CN107697947A - A kind of method that low-temperature burning prepares barium titanate superfine powder - Google Patents
A kind of method that low-temperature burning prepares barium titanate superfine powder Download PDFInfo
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- CN107697947A CN107697947A CN201710998941.2A CN201710998941A CN107697947A CN 107697947 A CN107697947 A CN 107697947A CN 201710998941 A CN201710998941 A CN 201710998941A CN 107697947 A CN107697947 A CN 107697947A
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- barium titanate
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- 239000000843 powder Substances 0.000 title claims abstract description 37
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 25
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims abstract description 38
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- 239000011812 mixed powder Substances 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000007791 liquid phase Substances 0.000 claims abstract description 7
- 239000000376 reactant Substances 0.000 claims abstract description 3
- 239000000919 ceramic Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 238000011017 operating method Methods 0.000 claims description 4
- LKDRXBCSQODPBY-VRPWFDPXSA-N D-fructopyranose Chemical compound OCC1(O)OC[C@@H](O)[C@@H](O)[C@@H]1O LKDRXBCSQODPBY-VRPWFDPXSA-N 0.000 claims description 2
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- 125000000896 monocarboxylic acid group Chemical group 0.000 claims description 2
- APLQTTYBCHJFIJ-UHFFFAOYSA-N [Ba].[N+](=O)(O)[O-] Chemical compound [Ba].[N+](=O)(O)[O-] APLQTTYBCHJFIJ-UHFFFAOYSA-N 0.000 claims 1
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 abstract description 14
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000005049 combustion synthesis Methods 0.000 abstract description 2
- 230000036632 reaction speed Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 230000004044 response Effects 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical class [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- -1 various sensors Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of method that low-temperature burning prepares barium titanate superfine powder.This method comprises the following steps：Barium nitrate and titanium dioxide raw material are uniformly mixed according to equimolar ratio in batch mixer, obtain raw material mixed powder body, stoichiometrically add incendiary agent, add a certain proportion of liquid phase medium, it is slowly stirred at a room temperature certain time, incendiary agent and mixed powder is set uniformly to mix, obtain mixture of viscous form, it is put into container, it is brought rapidly up with the programming rate per minute not less than 10 DEG C to reactant ignition temperature, make raw material that low-temperature burning reaction occur, reacted powder sieves by grinding, obtains Super-fine Barium Titanate.The present invention utilizes low-temperature combustion synthesis, using incendiary agent barium carbonate powder is prepared in high-energy caused by ignition temperature, preparation temperature is low, and reaction speed is fast, and preparation time is short, equipment is simple, the time for preparing barium carbonate powder and energy consumption are greatly reduced, so as to improve efficiency, has saved cost, ultra-fine barium carbonate powder can be obtained simultaneously, there is extraordinary industrialization prospect.
Description
Technical field
The present invention relates to electronic ceramics technical field of powdered material preparation, and metatitanic acid is prepared more particularly to a kind of low-temperature burning
The method of barium superfine powder.
Background technology
With the development of society, electronic ceramics is in the industry using more and more, electronic ceramics industry is in China's shape
Into the industrial production system of independent completion.Wherein barium titanate ceramics material is the widest electronic ceramics of current domestic and international application
One of raw material, because it has higher dielectric constant, good ferroelectricity, piezoelectricity, pressure-resistant and insulating properties, it is mainly used in making
Capacitor, multi layer substrate, various sensors, semi-conducting material and sensing element.With barium titanate ceramics performance discovery and
As the utilization of electronic ceramic device, higher requirement is proposed to barium titanate ceramics material performance.The matter of ceramic powder
Amount directly affects the quality of final products, so the matter of utmost importance for developing barium titanate ceramics material is to prepare to meet properties of product
It is required that material powder.Mainly have to the method for preparing barium titanate ceramics powder raw material both at home and abroad at present：Solid reaction process, liquid phase
Reaction method, sol-gal process and hydro-thermal method etc..
The barium carbonate powder that traditional solid reaction process obtains exist shape of particle is irregular, particle diameter distribution is wide, component not
Uniformly, the defects of impurity content is high, and need to react at high temperature, high energy consumption, cost is high.Its technological process of sol-gal process
Length is, it is necessary to first prepare precursor, and to consume relatively expensive chemical raw material, while impurity in products is more.Liquid phase reactor method and
Hydro-thermal method adds technological process, and generated time is long, it is necessary to high using a large amount of soda acids, cost.
The content of the invention
The present invention is intended to provide a kind of method that low-temperature burning prepares barium titanate superfine powder.
To achieve these goals, specific technical scheme is as follows：
A kind of the first aspect of the present invention, there is provided operating procedure.
（1）Barium nitrate and titanium dioxide raw material are uniformly mixed according to equimolar ratio in batch mixer, obtain raw material mixing
Powder；
（2）By step（1）Mixed powder stoichiometrically adds incendiary agent, and it is 5-10 to add with mixed powder volume ratio:1
Liquid phase medium, 20-40min is slowly stirred at a room temperature, incendiary agent and mixed powder is uniformly mixed, obtain thick mixing
Thing；
（3）By step（2）Mixture of viscous form is put into container, with the programming rate per minute not less than 10 DEG C be brought rapidly up to
Reactant ignition temperature, low-temperature burning reaction occurs；
（4）By step（3）Reacted powder sieves by grinding, obtains Super-fine Barium Titanate.
Further, the incendiary agent is CO (NH2)2、(COOH)2·H2O、CH3COONH4、C6H8O7、C6H12O6、
CH3COOC2H5、NH4NO3In one or more.
Further, the liquid phase medium is absolute ethyl alcohol and/or isopropanol.
Further, the ignition temperature is 200 DEG C to 300 DEG C.
Further, the average grain diameter of the obtained Super-fine Barium Titanate is 40-50 nanometers.
On the other hand, the method that described low-temperature burning prepares barium titanate superfine powder, barium nitrate and titanium dioxide is former
Material uniformly mixes in batch mixer according to a certain percentage, and the mol ratio of barium nitrate and titanium dioxide is 1:1, add a certain amount of combustion
Burn agent C6H8O7, the mol ratio of incendiary agent and barium nitrate is 3:1, it is 5 to add with mixed powder volume ratio:1 absolute ethyl alcohol,
30min is slowly stirred at room temperature, incendiary agent and mixed powder is uniformly mixed, obtains mixture of viscous form, by thick mixing
Thing is put into container, is brought rapidly up to 300 DEG C with the programming rate per minute not less than 10 DEG C, after question response, powder is passed through
Grinding screening, obtains Super-fine Barium Titanate.
Further, the method that described low-temperature burning prepares barium titanate superfine powder, barium nitrate and titanium dioxide is former
Material uniformly mixes in batch mixer according to a certain percentage, and the mol ratio of barium nitrate and titanium dioxide is 1:1, add a certain amount of combustion
Burn agent CH3COONH4, the mol ratio of incendiary agent and barium nitrate is 2:1, it is 7 to add with mixed powder volume ratio:1 absolute ethyl alcohol,
25min is slowly stirred at a room temperature, incendiary agent and mixed powder is uniformly mixed, obtains mixture of viscous form, will be thick mixed
Compound is put into container, is brought rapidly up to 250 DEG C with the programming rate per minute not less than 10 DEG C, after question response, powder is passed through
Grinding screening is crossed, obtains Super-fine Barium Titanate.
The present invention has advantages below or feature：
The present invention proposes a kind of method that low-temperature burning prepares barium titanate superfine powder, using low-temperature combustion synthesis, utilizes
Incendiary agent prepares barium carbonate powder in high-energy caused by ignition temperature, and preparation temperature is low, and reaction speed is fast, and preparation time is short,
Equipment is simple, greatly reduces the time for preparing barium carbonate powder and energy consumption, so as to improve efficiency, has saved cost, simultaneously
Ultra-fine barium carbonate powder can be obtained, there is extraordinary industrialization prospect.
Brief description of the drawings
Fig. 1 is the process chart of the present invention；
Fig. 2 is the XRD of Super-fine Barium Titanate prepared by the embodiment of the present invention 1
Fig. 3 is the scanning electron microscope (SEM) photograph of Super-fine Barium Titanate prepared by the embodiment of the present invention 2.
Embodiment
The preparation method of the compound of the present invention is specifically described below by embodiment.
Embodiment 1
Barium nitrate and titanium dioxide raw material are uniformly mixed in batch mixer according to a certain percentage, barium nitrate and titanium dioxide rub
You are than being 1:1, add a certain amount of incendiary agent C6H8O7, the mol ratio of incendiary agent and barium nitrate is 3:1, add and mixed powder
Volume ratio is 5:1 absolute ethyl alcohol, is slowly stirred at a room temperature 30min, incendiary agent and mixed powder is uniformly mixed, is glued
Thick shape mixture, mixture of viscous form is put into container, is brought rapidly up with the programming rate per minute not less than 10 DEG C to 300
DEG C, after question response, powder is sieved by grinding, obtains Super-fine Barium Titanate.
Embodiment 2
Barium nitrate and titanium dioxide raw material are uniformly mixed in batch mixer according to a certain percentage, barium nitrate and titanium dioxide rub
You are than being 1:1, add a certain amount of incendiary agent CH3COONH4, the mol ratio of incendiary agent and barium nitrate is 2:1, add and mixed powder
Body volume ratio is 7:1 absolute ethyl alcohol, is slowly stirred at a room temperature 25min, incendiary agent and mixed powder is uniformly mixed, obtains
Mixture of viscous form, mixture of viscous form is put into container, with the programming rate per minute not less than 10 DEG C be brought rapidly up to
250 DEG C, after question response, powder is sieved by grinding, obtains Super-fine Barium Titanate.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention.For those skilled in the art
For member, the present invention can have various modifications and variations, within the spirit and principles of the invention, any modification for being made, etc.
With replacement, improvement etc., should be included in the scope of the protection.
Claims (8)
1. a kind of method that low-temperature burning prepares barium titanate superfine powder, it is characterised in that carried out according to following operating procedure：
（1）Barium nitrate and titanium dioxide raw material are uniformly mixed according to equimolar ratio in batch mixer, obtain raw material mixed powder body；
（2）By step（1）The mixed powder stoichiometrically adds incendiary agent, and it is 5- to add with mixed powder volume ratio
10:1 liquid phase medium, is slowly stirred at a room temperature 20-40min, incendiary agent and mixed powder is uniformly mixed, and obtains thick
Mixture；
（3）By step（2）The mixture of viscous form is put into container, is risen rapidly with the programming rate per minute not less than 10 DEG C
Temperature makes raw material that low-temperature burning reaction occur to reactant ignition temperature；
（4）By step（3）The reacted powder sieves by grinding, obtains Super-fine Barium Titanate.
2. the method that a kind of low-temperature burning described in claim 1 prepares barium titanate superfine powder, it is characterised in that the nitric acid
Barium raw material is analysis pure raw material, and titanium dioxide raw material is industrial raw material.
3. the method that a kind of low-temperature burning according to claim 1 prepares barium titanate superfine powder, it is characterised in that described
Incendiary agent is CO (NH2)2、(COOH)2·H2O、CH3COONH4、C6H8O7、C6H12O6、CH3COOC2H5、NH4NO3In one kind or
Person is a variety of.
4. the method that a kind of low-temperature burning according to claim 1 prepares barium titanate superfine powder, it is characterised in that described
Liquid phase medium is absolute ethyl alcohol and/or isopropanol.
5. the method that a kind of low-temperature burning according to claim 1 prepares barium titanate superfine powder, it is characterised in that described
Ignition temperature is 200 DEG C to 300 DEG C.
6. the method that a kind of low-temperature burning according to claim 1 prepares barium titanate superfine powder, it is characterised in that obtain
The average grain diameter of superfine barium titanate ceramic powder be 40-50 nanometers.
7. the method that a kind of low-temperature burning according to claim any one of 1-6 prepares barium titanate superfine powder, its feature
It is, is carried out according to following operating procedure：
（1）Barium nitrate and titanium dioxide raw material are uniformly mixed according to equimolar ratio in batch mixer, obtain raw material mixed powder body；
（2）By step（1）The mixed powder is 3 by the mol ratio of incendiary agent and barium nitrate:1 adds incendiary agent C6H8O7, add
It is 5 with mixed powder volume ratio:1 absolute ethyl alcohol, is slowly stirred at a room temperature 30min, makes incendiary agent and mixed powder uniform
Mixing, obtains mixture of viscous form；
（3）By step（2）The mixture of viscous form is put into container, is risen rapidly with the programming rate per minute not less than 10 DEG C
Temperature makes raw material that low-temperature burning reaction occur to 300 DEG C；
（4）By step（3）The reacted powder sieves by grinding, obtains Super-fine Barium Titanate.
8. the method that a kind of low-temperature burning according to claim any one of 1-6 prepares barium titanate superfine powder, its feature
It is, is carried out according to following operating procedure：
（1）Barium nitrate and titanium dioxide raw material are uniformly mixed according to equimolar ratio in batch mixer, obtain raw material mixed powder body；
（2）By step（1）The mixed powder is 2 by the mol ratio of incendiary agent and barium nitrate:1 adds incendiary agent CH3COONH4,
It is 7 to add with mixed powder volume ratio:1 absolute ethyl alcohol, is stirred at room temperature 25min, makes incendiary agent and mixed powder uniform
Mixing, obtains mixture of viscous form；
（3）By step（2）The mixture of viscous form is put into container, is risen rapidly with the programming rate per minute not less than 10 DEG C
Temperature makes raw material that low-temperature burning reaction occur to 250 DEG C；
（4）By step（3）The reacted powder sieves by grinding, obtains Super-fine Barium Titanate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710998941.2A CN107697947A (en) | 2017-10-24 | 2017-10-24 | A kind of method that low-temperature burning prepares barium titanate superfine powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710998941.2A CN107697947A (en) | 2017-10-24 | 2017-10-24 | A kind of method that low-temperature burning prepares barium titanate superfine powder |
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ID=61182157
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| CN201710998941.2A Pending CN107697947A (en) | 2017-10-24 | 2017-10-24 | A kind of method that low-temperature burning prepares barium titanate superfine powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20230183088A1 (en) * | 2021-12-10 | 2023-06-15 | Wuhan Institute Of Technology | Method for making barium titanate nanopowders |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273563A (en) * | 1998-05-20 | 2000-11-15 | 东邦钛株式会社 | Barium titanate powder |
| CN1390806A (en) * | 2002-07-10 | 2003-01-15 | 清华大学 | Process for preparing tetragonal nanoparticles of barium titanate |
-
2017
- 2017-10-24 CN CN201710998941.2A patent/CN107697947A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273563A (en) * | 1998-05-20 | 2000-11-15 | 东邦钛株式会社 | Barium titanate powder |
| CN1390806A (en) * | 2002-07-10 | 2003-01-15 | 清华大学 | Process for preparing tetragonal nanoparticles of barium titanate |
Non-Patent Citations (1)
| Title |
|---|
| 胡芳仁等: ""硝酸根与柠檬酸的摩尔比对低温燃烧合成钛酸钡的影响"", 《宇航材料工艺》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20230183088A1 (en) * | 2021-12-10 | 2023-06-15 | Wuhan Institute Of Technology | Method for making barium titanate nanopowders |
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Application publication date: 20180216 |