CN106495171A - A kind of LaxBa2‑xTiSi2O8Amorphous and preparation method thereof - Google Patents
A kind of LaxBa2‑xTiSi2O8Amorphous and preparation method thereof Download PDFInfo
- Publication number
- CN106495171A CN106495171A CN201610999653.4A CN201610999653A CN106495171A CN 106495171 A CN106495171 A CN 106495171A CN 201610999653 A CN201610999653 A CN 201610999653A CN 106495171 A CN106495171 A CN 106495171A
- Authority
- CN
- China
- Prior art keywords
- tisi
- raw material
- laser
- block raw
- amorphous
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a kind of LaxBa2‑xTiSi2O8Amorphous and preparation method thereof, the method include：Prepare the LaxBa2‑xTiSi2O8Block raw material；Laser levitation stove is taken, the block raw material mated with the jet hole size of the laser levitation stove is cut and is put in the jet hole；Adjust laser power and the air-flow velocity of the laser levitation stove, when the block raw material be in liquid stabilising suspended state when, the laser power is reduced to rapidly zero, both the LaxBa2‑xTiSi2O8Amorphous.The application adopts La3+Substitute Ba2+Donor doping can produce Lacking oxygen, cause Ti4+It is changed into Ti3+Ionic valence condition, can further affect Ba2TiSi2O8Performance.La is prepared using based on rapid solidification, laser auxiliary heating without container technology of preparingxBa2‑xTiSi2O8Non-crystalline material is highly significant.
Description
Technical field
The present invention relates to non-crystalline material preparing technical field, more particularly to a kind of LaxBa2-xTiSi2O8Amorphous and its system
Preparation Method.
Background technology
Amorphous shortrange order, longrange disorder, isotropism, with many physical properties for being better than crystal, chemical property, electricity
Magnetic property.Have broad application prospects at aspects such as information, the energy, biology, precision machinery, Aero-Space, receive both at home and abroad
The extensive concern of researcher.The liquid of upper state is in, as temperature reduces or pressure rise, can tend to low-energy steady
Weighing apparatus crystalline state is allocated, can there are a lot of thermodynamics metastable phases between liquid and crystalline state, including the metastable non-of different-energy state
Crystalline phase, as the structure that energy reduces non-crystalline material changes the crystalline state that is changed into stable, crystallization process is different, can generate not
With the state of microstructure, different performances are produced.
In prior art, in terms of preparing non-crystal method：It is concentrated mainly on copper mold casting method, water quenching, suction casting method, orientation area
The methods such as domain smelting process, amorphous powder extrinsion pressing.But these preparation methods generally relate to the physics with hardened face
Contact, may produce heterogeneous forming core, affect amorphous formation；In addition quickly heat release is likely to the generation for causing defect.
Ba2TiSi2O8Belong to tetragonal crystal system, non-centrosymmetrical space group structure, as a kind of new ferroelectricity mineral, with
Many different particularity.It is a kind of non-lead base ferroelectric, and with abnormal piezoelectric coefficient d 33 and d31, temperature is high, stability
Good, with potential using value.Using preparation Ba in prior art2TiSi2O8Often production efficiency is not high for the method for amorphous, with
When the Ba for preparing2TiSi2O8Amorphous often contains impurity.
Content of the invention
The invention provides a kind of LaxBa2-xTiSi2O8Amorphous and preparation method thereof.
The invention provides following scheme：
A kind of LaxBa2-xTiSi2O8The preparation method of amorphous, the method include：
Prepare the LaxBa2-xTiSi2O8Block raw material；Laser levitation stove is taken, the nozzle with the laser levitation stove is cut
The block raw material of mouth size coupling are put in the jet hole；
Laser power and the air-flow velocity of the laser levitation stove is adjusted, when the block raw material suspend in liquid stable
During state, the laser power is reduced to rapidly zero, both the LaxBa2-xTiSi2O8Amorphous.
Preferably：Described prepare the LaxBa2-xTiSi2O8Block raw material；Including：
Lanthanum nitrate, citric acid, tetra-n-butyl titanate, tetraethyl orthosilicate, barium acetate, citric acid are dissolved in mixed solvent respectively
In, mixed liquor of the mixed solvent for deionized water, absolute ethyl alcohol and glacial acetic acid；
By the lanthanum nitrate being dissolved in the mixed solvent, citric acid, tetra-n-butyl titanate, tetraethyl orthosilicate, barium acetate,
Citric acid stirs into clear solution, is stored at room temperature into the wet gel of wet gel state；The wet gel is positioned in drying box
Xerogel is dried into, the xerogel is carried out the first grinding, first sieves, the first pre-burning, the first granulation, first is pressed into
Type, the first densified sintering product process both the LaxBa2-xTiSi2O8Block raw material.
Preferably：First calcined temperature is 820～850 DEG C, and the first densified sintering product temperature is 1100～1300
℃.
Preferably：Described prepare the LaxBa2-xTiSi2O8Block raw material；Including：Respectively by silica, carbonic acid
Barium, titanium dioxide, lanthana, grinding aid mixing and ball milling, by ball milling after the lanthana, gallium oxide, aluminum oxide be dried,
Second grinds, second sieves, the second pre-burning, the second granulation, second compressing, the second densified sintering product process both described
LaxBa2-xTiSi2O8Block raw material.
Preferably：Second calcined temperature is 850～900 DEG C, and the second densified sintering product temperature is 1100～1300
℃.
Preferably：The LaxBa2-xTiSi2O8Block raw material in La3+Ion, Ba2+Ion, Ti4+Ion, Si4+From
The molar percentage sum of son is 100%.
A kind of La prepared using described methodxBa2-xTiSi2O8Amorphous.
According to the specific embodiment that the present invention is provided, the invention discloses following technique effect：
By the invention it is possible to realize a kind of LaxBa2-xTiSi2O8Amorphous and preparation method thereof, under a kind of implementation, should
Method includes：Prepare the LaxBa2-xTiSi2O8Block raw material；Laser levitation stove is taken, is cut and the laser levitation stove
Jet hole size coupling the block raw material be put in the jet hole；Adjust the laser power of the laser levitation stove
And air-flow velocity, when the block raw material are in liquid stable suspended state, the laser power is reduced to rapidly zero,
Both the LaxBa2-xTiSi2O8Amorphous.The application adopts La3+Substitute Ba2+Donor doping can produce Lacking oxygen, cause Ti4+
It is changed into Ti3+Ionic valence condition, can further affect Ba2TiSi2O8Performance.Using the nothing based on rapid solidification, laser auxiliary heating
Container technology of preparing is preparing LaxBa2-xTiSi2O8Non-crystalline material is highly significant.
Certainly, the arbitrary product for implementing the present invention is it is not absolutely required to while reaching all the above advantage.
Specific embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described enforcement
Example is only a part of embodiment of the invention, rather than whole embodiment.Embodiment in based on the present invention, this area are common
The every other embodiment obtained by technical staff, belongs to the scope of protection of the invention.
In terms of preparing non-crystal method：It is concentrated mainly on copper mold casting method, water quenching, suction casting method, alignment regions smelting process, non-
The methods such as crystalline flour end extrinsion pressing.But these preparation methods generally relate to the physical contact with hardened face, may
Heterogeneous forming core is produced, amorphous formation is affected；In addition quickly heat release is likely to the generation for causing defect.Therefore, in order to obtain
Obtain super degree of supercooling greatly, it usually needs very fast cooling velocity（>105℃s-1）.However, having without container technology of preparing
Beneficial to above-mentioned issuable various problems are solved, at the same time, due to not contacting with chamber wall in whole solidification transition process,
The impurity effect that chamber wall brings is avoided simultaneously, it is suppressed that Heterogeneous Nucleation so that liquid melts are in relatively low cooling speed
Big supercooling is obtained with degree, is conducive to the formation of amorphous to be particularly the material system of amorphous formation ability difference.
Fresnoite (Ba2TiSi2O8) belonging to tetragonal crystal system, non-centrosymmetrical space group structure, used as a kind of new
Ferroelectricity mineral, with distinguished particularity.It is a kind of non-lead base ferroelectric, with abnormal 33 He of piezoelectric coefficient d
D31, temperature are high, and good stability, with potential using value.The application adopts La3+Substitute Ba2+Donor doping can produce oxygen
Room, causes Ti4+It is changed into Ti3+Ionic valence condition, can further affect Ba2TiSi2O8Performance.Using based on rapid solidification, swash
What light auxiliary was heated prepares La without container technology of preparingxBa2-xTiSi2O8Non-crystalline material is highly significant.
Embodiment
A kind of La provided in an embodiment of the present inventionxBa2-xTiSi2O8The preparation method of amorphous, the method include：
Prepare the LaxBa2-xTiSi2O8Block raw material；In actual applications, the block raw material can be solidifying using colloidal sol
Prepared by glue method, specifically respectively by lanthanum nitrate, citric acid, tetra-n-butyl titanate, tetraethyl orthosilicate, barium acetate, citric acid dissolving
In mixed solvent, mixed liquor of the mixed solvent for deionized water, absolute ethyl alcohol and glacial acetic acid；Institute is dissolved in by described
State the lanthanum nitrate in mixed solvent, citric acid, tetra-n-butyl titanate, tetraethyl orthosilicate, barium acetate, citric acid stir into transparent molten
Liquid, is stored at room temperature into the wet gel of wet gel state；The wet gel is positioned in drying box and is dried into xerogel, will be described
Xerogel carry out the first grinding, first sieve, the first pre-burning, the first granulation, first compressing, the first densified sintering product process both
Obtain the LaxBa2-xTiSi2O8Block raw material.Further, the absolute ethyl alcohol that includes in the mixed solvent and
Glacial acetic acid is 4 with the mol ratio of the tetra-n-butyl titanate:1.First calcined temperature is 820～850 DEG C, and described first burns
Knot densification temperature is 1100～1300 DEG C.Can also be prepared using solid phase method, specifically, respectively by silica, carbonic acid
Barium, titanium dioxide, lanthana, grinding aid mixing and ball milling, by ball milling after the lanthana, gallium oxide, aluminum oxide be dried,
Second grinds, second sieves, the second pre-burning, the second granulation, second compressing, the second densified sintering product process both described
LaxBa2-xTiSi2O8Block raw material.Further, second calcined temperature is 850～900 DEG C, second sintering
Densification temperature is 1100～1300 DEG C.The LaxBa2-xTiSi2O8Block raw material in La3+Ion, Ba2+Ion, Ti4+From
Son, Si4+The molar percentage sum of ion is 100%.
Laser levitation stove is taken, the block raw material mated with the jet hole size of the laser levitation stove is cut and is put into
In the jet hole；Laser have very high energy density, can any dystectic material of rapid melting, solidifying for orienting
Gu when temperature gradient of solid-liquid interface up to 103～104The K/cm orders of magnitude, far above traditional solidification technology of preparing and electricity
Beamlet suspension zone-melting technique.Realizing laser suspension zone-melting is that a kind of that metal or nonmetallic materials are carried out with region using high energy laser beam is molten
Change with without interface rapid thermal conduction from the Quench Rapid Directional Solidification method that quenches, with smelting temperature high, thermograde is high, solidification
Speed control high precision, material and environmental suitability extensively, without the need for crucible pollution-free the features such as, can quickly obtain tissue ultra-fine
Change, distributed mutually is uniform, the composite of orientation high precision.
Laser power and the air-flow velocity of the laser levitation stove is adjusted, when the block raw material are in liquid stable
During suspended state, the laser power is reduced to rapidly zero, in order to obtain big super degree of supercooling, it usually needs very fast cooling
Speed（>105℃s-1）.Both the LaxBa2-xTiSi2O8Amorphous.
A kind of La prepared using described methodxBa2-xTiSi2O8Amorphous.
In a word, the method that the application is provided is utilized without container technology of preparing, based on rapid solidification and laser auxiliary heating skill
Art, LaxBa2-xTiSi2O8Block raw material be frozen in uniform liquid condition, as levitation melting is connect without container during preparation
Touch, effectively inhibit Heterogeneous Nucleation so that liquid melts are obtained with big supercooling under relatively low cooling velocity, have
Formation beneficial to amorphous is particularly the material system of amorphous formation ability difference.
It should be noted that herein, such as first and second or the like relational terms are used merely to a reality
Body or operation are made a distinction with another entity or operation, and are not necessarily required or implied these entities or deposit between operating
In any this actual relation or order.And, term " including ", "comprising" or its any other variant are intended to
Nonexcludability includes, so that a series of process, method, article or equipment including key elements not only includes that those will
Element, but also other key elements including being not expressly set out, or also include for this process, method, article or equipment
Intrinsic key element.In the absence of more restrictions, the key element for being limited by sentence "including a ...", it is not excluded that
Also there is other identical element in process, method, article or equipment including the key element.
Presently preferred embodiments of the present invention is the foregoing is only, protection scope of the present invention is not intended to limit.All
Any modification, equivalent substitution and improvements that is made within the spirit and principles in the present invention etc., are all contained in protection scope of the present invention
Interior.
Claims (7)
1. a kind of LaxBa2-xTiSi2O8The preparation method of amorphous, it is characterised in that methods described includes：
Prepare the LaxBa2-xTiSi2O8Block raw material；
Take laser levitation stove, cut the block raw material mated with the jet hole size of the laser levitation stove be put into described
In jet hole；
Laser power and the air-flow velocity of the laser levitation stove is adjusted, when the block raw material suspend in liquid stable
During state, the laser power is reduced to rapidly zero, both the LaxBa2-xTiSi2O8Amorphous.
2. method according to claim 1, it is characterised in that described prepare the LaxBa2-xTiSi2O8Block former material
Material；Including：
Lanthanum nitrate, citric acid, tetra-n-butyl titanate, tetraethyl orthosilicate, barium acetate, citric acid are dissolved in mixed solvent respectively
In, mixed liquor of the mixed solvent for deionized water, absolute ethyl alcohol and glacial acetic acid；
By the lanthanum nitrate being dissolved in the mixed solvent, citric acid, tetra-n-butyl titanate, tetraethyl orthosilicate, barium acetate,
Citric acid stirs into clear solution, is stored at room temperature into the wet gel of wet gel state；The wet gel is positioned in drying box
Xerogel is dried into, the xerogel is carried out the first grinding, first sieves, the first pre-burning, the first granulation, first is pressed into
Type, the first densified sintering product process both the LaxBa2-xTiSi2O8Block raw material.
3. method according to claim 2, it is characterised in that first calcined temperature is 820～850 DEG C, described the
One densified sintering product temperature is 1100～1300 DEG C.
4. method according to claim 1, it is characterised in that described prepare the LaxBa2-xTiSi2O8Block former material
Material；Including：
Respectively by silica, brium carbonate, titanium dioxide, lanthana, grinding aid mixing and ball milling, by ball milling after the oxidation
Lanthanum, gallium oxide, aluminum oxide are dried, second grinds, second sieves, the second pre-burning, the second granulation, second compressing, the
Two densified sintering products process both the LaxBa2-xTiSi2O8Block raw material.
5. method according to claim 4, it is characterised in that second calcined temperature is 850～900 DEG C, described the
Two densified sintering product temperature are 1100～1300 DEG C.
6. the method according to claim 1, it is characterised in that the LaxBa2-xTiSi2O8Block raw material in La3+
Ion, Ba2+Ion, Ti4+Ion, Si4+The molar percentage sum of ion is 100%.
7. the La that prepared by a kind of method described in employing claim 1 to 6 any onexBa2-xTiSi2O8Amorphous.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610999653.4A CN106495171A (en) | 2016-11-14 | 2016-11-14 | A kind of LaxBa2‑xTiSi2O8Amorphous and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610999653.4A CN106495171A (en) | 2016-11-14 | 2016-11-14 | A kind of LaxBa2‑xTiSi2O8Amorphous and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106495171A true CN106495171A (en) | 2017-03-15 |
Family
ID=58324247
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610999653.4A Pending CN106495171A (en) | 2016-11-14 | 2016-11-14 | A kind of LaxBa2‑xTiSi2O8Amorphous and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106495171A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108706635A (en) * | 2018-06-12 | 2018-10-26 | 东北大学 | A kind of atom equimolar is than non-crystalline material and preparation method thereof |
| CN108821571A (en) * | 2018-07-10 | 2018-11-16 | 东北大学秦皇岛分校 | A kind of high entropy amorphous oxide and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1237149A (en) * | 1997-09-05 | 1999-12-01 | Tdk株式会社 | Barium titanate-base semiconductor ceramic |
| CN101402524A (en) * | 2008-11-13 | 2009-04-08 | 常熟通富电子有限公司 | Low-resistance, high-overpressure resistance barium titanate based ceramic thermal resistance and method of manufacturing the same |
-
2016
- 2016-11-14 CN CN201610999653.4A patent/CN106495171A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1237149A (en) * | 1997-09-05 | 1999-12-01 | Tdk株式会社 | Barium titanate-base semiconductor ceramic |
| CN101402524A (en) * | 2008-11-13 | 2009-04-08 | 常熟通富电子有限公司 | Low-resistance, high-overpressure resistance barium titanate based ceramic thermal resistance and method of manufacturing the same |
Non-Patent Citations (2)
| Title |
|---|
| ZHI-YONG MAO ET AL.: "Generation of tunable white light in blue-green self-activated Ba2TiSi2O8 phosphor by doping Sm3+ or Eu3+ ions", 《MATERIALS RESEARCH BULLETIN》 * |
| 向恒: "BaTiO3和BaTiO5陶瓷气动悬浮凝固及动力学研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108706635A (en) * | 2018-06-12 | 2018-10-26 | 东北大学 | A kind of atom equimolar is than non-crystalline material and preparation method thereof |
| CN108821571A (en) * | 2018-07-10 | 2018-11-16 | 东北大学秦皇岛分校 | A kind of high entropy amorphous oxide and preparation method thereof |
| CN108821571B (en) * | 2018-07-10 | 2021-09-28 | 东北大学秦皇岛分校 | High-entropy oxide amorphous and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110127661B (en) | Method for preparing two-dimensional ordered mesoporous nanosheet by inorganic salt interface induced assembly | |
| CN105622104A (en) | Preparation method of high-purity AlON transparent ceramic powder | |
| CN101348324A (en) | Non-transparent quartz crucible for polysilicon crystallization and manufacturing method thereof | |
| Chen et al. | Systematic optimization of ball milling for highly transparent Yb: YAG ceramic using co-precipitated raw powders | |
| CN111995393B (en) | Method for preparing aluminum titanate ceramic fiber from titanium-aluminum polymer precursor | |
| CN110963530B (en) | Preparation method of yttrium tantalate powder | |
| CN106495171A (en) | A kind of LaxBa2‑xTiSi2O8Amorphous and preparation method thereof | |
| CN105565810A (en) | Preparation method of rare-earth-doped yttrium oxide laser ceramic optical fiber | |
| Liu et al. | Effect of ammonium carbonate to metal ions molar ratio on synthesis and sintering of Nd: YAG nanopowders | |
| CN106495208B (en) | A kind of lanthanum gallate amorphous and preparation method thereof | |
| CN103767882A (en) | Ceramic powder for denture preparation and preparation method of ceramic powder | |
| Wang et al. | Applying the chemical bonding theory of single crystal growth to a Gd 3 Ga 5 O 12 Czochralski growth system: both thermodynamic and kinetic controls of the mesoscale process during single crystal growth | |
| CN106518044B (en) | YSAG base nano-powder and preparation method thereof | |
| CN107759240A (en) | A kind of Si3 N4The preparation method of/BAS diphase ceramic materials | |
| CN110373717A (en) | A method of REBCO high-temperature superconducting block is grown using component hierarchical control method | |
| US20080200327A1 (en) | Barium titanate single crystal and preparation method thereof | |
| CN101864620A (en) | Preparation method of silicon nitride whisker | |
| Wang et al. | A new strategy to realize phase structure and morphology of BaTiO3 nanowires controlled in ZnO-B2O3-SiO2 glass | |
| CN105401217B (en) | Utilize the method for sheet REBCO crystal growth REBCO bulk | |
| CN104445220B (en) | A kind of method preparing nano-silica powder with VTES | |
| CN110980813B (en) | High near-infrared reflectivity yttrium ferrite powder and preparation method thereof | |
| CN106631022A (en) | Tm sensitized yttria-based laser ceramic and preparation method | |
| CN106517310A (en) | Method for preparing amorphous aluminum lanthanum gallate | |
| CN106810256B (en) | Yttria-based powder with core-shell structure and preparation method thereof | |
| CN109467313A (en) | High energy storage density barium sodium niobate (BNN) base glass ceramics energy storage material and its preparation and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170315 |
|
| RJ01 | Rejection of invention patent application after publication |