CN107399968A - A kind of method of low-temperature in-site method production barium titanate nano particle - Google Patents
A kind of method of low-temperature in-site method production barium titanate nano particle Download PDFInfo
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- CN107399968A CN107399968A CN201610332794.0A CN201610332794A CN107399968A CN 107399968 A CN107399968 A CN 107399968A CN 201610332794 A CN201610332794 A CN 201610332794A CN 107399968 A CN107399968 A CN 107399968A
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- barium titanate
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- 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
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- 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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
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- 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
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- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
Abstract
The present invention relates to a kind of a kind of new method of low-temperature in-site method production barium titanate nano particle.The barium titanate nano particle is prepared in accordance with the following methods：Titanium source is provided using liquid titanium-based metal organic compound, with barium hydroxide directly in forerunner's slurry is made through being stirred at room temperature, then rheology phase precursor is transferred to close container, thermostatic drying chamber is placed in after sealing, by controlling the temperature and time of solid-liquid reaction, spherical core-shell nano is prepared under cryogenic.In the preparation process, with barium hydroxide in-situ hydrolysis reaction occurs for organic titanium source, ultimately generates barium titanate.The present invention has technique simple, reaction temperature is low, environment-friendly, the advantages that unit volume yield is high, cost is cheap, obtained barium titanate nano particle is subsphaeroidal, and even size distribution, granularity is controllable, can be as the ceramic matrix raw material of the electronic components such as high-end chip capacitor, PTC thermistor.
Description
Technical field
The present invention relates to a kind of method that barium titanate nano spherical particle is prepared using low-temperature in-site rheological phase method.
Background technology
Barium titanate is a kind of strong dielectric compound material, has high-k, low-dielectric loss, without toxic element etc.
Feature, it is one of most popular material in electronic ceramics, is widely used in multiple-layer sheet ceramic capacitor, positive temperature coefficient
The fields such as thermistor, composite ceramic packing, it is referred to as the pillar of electronic ceramics industry.With modern advanced manufacturing industry pair
In the requirement more and more higher of control accuracy, it is also more and more high mutually to tackle the requirement that electronic component is integrated, minimizes.For pottery
The nanosizing of porcelain persursor material granularity proposes new requirement.At present, industrial generally use high temperature solid-state method prepares high-volume
Barium titanate ceramics powder material, its raw material is metal oxide, and the method has the obvious disadvantage that in modern industrial technology, example
Such as, the calcining heat of presoma is higher, and power consumption is high；Powder granularity is uneven, and quality conformance is difficult to ensure that；Granularity is generally higher than
100 nm, powder active is low, therefore this method has certain limitation, it is difficult to reaches the requirement of modern manufacturing industry.At present, only generation
Minority enterprise of boundary can provide high-volume nanoscale barium carbonate powder（Such as Japanese Sakai chemistry, nanoscale of the monopolization whole world more than 90%
Barium carbonate powder market）, it mainly uses liquid phase hydrothermal method, and this method equipment cost is higher, and preparation process needs to use
A large amount of liquid phase mediums and anti-agglomeration agent, unit of product yield is relatively low, and production efficiency is not high.
The present invention increasingly increases for the Barium Titanate nano-powder market demand, the high background of technology barriers, utilizes liquid titanium
Base Metal organic compound provides titanium source, is directly stirred at room temperature with barium hydroxide and forerunner's slurry is made, then by rheology phase front
Drive body to be transferred in container, by controlling the temperature and time of solid-liquid reaction, prepare spherical core-shell nano.The preparation
During, with barium hydroxide in-situ hydrolysis reaction occurs for organic titanium source, ultimately generates barium titanate.The present invention has technique simple
The advantages that single, reaction temperature is low, environment-friendly, and unit volume yield is high, cost is cheap, obtained barium titanate nano particle is near
It is spherical, and even size distribution, granularity is controllable, can be used as the electronics member devices such as high-end chip ceramic capacitor, PTC thermistor
The ceramic matrix raw material of part.
The content of the invention
It is an object of the invention to provide a kind of low energy consumption, the synthetic method of spherical barium titanate nano particle；This method profit
Barium ions is provided with barium hydroxide, liquid titanium-based metal-organic compound is titanium source, formation rheology phase forerunner after being well mixed
Body, low-temperature in-site reaction is used to prepare size as the closely spherical nano-particle of 20-100 nm barium titanate.It is of the present invention to receive
Rice corpuscles preparation method has that Product size is controllable, cost is cheap, unit volume yield is high, environment-friendly, favorable repeatability etc.
Advantage, available for fields such as chip ceramic capacitor, PTC thermistor, composite ceramic matrixs.
Low temperature rheology phase barium titanate nano-particle preparation method involved in the present invention follows these steps to carry out：
(a) barium hydroxide of certain mass is placed in beaker；
(b) the titanium-based metal organic compound of equimolar quality is added in the container in a steps；
(c) solid-liquid mixtures obtained by b step are stirred into 30 min, is well mixed solid and liquid, forms homogeneous rheology
Phase precursor；
(d) gained rheology phase precursor in step c is transferred in container, it is 10-80 % that presoma, which accounts for volume of a container,；
(e) container in Step d is sealed, be placed in insulating box, reaction temperature is 80-160 DEG C, reaction time 0.5-
15 h；
(f) step e products therefroms are transferred in Buchner funnel, are washed 3 times with 0.05-0.2 mol/L watery hydrochloric acid；
(g) step f products therefroms are distributed in centrifuge tube, and decentralized medium is deionized water, centrifuge speed 3000-5000 r/
Min, centrifuges 10-30min every time, and above-mentioned steps repeat 3-5 times；
(h) centrifugation product is placed in vacuum drying chamber and dries 24h obtained by step g.
Barium titanate nano particle of the present invention is expected to be applied to high-end chip ceramic capacitor, PTC thermistor etc.
Ceramic matrix raw material of electronic component etc..
Demand of the present invention for industrial circle for Barium Titanate nano-powder, there is provided a kind of cost is cheap, technique is simple,
Environment-friendly Barium Titanate nano-powder high-volume synthetic method, the nano-particle of this method synthesis have particle size it is small,
The advantages that pattern composition is adjustable, even size distribution, good crystallinity.
During synthesis of barium titanate nano-powder of the present invention, in the following areas with unique distinction：
(1) compared with solid phase reaction, whole preparation process temperature is more gentle（Less than 200 DEG C）, mass energy is saved, reduces system
Standby cost；
(2) same volume container yield is high, is liquid phase reactor（Hydro-thermal, sol-gal process, coprecipitation etc.）Hundreds times very
To thousands of times, production efficiency is improved；
(3) the nano-powder yardstick prepared by is homogeneous, close to single dispersing, and can adjust Product size by adjusting response parameter；
(4) in course of reaction in addition to basic titanium source and barium source, whole course of reaction participates in without other materials, the nano-powder of preparation
Purity is high, and impurity content is few；
(5) nuclear shell type nano meter particle prepared by includes following aspect application：
(a) application in high-end chip ceramic capacitor；
(b) application in PTC thermistor；
(c) application in composite ceramic matrix；
(d) application in electric powered motor power supply.
Case is embodied
Embodiment 1.
(a) barium hydroxide octahydrate of certain mass is placed in beaker；
(b) isopropyl titanate of equimolar quality is added in the container in a steps；
(c) solid-liquid mixtures obtained by b step are stirred into 30 min, is well mixed solid and liquid, forms homogeneous rheology
Phase precursor；
(d) gained rheology phase precursor in step c is transferred in container, it is 10 % that presoma, which accounts for volume of a container,；
(e) container in Step d is sealed, be placed in thermostatic drying chamber, reaction temperature is 80 DEG C, and the reaction time is 15 h；
(f) step e products therefroms are transferred in Buchner funnel, washed 3 times with 0.05mol/L watery hydrochloric acid；
(g) step f products therefroms are distributed in centrifuge tube, decentralized medium is deionized water, the r/ of centrifuge speed 3000
Min, centrifuges 20 min every time, and above-mentioned steps are repeated 5 times；
(h) centrifugation product obtained by step g is placed in drying box in vacuum drying chamber and dries 24h；
Gained powder is spherical barium titanate nano particle, and powder average grain diameter is about 30 nm.
Embodiment 2.
(a) barium hydroxide octahydrate of certain mass is placed in beaker；
(b) butyl titanate of equimolar quality is added in the container in a steps；
(c) solid-liquid mixtures obtained by b step are stirred into 30 min, is well mixed solid and liquid, forms homogeneous rheology
Phase precursor；
(d) gained rheology phase precursor in step c is transferred in container, it is 50 % that presoma, which accounts for volume of a container,；
(e) container in Step d is sealed, be placed in thermostatic drying chamber, reaction temperature is 120 DEG C, and the reaction time is 2 h；
(f) step e products therefroms are transferred in Buchner funnel, washed 3 times with 0.1 mol/L watery hydrochloric acid；
(g) step f products therefroms are distributed in centrifuge tube, decentralized medium is deionized water, the r/ of centrifuge speed 4000
Min, centrifuges 30 min every time, and above-mentioned steps are repeated 5 times；
(h) centrifugation product obtained by step g is placed in drying box in vacuum drying chamber and dries 24h；
Gained powder is spherical barium titanate nano particle, and powder average grain diameter is about 50 nm..
Embodiment 3.
(a) dried barium hydroxide of certain mass is placed in beaker；
(b) cyclopentadienyl titanium dichloride of equimolar quality is added in the container in a steps；
(c) solid-liquid mixtures obtained by b step are stirred into 30 min, is well mixed solid and liquid, forms homogeneous rheology
Phase precursor；
(d) gained rheology phase precursor in step c is transferred in container, it is 80 % that presoma, which accounts for volume of a container,；
(e) container in Step d is sealed, be placed in thermostatic drying chamber, reaction temperature is 150 DEG C, and the reaction time is 6 h；
(f) step e products therefroms are transferred in Buchner funnel, washed 3 times with 0.2 mol/L watery hydrochloric acid；
(g) step f products therefroms are distributed in centrifuge tube, decentralized medium is deionized water, the r/ of centrifuge speed 5000
Min, centrifuges 30 min every time, and above-mentioned steps are repeated 5 times；
(h) centrifugation product obtained by step g is placed in drying box in vacuum drying chamber and dries 24h；
Gained powder is spherical barium titanate nano particle, and powder average grain diameter is about 100 nm.
Claims (7)
- A kind of 1. new type low temperature method in situ for preparing barium titanate nano particle, it is characterised in that：With barium hydroxide and titanium-based gold Category organic compound is initial reactant, to form solid-liquid rheology phase precursor by the way that reaction raw materials are mixed, pass through control Reaction temperature and time, the Barium Titanate nano-powder of size uniformity is obtained under cryogenic.
- 2. in accordance with the method for claim 1, it is characterised in that the titanium source in course of reaction（Titanium-based metal organic compound） For liquid metal organic compound, include but is not limited to：Isopropyl titanate, butyl titanate, cyclopentadienyl titanium dichloride.
- 3. according to the method described in claim 1 or 2, it is characterised in that the barium source in course of reaction is solid-state barium hydroxide or water Barium hydroxide is closed, is included but is not limited to：Barium hydroxide, dried barium hydroxide, barium hydroxide octahydrate.
- 4. according to the method for claim 3, it is characterised in that：Described mixing solid-liquid rheology phase precursor is according to following Method is prepared：(a) the hydronium(ion) barium monoxide of certain mass is placed in beaker；(b) the titanium-based metal organic compound of equimolar quality is added in the beaker in a steps；(c) solid-liquid mixtures obtained by b step are stirred into 30 min, is well mixed solid and liquid, forms homogeneous rheology Phase precursor.
- 5. according to the method described in claim 1, it is characterised in that：Solid-liquid rheology phase precursor is placed in sealing container, instead Low-temp reaction should be carried out in thermostatic drying chamber, reaction temperature is 80-160 DEG C, and the reaction time is 0.5-15 h.
- 6. according to the method for claim 5, it is characterised in that：After low-temp reaction, products therefrom is handled as follows：(a) products therefrom is transferred in Buchner funnel, is washed 3 times with 0.05-0.2 mol/L watery hydrochloric acid；(b) step a products therefroms are distributed in centrifuge tube, decentralized medium is deionized water, centrifuge speed 3000-5000 R/min, centrifuges 10-30min every time, and above-mentioned steps repeat 3-5 times；(c) centrifugation product obtained by step b is placed in drying box in vacuum drying chamber and dries 24h.
- 7. according to the method for claim 6, it is characterised in that products therefrom is the closely spherical barium titanate nano grain of single dispersing Son, its size are 20-100 nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610332794.0A CN107399968A (en) | 2016-05-19 | 2016-05-19 | A kind of method of low-temperature in-site method production barium titanate nano particle |
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| CN201610332794.0A CN107399968A (en) | 2016-05-19 | 2016-05-19 | A kind of method of low-temperature in-site method production barium titanate nano particle |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114196108A (en) * | 2021-12-08 | 2022-03-18 | 丹阳新华美塑料有限公司 | Modified polypropylene film material for capacitor and preparation method thereof |
| CN114560496A (en) * | 2022-03-18 | 2022-05-31 | 中国科学院新疆理化技术研究所 | Method for preparing perovskite nano particles through low-temperature rheological phase |
-
2016
- 2016-05-19 CN CN201610332794.0A patent/CN107399968A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114196108A (en) * | 2021-12-08 | 2022-03-18 | 丹阳新华美塑料有限公司 | Modified polypropylene film material for capacitor and preparation method thereof |
| CN114560496A (en) * | 2022-03-18 | 2022-05-31 | 中国科学院新疆理化技术研究所 | Method for preparing perovskite nano particles through low-temperature rheological phase |
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Application publication date: 20171128 |