions：First, it is nanocrystalline
Size in glass is very small (generally in 10-50nm), more preferably less than the wavelength of visible ray, and Size Distribution is narrower；Second, receive
The refractive index of meter Jing and glass two-phase is tried one's best relatively, and this will often be realized by controlling nanocrystalline size.It can be seen that receiving
Meter Jing controllable growths in glass have become a unavoidable problem in science, are also that current nanocrystalline glass ceramics is ground
Such issues that bottleneck problem during studying carefully, solution, all has higher for this kind of material in basic research and application field
Art meaning and vast potential for future development.
The content of the invention
Based on above mentioned problem, present invention aim at a kind of preparation method for realizing controllable nano crystal glass ceramics of offer,
The nano particle controllable by synthesizing size, is then formed in optical property in glass matrix and has embodied tunable characteristic
Serial controllable nano crystal glass ceramics, this characteristic for this kind of material the basic research of optoelectronic areas and application tool
It is significant.
For problem above, there is provided following technical scheme：Wet chemistry method builds the preparation of controllable nano crystal glass ceramics
Method, it is characterised in that comprise the following steps：
(1) synthesis different size is nanocrystalline：Using stearic acid or oleic-acid as nanocrystalline precursor, injected using heat
Method obtains different size distribution and dispersiveness is preferably nanocrystalline；
(2) synthetic glass matrix：Sodium boron silicon-based glass colloidal sol or silicon dioxide gel conduct are synthesized using sol-gel process
Glass basis；
(3) nanocrystalline glass ceramics is bonded together to form：By the sodium borosilicate obtained by the nanocrystalline and step (2) obtained by step (1)
Glass colloidal sol or silicon dioxide gel are merged and are fitted into container, are placed on dry shady place at least seven days, are formed it into wet
Gel, is then put into vacuum oven by wet gel, obtains the xerogel of bulk, and xerogel is placed on into atmosphere sintering furnace
In, oxygen atmosphere is passed through between 25~450 DEG C, hydrogen is passed through at 450 ± 20 DEG C and 9-11 hour, Ran Hou is incubated
450 DEG C~600 DEG C are passed through H2Or/and H2S or/and O2, that is, form homogeneous, transparent nanocrystalline glass ceramics.
The present invention is further arranged to, in the step (1) it is nanocrystalline be doped to proportion in glass basis be 1%~
1.5%.
The present invention is further arranged to, and xerogel sintering obtains nanocrystalline glass ceramics for oxidation is produced in the step (3)
Thing, then 450 DEG C~600 DEG C are passed through O2, obtain nanocrystalline glass ceramics for reduzate, then 450 DEG C~600 DEG C are passed through H2, obtain
It is sulfur product to nanocrystalline glass ceramics, then 450 DEG C~600 DEG C are passed through H2S.
The present invention is further arranged to, the nanocrystalline use CsPbX3, X is halogen, and the glass basis is used
Sodium boron silicon-based glass colloidal sol, synthesizes CsPbX3Nanocrystalline glass ceramics is comprised the following steps：
(1) various sizes of CsPbX3The synthesis of nano-particle
1. the synthesis of oleic acid caesium：CsCO3Octadecylene (ODE) and oleic acid (OA) are added, dry 1 at 110~130 DEG C~
1.2h, then in N2150~160 DEG C are heated under atmosphere, go directly CsCO3It is complete with OA reactions；
②CsPbX3Synthesis：By ODE and PbX21~1.2h is dried under 110~130 DEG C of vacuum, in N2Add under atmosphere
Enter dry oleic acid (OA) and oleyl amine (OLA), until PbX2After dissolving, 140 DEG C -200 DEG C are warming up to, change the CsPbX of synthesis3
Receive the size of art particle, be then rapidly injected the oleic acid caesium of 1. middle synthesis, be put into after 5s or so in ice-water bath and reacted；
3. by the CsPbX of 2. middle synthesis3Centrifugation, during the particle after centrifugation is distributed into toluene or n-hexane, storage is standby
With；
(2) synthesis of glass basis
1. under strong stirring, tetraethyl orthosilicate (TEOS) is dropwise instilled by absolute ethyl alcohol (EtOH), deionized water
(H2) and 2M nitric acid (HNO O3) composition mixed solution quickly stirred, be fully hydrolyzed, solution present water white transparency without cotton-shaped
Precipitation；
2. by H3BO3It is dissolved in EGME and is thermally formed the precursor solution of the clarification containing B；Na and absolute ethyl alcohol
Reaction precursor solution --- caustic alcohol of the generation containing Na ions；
3. by step 2. in slowly instill the step of being fully hydrolyzed respectively in order containing the precursor solution of B and Na ions
1. in the mixed solution in and it is stirred vigorously, successively stirring can obtain Na20-B203-Si02 glass colloidal sol；
(3) nanocrystalline being bonded with glass basis
After the standby various sizes of nano-particle of storage in (1) is merged with the glass basis of synthesis in (2), it is placed on dry
Dry shady place at least seven days, forms it into wet gel, and this wet gel is put into vacuum oven, obtains the dry solidifying of bulk
, then be placed on xerogel in atmosphere sintering furnace by glue, and oxygen atmosphere is led between 25~450 DEG C, and hydrogen is passed through at 450 DEG C simultaneously
10 hours of insulation, then continue to be passed through H at 450 DEG C~600 DEG C2, form homogeneous, transparent CsPbX3Nanocrystalline glass ceramics.
The present invention is further arranged to, and the composition of each group component mole fraction of the sodium boron silicon-based glass colloidal sol is：R
(Na2O/SiO2)=0.1 ± 0.01, R (B2O3/SiO2)=0.3 ± 0.04.
The present invention is further arranged to, nanocrystalline nanocrystalline including metal or salt compounds in the step (1).
The present invention is further arranged to, the nanocrystalline use metal, sulfide or nitride-based hot injection method synthesis,
Correspondence introduces reduction, vulcanization or ammonification atmosphere and realizes nanocrystalline effective growth.
The present invention has the advantages that following several respects compared with prior art：
(1) the nanocrystalline glass ceramics block material of controlled dimensions can be synthesized with reference to sol-gel process by heat injection
Material.
(2) the controllable serial nano crystal glass ceramics of the technical program synthesis have embodied tunable spy in optical property
Property, this characteristic is significant in the basic research of optoelectronic areas and application for this kind of material.
(3) method of heat injection combination sol-gel has versatility in the controllable serial nano crystal glass ceramics of synthesis.
Specific embodiment
With reference to embodiment, specific embodiment of the invention is described in further detail.Following examples are used for
The present invention is illustrated, but is not limited to the scope of the present invention.
Embodiment 1：
The nanocrystalline use CsPbX3, X is halogen, and the glass basis uses sodium boron silicon-based glass colloidal sol, is closed
Into CsPbX3Nanocrystalline glass ceramics is comprised the following steps：
1. various sizes of CsPbX3The synthesis of nano-particle
1. the synthesis of oleic acid caesium
First by the CsCO of 0.6-1.2g3It is added in the there-necked flask of 100ml, adds octadecylene (ODE) and oleic acid
(OA) 1h, is dried at 120 DEG C, then in N2150 DEG C are heated under atmosphere, go directly CsCO3It is complete with OA reactions.
②CsPbX3Synthesis
By the PbX of ODE and 0.188mmol2Or their mixture is added in the there-necked flask of 25ml, at 120 DEG C
Vacuum under dry 1h, in N2Dry oleic acid (OA) and oleyl amine (OLA) are added under atmosphere.When PbX2After salt dissolving, it is warming up to
140 DEG C -200 DEG C, change the CsPbX of synthesis3The size of nano-particle, then again by the oleic acid caesium of 1. middle synthesis
(0.125mol) is rapidly injected, and there-necked flask is put into ice-water bath after 5s is reacted.
For CsPbCl3Need temperature and tri octyl phosphine (TOP) dissolving PbCl higher2。
3. by the CsPbX of 2. middle synthesis3Centrifugation, during the particle after centrifugation is distributed into toluene or n-hexane, storage is standby
With.
2. the synthesis of glass basis
1. under strong stirring, tetraethyl orthosilicate (TEOS) is dropwise instilled by absolute ethyl alcohol (EtOH), deionized water
(H2) and 2M nitric acid (HNO O3) composition mixed solution quickly stirred, be fully hydrolyzed, solution present water white transparency without cotton-shaped
Precipitation；
2. by H3BO3It is dissolved in EGME and is thermally formed the precursor solution of the clarification containing B；Na and absolute ethyl alcohol
Reaction precursor solution (caustic alcohol) of the generation containing Na ions；
3. by step 2. in slowly instill the step of being fully hydrolyzed respectively in order containing the precursor solution of B and Na ions
1. in the mixed solution in and it is stirred vigorously, successively stirring can obtain Na20-B203-Si02 glass colloidal sol.
3. nanocrystalline being bonded with glass basis
Standby various sizes of nano-particle will be stored in above-mentioned steps 1 and is merged with the glass basis synthesized in step 2
Afterwards, it is placed on dry shady place at least seven days, forms it into wet gel, this wet gel is put into vacuum oven, obtains
, then be placed on xerogel in atmosphere sintering furnace by block xerogel, i.e., lead to oxygen atmosphere between 25~450 DEG C, at 450 DEG C
Left and right is passed through hydrogen and 10 hours of soaking time, then continues to be passed through H at 450 DEG C~600 DEG C2, you can form homogeneous, it is transparent
CsPbX3Nanocrystalline glass ceramics.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, on the premise of the technology of the present invention principle is not departed from, some improvement and modification can also be made, above-mentioned hypothesis these
Improve and modification also should be regarded as protection scope of the present invention.
Claims (7)
1. wet chemistry method builds the preparation method of controllable nano crystal glass ceramics, it is characterised in that comprise the following steps：
(1) synthesize various sizes of nanocrystalline：Using stearic acid or oleic-acid as nanocrystalline precursor, using hot injection method
Obtain different size distribution and dispersiveness is preferably nanocrystalline；
(2) synthetic glass matrix：Sodium boron silicon-based glass colloidal sol or silicon dioxide gel are synthesized as glass using sol-gel process
Matrix；
(3) nanocrystalline glass ceramics is bonded together to form：By the Na20-B203-Si02 glass obtained by the nanocrystalline and step (2) obtained by step (1)
Colloidal sol or silicon dioxide gel are merged and are fitted into container, are placed on dry shady place at least seven days, form it into wet gel,
Then wet gel is put into vacuum oven, obtains the xerogel of bulk, and xerogel is placed in atmosphere sintering furnace,
Oxygen atmosphere is passed through between 25~450 DEG C, hydrogen and 9-11 hour of soaking time is passed through at 450 ± 20 DEG C, then 450
DEG C~600 DEG C be passed through H2Or H2S or O2, that is, form homogeneous, transparent nanocrystalline glass ceramics.
2. wet chemistry method according to claim 1 builds the preparation method of controllable nano crystal glass ceramics, it is characterised in that：
It is nanocrystalline in the step (1) that to be doped to proportion in glass basis be 1%~1.5%.
3. wet chemistry method according to claim 1 and 2 builds the preparation method of controllable nano crystal glass ceramics, and its feature exists
In：Xerogel sintering obtains nanocrystalline glass ceramics for oxidation product in the step (3), then 450 DEG C~600 DEG C are passed through O2,
Nanocrystalline glass ceramics is obtained for reduzate, then 450 DEG C~600 DEG C are passed through H2, nanocrystalline glass ceramics is obtained for vulcanization is produced
Thing, then 450 DEG C~600 DEG C are passed through H2S。
4. wet chemistry method according to claim 2 builds the preparation method of controllable nano crystal glass ceramics, it is characterised in that：
The nanocrystalline use CsPbX3, X is halogen, and the glass basis uses sodium boron silicon-based glass colloidal sol, synthesizes CsPbX3Receive
Rice crystal glass ceramics are comprised the following steps：
(1) various sizes of CsPbX3The synthesis of nano-particle
1. the synthesis of oleic acid caesium：CsCO3Octadecylene (ODE) and oleic acid (OA) are added, 1~1.2h is dried at 110~130 DEG C, so
Afterwards in N2150~160 DEG C are heated under atmosphere, go directly CsCO3It is complete with OA reactions；
②CsPbX3Synthesis：By ODE and PbX21~1.2h is dried under 110~130 DEG C of vacuum, in N2Added under atmosphere dry
Dry oleic acid (OA) and oleyl amine (OLA), until PbX2After dissolving, 140 DEG C -200 DEG C are warming up to, change the CsPbX of synthesis3Nanometer
, then be rapidly injected for the oleic acid caesium of 1. middle synthesis by the size of particle, and reaction in ice-water bath is put into after 5s or so；
3. by the CsPbX of 2. middle synthesis3Centrifugation, during the particle after centrifugation is distributed into toluene or n-hexane, storage is standby；
(2) synthesis of glass basis
1. under strong stirring, tetraethyl orthosilicate (TEOS) is dropwise instilled by absolute ethyl alcohol (EtOH), deionized water (H2O) and
2M nitric acid (HNO3) composition mixed solution quickly stirred, be fully hydrolyzed, solution present water white transparency without flocculent deposit；
2. by H3BO3It is dissolved in EGME and is thermally formed the precursor solution of the clarification containing B；Na reacts with absolute ethyl alcohol
Precursor solution --- caustic alcohol of the generation containing Na ions；
3. by step 2. in the precursor solution containing B and Na ions slowly instill the step of being fully hydrolyzed respectively in order 1.
Mixed solution in and be stirred vigorously, successively stirring can obtain Na20-B203-Si02 glass colloidal sol；
(3) nanocrystalline being bonded with glass basis
After the standby various sizes of nano-particle of storage in (1) is merged with the glass basis of synthesis in (2), it is placed on dry
Shady place at least seven days, forms it into wet gel, and this wet gel is put into vacuum oven, obtains the xerogel of bulk,
Then xerogel is placed in atmosphere sintering furnace, oxygen atmosphere is led between 25~450 DEG C, hydrogen is passed through at 450 DEG C and is protected
Warm 10 hours, then continue to be passed through H at 450 DEG C~600 DEG C2, form homogeneous, transparent CsPbX3Nanocrystalline glass ceramics.
5. wet chemistry method according to claim 4 builds the preparation method of controllable nano crystal glass ceramics, it is characterised in that：
The composition of each group component mole fraction of the sodium boron silicon-based glass colloidal sol is：R(Na2O/SiO2)=0.1 ± 0.01, R (B2O3/
SiO2)=0.3 ± 0.04.
6. wet chemistry method according to claim 1 builds the preparation method of controllable nano crystal glass ceramics, it is characterised in that：
It is nanocrystalline nanocrystalline including metal or salt compounds in the step (1).
7. wet chemistry method according to claim 1 builds the preparation method of controllable nano crystal glass ceramics, it is characterised in that：
The nanocrystalline use metal, sulfide or nitride-based hot injection method synthesis, correspondence introduce reduction, vulcanization or ammonification gas
Atmosphere realizes nanocrystalline effective growth.
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| CN107934916A (en) * | 2017-11-16 | 2018-04-20 | 中山大学 | It is a kind of to stablize the nanocrystalline preparation methods of unleaded full-inorganic double-perovskite A2BB ' X6 |
| CN108424001A (en) * | 2018-04-04 | 2018-08-21 | 武汉理工大学 | A kind of CsPbX3Nanocrystalline doping boron-containing glass and preparation method thereof |
| CN108947242A (en) * | 2018-08-14 | 2018-12-07 | 华南理工大学 | A kind of moisture environment intelligent response glass and its preparation method and application |
| WO2019183840A1 (en) * | 2018-03-28 | 2019-10-03 | 中山大学 | Bivalent manganese-doped full inorganic perovskite quantum dot glass and preparation method therefor and use thereof |
| CN112897886A (en) * | 2021-02-04 | 2021-06-04 | 中国科学院福建物质结构研究所 | Pure silica-based glass ceramic membrane composite material |
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| CN107934916A (en) * | 2017-11-16 | 2018-04-20 | 中山大学 | It is a kind of to stablize the nanocrystalline preparation methods of unleaded full-inorganic double-perovskite A2BB ' X6 |
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| CN108947242A (en) * | 2018-08-14 | 2018-12-07 | 华南理工大学 | A kind of moisture environment intelligent response glass and its preparation method and application |
| CN108947242B (en) * | 2018-08-14 | 2021-07-20 | 华南理工大学 | Intelligent response glass for moisture environment and preparation method and application thereof |
| CN112897886A (en) * | 2021-02-04 | 2021-06-04 | 中国科学院福建物质结构研究所 | Pure silica-based glass ceramic membrane composite material |
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