CN109678498A - A kind of method of low temperature Fast Sintering NBT piezoelectric ceramics - Google Patents
A kind of method of low temperature Fast Sintering NBT piezoelectric ceramics Download PDFInfo
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- CN109678498A CN109678498A CN201910058819.6A CN201910058819A CN109678498A CN 109678498 A CN109678498 A CN 109678498A CN 201910058819 A CN201910058819 A CN 201910058819A CN 109678498 A CN109678498 A CN 109678498A
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- nbt
- piezoelectric ceramics
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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
- C04B35/475—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 bismuth titanates
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- 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
- C04B35/64—Burning or sintering processes
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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
- C04B2235/30—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
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
Abstract
The invention discloses a kind of methods of low temperature Fast Sintering NBT piezoelectric ceramics, while being sintered to NBT piezoelectric ceramics, apply electric field to its ceramic body both ends.Under electric field action, quick densifying is may be implemented in ceramics at low temperature；Solve the problems, such as the Bi element evaporation and high energy consumption caused by NBT is sintered during conventional sintering high temperature for a long time.NBT piezoelectric ceramics consistency prepared by the present invention is high, has application prospect.
Description
Technical field
Fields of the present invention are electric function ceramic fabricating technology field, and in particular to a kind of low temperature Fast Sintering
The method of NBT piezoelectric ceramics.
Background technique
Bismuth-sodium titanate (Na0.5Bi0.5TiO3Abbreviation NBT) it is the compound unleaded perovskite piezoelectricity pottery in a kind of important position A
Porcelain has many advantages, such as that piezoelectric property is strong, easily doping, stability is good.Due to electrology characteristics such as its excellent piezoelectricity, ferroelectricity, dielectrics,
The high-tech sectors such as electronics, space flight can be widely used in, sensor, energy converter, ferroelectric memory, dielectric are used to prepare
The electronic components such as capacitor are a kind of electric function ceramic materials that development prospect is wide.
Under normal conditions, for NBT piezoelectric ceramics sintering temperature at 1100 DEG C or more, sintering time is about 2h.In high temperature and length
Under the sintering condition of time, Bi2O3It is readily volatilized, so that the stoichiometric ratio of NBT piezoelectric ceramics deviates, lead to piezoelectricity
It can deteriorate.In order to reduce Bi under high temperature2O3Volatilization, excessive Bi usually is added into initial NBT green body2O3.However this side
The content that method is difficult to be accurately controlled Bi in NBT ceramics causes performance unstable so that Bi content is uncertain in product.
In addition, reducing the sintering temperature of NBT ceramics by liquid phase assisted sintering by the way that low melting point oxide is added in NBT powder.So
And often will appear the growth of miscellaneous phase or abnormal grain during the sintering process, lead to NBT piezoelectric ceramics reduced performance.
Summary of the invention
For the defect of existing sintering processing, the invention proposes a kind of method of low temperature Fast Sintering NBT piezoelectric ceramics,
This method simple process has application value.
To achieve the goals above, the technical solution adopted by the present invention is as follows:
Step 1: NBT ceramic green is heated to critical-temperature；The critical-temperature is lucky in the case where applying respective electric field intensity
There is the temperature of Fast Sintering；
Step 2: critical electric field is applied to ceramic idiosome and forms a carrying current, and duration t (20 s≤t≤
40 s), and the sintering of ceramics is completed in time t；The critical electric field is the electric field strength that Fast Sintering can occur for ceramics；Institute
It states carrying current and refers to the electric current that ceramic green can densify completely；
The electric field strength is 120 ~ 160 V/cm.
The temperature includes starting to warm up from room temperature, and until temperature reaches 800 ~ 1000 DEG C, soaking time is 20 s
~ 40 s, heating rate are 5 ~ 15 DEG C/min.
The method of the low temperature Fast Sintering NBT piezoelectric ceramics, is that NBT ceramic green is placed in sintering furnace, passes through platinum
NBT piezoelectric ceramics idiosome is connected to form access by silk with high voltage power supply, to apply electric field.
The limiting current density is 20 ~ 50mA/mm2。
The method provided by the invention for preparing NBT piezoelectric ceramics, has the advantage that
By the application of extra electric field, Fast Sintering fine and close NBT piezoelectric ceramics can be prepared under cryogenic；Pass through control
The time of added electric field processed can control the consistency of NBT ceramics；By adjusting carrying current, the acquired not isomorphous can be controlled
The NBT piezoelectric ceramics of particle size, this method is simple, has broad prospect of application.
Detailed description of the invention
Fig. 1 is the schematic device of the invention；
Fig. 2 is to apply different field current density with the change curve of furnace temperature in embodiment；
Fig. 3 is that power dissipation changes over time curve in embodiment.
Specific embodiment
The method that the present invention prepares NBT piezoelectric ceramics is that ceramic body is placed in sintering furnace, by platinum filament by ceramic blank
Body and high voltage power supply connect and apply electric field, then under specific sintering temperature, electric field strength and limiting current density
It is sintered, to prepare fine and close NBT piezoelectric ceramics.
Specifically, a kind of method of low temperature Fast Sintering NBT piezoelectric ceramics of the invention, comprising the following steps:
1) NBT ceramic body is placed in sintering furnace, and is connected ceramic body and high voltage power supply with platinum filament；
2) stove is started to warm up from room temperature, until furnace temperature reaches 800 ~ 1000 DEG C, soaking time is the s of 20s ~ 40, heating speed
Rate is 1 ~ 20 DEG C/min；
3) electric field during the sintering process, is provided to NBT ceramic body by high voltage power supply, electric field level is 120 ~ 160V/cm；And
Being arranged through the limiting current density in NBT ceramic body is 20 ~ 50 mA/mm2；
4) sample keeps a period of time under carrying current, closes power supply, and 1 ~ 10 DEG C/min of stove is down to room temperature.
The present invention promotes the sintering densification process of NBT piezoelectric ceramics by the effect of extra electric field, realizes low temperature
(≤900 DEG C) quickly (≤5min) prepare NBT piezoelectric ceramics, overcome the defect and deficiency of conventional sintering mode, the preparation side
Method is simple, there is broad prospect of application.
The present invention is further described with Figure of description combined with specific embodiments below.
Embodiment one:
NBT ceramic powder is pressed by dog bone-shaped green body using forming technique, the then pressure maintaining under the isostatic cool pressing of 200MPa
180s.NBT ceramic body is placed in sintering furnace, is connected green body and DC high-voltage power supply by platinum filament, such as Fig. 1 institute
Show.Setting electric field is 120V/cm, limiting current density 30mA/mm2, sintering furnace is then started to warm up 850 DEG C from room temperature,
Heating rate is 10 DEG C/min, and power supply is changed into constant current mode from constant voltage mode, after keeping 30s, closes power supply, stove 1 ~ 10
DEG C/min is down to room temperature, take out sample.
Embodiment two:
NBT ceramic powder is pressed by dog bone-shaped green body using forming technique, the then pressure maintaining under the isostatic cool pressing of 200MPa
180s.NBT ceramic body is placed in sintering furnace, is connected green body and DC high-voltage power supply by platinum filament, such as Fig. 1 institute
Show.Setting electric field is 140V/cm, limiting current density 30mA/mm2, sintering furnace is then started to warm up 910 DEG C from room temperature,
Heating rate is 10 DEG C/min, and power supply is changed into constant current mode from constant voltage mode, after keeping 30s, closes power supply, stove 1 ~ 10
DEG C/min is down to room temperature, take out sample.
Embodiment three:
NBT ceramic powder is pressed by dog bone-shaped green body using forming technique, the then pressure maintaining under the isostatic cool pressing of 200MPa
180s.NBT ceramic body is placed in sintering furnace, is connected green body and DC high-voltage power supply by platinum filament, such as Fig. 1 institute
Show.Setting electric field is 160V/cm, limiting current density 30mA/mm2, sintering furnace is then begun to warm to 960 from room temperature,
Heating rate is 10 DEG C/min, and power supply is changed into constant current mode from constant voltage mode, after keeping 30s, closes power supply, stove 1 ~ 10
DEG C/min is down to room temperature, take out sample.
Fig. 2 is not change curve of same electric field (120V/cm, the 140V/cm, 160V/cm) current density with furnace temperature, Cong Tuzhong
As can be seen that the corresponding Fast Sintering temperature of increase ceramics with electric field is decreased obviously, illustrate the sintering processing of electric field-assisted
Effectively reduce the sintering temperature of ceramics.
Fig. 3 is to apply not that power dissipation changes over time curve in same electric field sample, as can be seen from the figure along with when
Between passage, have an apparent sharp power density peak, illustrate that Fast Sintering phenomenon has occurred at this moment in sample.
Table is electric field-assisted sintering process and conventional sintering technique (NaCO3、Bi2O3、TiO2Stoichiometrically formula
Na0.5Bi0.5TiO3, 1100 DEG C of sintering 2h) obtained sample the comparison of piezoelectric coefficient d 33.
The prepared sample of electric field-assisted sintering is found out from table one, there is higher piezoelectric modulus, is conducive to improve ceramics
Piezoelectric property.
Claims (7)
1. a kind of method of low temperature Fast Sintering NBT piezoelectric ceramics, which comprises the steps of: make pottery to NBT piezoelectricity
While porcelain is sintered, apply electric field to its ceramic body both ends, so that quick densifying may be implemented in ceramics at low temperature.
2. a kind of method of low temperature Fast Sintering NBT piezoelectric ceramics according to claim 1, which is characterized in that described
Electric field strength is 120 ~ 160 V/cm.
3. a kind of method of low temperature Fast Sintering NBT piezoelectric ceramics according to claim 1, which is characterized in that the burning
Junction temperature is 800 ~ 1000 DEG C, and soaking time is 20 ~ 40 s, and heating rate is 5 ~ 15 DEG C/min.
4. a kind of method of low temperature Fast Sintering NBT piezoelectric ceramics according to claim 1, which is characterized in that by NBT
Ceramic green is placed in sintering furnace, connects to form access with high voltage power supply by NBT piezoelectric ceramics idiosome by platinum filament.
5. a kind of method of low temperature Fast Sintering NBT piezoelectric ceramics according to claim 1, which is characterized in that described
High voltage power supply carrying current be 200 ~ 2000 mA.
6. a kind of method of low temperature Fast Sintering NBT piezoelectric ceramics according to claim 1, which is characterized in that described
High voltage power supply be direct current or AC power source.
7. a kind of method of low temperature Fast Sintering NBT piezoelectric ceramics according to claim 1, which is characterized in that be used for
The NBT piezoelectric ceramics green compact being sintered is by isostatic cool pressing technological forming.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110294629A (en) * | 2019-08-15 | 2019-10-01 | 内蒙古科技大学 | A kind of chromic lanthanum ceramics and preparation method thereof |
| CN112919902A (en) * | 2021-03-26 | 2021-06-08 | 上海大学 | Preparation method of electric field assisted low-temperature rapid sintering fine-grain barium titanate capacitor ceramic |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6461532B1 (en) * | 1999-10-29 | 2002-10-08 | Tdk Corporation | Piezoelectric ceramic material |
| CN102863210A (en) * | 2012-10-12 | 2013-01-09 | 武汉理工大学 | Preparation method of high-density high-conductivity tin antimony oxide ceramic |
| CN105645987A (en) * | 2016-01-20 | 2016-06-08 | 西北工业大学 | Method for electric-field-assisted low-temperature fast sintering of porous ceramics |
| CN106630974A (en) * | 2016-11-25 | 2017-05-10 | 中国工程物理研究院材料研究所 | Flash sintering method of low-temperature flash sintering ceramic and obtained ceramic and device thereof |
| CN106915964A (en) * | 2017-02-21 | 2017-07-04 | 陕西科技大学 | A kind of unleaded high energy storage density ceramic material and preparation method thereof |
-
2019
- 2019-01-22 CN CN201910058819.6A patent/CN109678498A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6461532B1 (en) * | 1999-10-29 | 2002-10-08 | Tdk Corporation | Piezoelectric ceramic material |
| CN102863210A (en) * | 2012-10-12 | 2013-01-09 | 武汉理工大学 | Preparation method of high-density high-conductivity tin antimony oxide ceramic |
| CN105645987A (en) * | 2016-01-20 | 2016-06-08 | 西北工业大学 | Method for electric-field-assisted low-temperature fast sintering of porous ceramics |
| CN106630974A (en) * | 2016-11-25 | 2017-05-10 | 中国工程物理研究院材料研究所 | Flash sintering method of low-temperature flash sintering ceramic and obtained ceramic and device thereof |
| CN106915964A (en) * | 2017-02-21 | 2017-07-04 | 陕西科技大学 | A kind of unleaded high energy storage density ceramic material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| SHI RUIKE: "particle transport mode during flash sintering of sodium bismuth titanate ceramic", 《CERAMICSINTERNATIONAL》 * |
| 古训玖: "Na0.5Bi 0.5TiO3基无铅压电陶瓷与晶体的制备及电性能的研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110294629A (en) * | 2019-08-15 | 2019-10-01 | 内蒙古科技大学 | A kind of chromic lanthanum ceramics and preparation method thereof |
| CN112919902A (en) * | 2021-03-26 | 2021-06-08 | 上海大学 | Preparation method of electric field assisted low-temperature rapid sintering fine-grain barium titanate capacitor ceramic |
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Application publication date: 20190426 |