CN106116567A - The preparation method of high density nano barium titanate titanate ceramics - Google Patents
The preparation method of high density nano barium titanate titanate ceramics Download PDFInfo
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- CN106116567A CN106116567A CN201610454883.2A CN201610454883A CN106116567A CN 106116567 A CN106116567 A CN 106116567A CN 201610454883 A CN201610454883 A CN 201610454883A CN 106116567 A CN106116567 A CN 106116567A
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- pyrophyllite
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- 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
Abstract
The present invention proposes a kind of method preparing high density nano barium titanate titanate ceramics, comprises the steps: 1), at room temperature, by steel mold, nanometer barium titanate powder is pressed into thin slice with the unidirectional pressurization of the pressure of 8Mpa on tablet machine, the dwell time is 6 10 minutes；2), the thin slice pressed in step 1) is annealed；3), nano barium phthalate chip sample is taken out from annealing furnace, sample native silver is wrapped, it is then placed in boron nitride tube, again boron nitride tube is put in hollow plumbago post, boron nitride tube two ends boron nitride post is blocked, afterwards hollow plumbago post is loaded in the pyrophyllite in lumps being equipped with hole, hollow plumbago post two ends put graphite flake and molybdenum sheet successively, the last whole pyrophyllite hole steel loop having aluminium foil to wrap blocks, pyrophyllite makees transmission medium, heating furnace is used as by hollow plumbago post, the pyrophyllite installed is put into cubic hinge press is carried out hot-forming, hot pressing takes out sample after completing, i.e. available fine and close nano barium titanate titanate ceramics.
Description
Technical field
The present invention relates to a kind of utilize high pressure to obtain the preparation method of high density nano barium titanate titanate ceramics, wherein, pass through
Specific annealing steps and high-pressure sinter step obtain the high density nano barium titanate titanate ceramics of high-compactness.
Background technology
Pottery is the material that the raw material that the mankind utilize nature to be provided the earliest manufactures, and has long history.In this century
Since Ye, due to the development of ceramic technology, the pottery of some function admirables occurs successively.Function ceramics refers to have special power
, electricity, thermal property and the ceramic material that can intercouple between mechanical, electrical, sound, light, thermal and magnetic.Function ceramics has
Many special performances: high-dielectric coefficient, piezoelectricity, ferroelectricity, semiconductive, induced transformation etc..Main group of function ceramics
One-tenth part is dielectric ceramics and ferroelectricity, piezoelectric ceramics, such as Barium metatitanate., and its main application fields is extensive in information technology
The electronic devices and components of application.Along with mobile communication and the development of satellite communication, the most in the last few years, a weight of function ceramics
The development trend wanted is exactly that device weight constantly alleviates, size constantly reduces, miniaturization, integrated, chip type, multiple stratification, many
Functionalization becomes the main flow of development gradually, the microelectric technique since 21st century, based on quasiconductor
Development, characteristic size would fall to below 100nm, and function ceramics must be in the face of the challenge of nanotechnology, and this is to realize
The technical foundation of miniaturization/miniaturization.Therefore, function ceramics nanorize, nano ceramics, nano-device are that information pottery is further
The inexorable trend of development, is the most just becoming a new focus of international research.Nano-functional Ceramics the most only has nanostructured
Undersized feature, and the most all special unusual performances, this is to design new functional material to provide possibility, is also
The future of function ceramics provides tempting prospect.
Sintering is the process that ceramic material densification, crystal grain are grown up, crystal boundary is formed, be ceramic standby during most important
Stage.The sintering of conventional ceramic typically need not too consider the growth of crystal grain, the most necessary in the sintering process of nano ceramics
Take all necessary measure and control growing up of crystal grain.In the sintering of nano ceramics, the raw material of use is nano-powder, at sintering
During there will be new problem.Due to the huge surface area of nano-powder, the surface as sintering driving force can be also along with play
Increasing, diffusion rate increases, and the evolving path shortens, and nuclearing centre is also uprushed so that reaction distance shortens, and contact surface increases, thus
Reaction rate is accelerated, and sintering temperature is greatly lowered.In the sintering process of nano material, how to control various technological parameter,
Suppression nano-particle crystal grain in sintering process is grown up so that it is keeps primary characteristic, makes sintered body high compaction again, be to receive
The technical barrier that the rice block materials person of preparation faces.The principal element causing crystal grain to be grown up has 2 points: one is sintering temperature,
Crystallite dimension significantly increases along with the rising of sintering temperature；Two is temperature retention time, and crystallite dimension is along with the prolongation of temperature retention time
And increase.Therefore, conventional sintering process is used to be difficult to keep the characteristic of nano material.Existing a lot of by high-pressure sintering process, example
As, it is sintered under several ten thousand atmospheric pressure by tabletting prepared by nano ceramics, although compared with conventional method, high pressure combustion
Connection has many good qualities, but, at about 60,000 atmospheric pressure of 6GPa() high pressure under, around pyrophillite formed sealing strip, sample is several
It is in the atmosphere of vacuum, when nano barium titanate titanate ceramics sinters in vacuum, inert atmosphere or reducing atmosphere, oxygen can be produced
Room, the existence of Lacking oxygen not only can affect the compactness of nano barium titanate titanate ceramics, also can affect its ferroelectric properties.
Summary of the invention
It is an object of the invention to by special cycle of annealing and special high-pressure sinter program, it is provided that one prepares height
The method of density nano barium titanate titanate ceramics.The barium titanate ceramics using the method for the invention to prepare not only have high densification
Degree, also has good ferroelectric properties.
The object of the present invention is achieved like this:
A kind of method preparing high density nano barium titanate titanate ceramics, comprises the steps:
1), at room temperature, by steel mold, nanometer barium titanate powder is pressed into thin with the unidirectional pressurization of the pressure of 8Mpa on tablet machine
Sheet, the dwell time is 6-10 minute；
2), annealing the thin slice pressed in step 1), concrete annealing steps is as follows:
(1) the nano barium phthalate thin slice suppressed is put on the specimen holder of annealing furnace, closed annealing stove, it is passed through in annealing furnace
Oxygen；
(2) use accurate temperature controller, with the heating rate of 2 DEG C/min, the sample in annealing furnace is heated to 120 DEG C, be incubated 2h,
Sample in annealing furnace is heated to 400 DEG C by the heating rate using accurate temperature controller 5-10 DEG C/min, is incubated 1h；Then use
Sample in annealing furnace is heated to 600 DEG C with the heating rate of 2-4 DEG C/min by accurate temperature controller, is incubated 6h；
(3) close accurate temperature controller, make annealing furnace be naturally cooling to room temperature；
3), from annealing furnace, take out nano barium phthalate chip sample, sample native silver wrapped, is then placed in boron nitride tube,
Being put into by boron nitride tube in hollow plumbago post, boron nitride tube two ends boron nitride post is blocked again, and is loaded by hollow plumbago post afterwards
Being equipped with in the pyrophyllite in lumps in hole, hollow plumbago post two ends put graphite flake and molybdenum sheet successively, and last whole pyrophyllite hole is with there being aluminium foil
The steel loop (filling up with pyrophyllite fragment in ring) wrapped blocks, and pyrophyllite makees transmission medium, and heating furnace is used as by hollow plumbago post, will
The pyrophyllite installed is put in cubic hinge press and is pressurized to 6GPa, begins to warm up after reaching pressure, and being heated to temperature is 900
～1100 DEG C, heating rate 200～250 DEG C/min, under the conditions of this high pressure-temperature, then it is incubated 5～15min, then starts
Blood pressure lowering, pressure is down to 3GPa, pressurize 10min, is started release of lowering the temperature, and is down to atmospheric pressure and room temperature, takes out sample, then peels off
Native silver on sample, i.e. available fine and close nano barium titanate titanate ceramics.
Preferably, heating rate sample being heated to 400 DEG C in annealing steps (2) is 7-8 DEG C/min.
Preferably, heating rate sample being heated to 600 DEG C in annealing steps (2) is 3 DEG C/min.
Preferably, in step 3), the 6GPa lower dwell time is 10min.
Preferably, in step 3), under 6GPa, pressurize temperature is 1000 DEG C.
It practice, the existence of Lacking oxygen causes appraising at the current rate of Ti ion in lattice, there is Ti4+Become Ti3+So that in sample
Carrier increase, resistivity reduce.In sample, the existence of Lacking oxygen and the resistivity that thus causes reduce to carry out dielectric material
Saying it is the most disadvantageous, the present invention improves the Lacking oxygen in nano barium phthalate ceramics sample by stage cycle of annealing, carries
High consistency and ferroelectric properties.
Accompanying drawing explanation
Fig. 1 is the work simulation figure of the cubic hinge press of the present invention；
Fig. 2 is the SEM photograph after the annealed process of nano barium phthalate ceramics sample of the present invention and HIGH PRESSURE TREATMENT；
Sample assembly schematic diagram when Fig. 3 is to carry out High Temperature High Pressure sintering in the present invention；
Fig. 4 be the present invention the annealed process of nano barium phthalate ceramics sample and without annealing dielectric constant-temperature
Degree characteristic；
Fig. 5 a is that the nano barium phthalate ceramics sample of the present invention is without ferroelectric hysteresis loop detected after annealing；
Fig. 5 b is ferroelectric hysteresis loop detected after the annealed process of nano barium phthalate ceramics sample of the present invention；
Fig. 6 is the drain current versus before and after the nano barium phthalate ceramics sample annealing of the present invention.
Detailed description of the invention:
1), at room temperature, by steel mold, nanometer barium titanate powder is pressed into thin with the unidirectional pressurization of the pressure of 8Mpa on tablet machine
Sheet, the dwell time is 8 minutes；
2), annealing the thin slice pressed in step 1), concrete annealing steps is as follows:
(1) the nano barium phthalate thin slice suppressed is put on the specimen holder of annealing furnace, closed annealing stove, it is passed through in annealing furnace
Oxygen；
(2) use accurate temperature controller, with the heating rate of 2 DEG C/min, the sample in annealing furnace is heated to 120 DEG C, be incubated 2h,
Sample in annealing furnace is heated to 400 DEG C by the heating rate using accurate 7 DEG C/min of temperature controller, is incubated 1h；Then essence is used
Sample in annealing furnace is heated to 600 DEG C with the heating rate of 3 DEG C/min by close temperature controller, is incubated 6h；
(3) close accurate temperature controller, make annealing furnace be naturally cooling to room temperature；
3), from annealing furnace, take out nano barium phthalate chip sample, sample native silver wrapped, is then placed in boron nitride tube,
Being put into by boron nitride tube in hollow plumbago post, boron nitride tube two ends boron nitride post is blocked again, and is loaded by hollow plumbago post afterwards
Being equipped with in the pyrophyllite in lumps in hole, hollow plumbago post two ends put graphite flake and molybdenum sheet successively, and last whole pyrophyllite hole is with there being aluminium foil
The steel loop (filling up with pyrophyllite fragment in ring) wrapped blocks, and pyrophyllite makees transmission medium, and heating furnace is used as by hollow plumbago post, will
The pyrophyllite installed is put in cubic hinge press and is pressurized to 6GPa, begins to warm up after reaching pressure, is heated to temperature and is
1000 DEG C, heating rate 230 DEG C/min, then under the conditions of this high pressure-temperature, it is incubated 10 minutes, then starts blood pressure lowering, pressure
It is down to 3GPa, pressurize 10min, starts release of lowering the temperature, be down to atmospheric pressure and room temperature, take out sample, then peel off on sample
Native silver, i.e. available fine and close nano barium titanate titanate ceramics.
Accompanying drawing 1 illustrates the operating diagram of the cubic hinge press of the present invention, and cubic hinge press belongs to prior art, its structure
Do not repeat with operation principle.
Accompanying drawing 2 illustrates the SEM picture of the nano barium titanate titanate ceramics sintered, and is not difficult to find out from this figure, barium titanate nano
Close-packed arrays between crystal grain, its consistency is more than 99%.
Accompanying drawing 3 illustrates the assembling schematic diagram before high-temperature sample high-pressure sinter.Pyrophyllite block, graphite and conduct conduction in figure
The steel loop of joint, molybdenum sheet are standard components.Transmission medium in graphite furnace is h-BN, and it has excellent pressure transmission and machinery adds
Work.Its chemical property is more stable, and shear strength is relatively big, can reduce graphite furnace deformation under high pressure.It addition, it
Conductivity of heat also preferable, be conducive to reducing the thermograde in graphite furnace.
Accompanying drawing 4 illustrates the annealed process of nano barium phthalate ceramics sample and the dielectric constant-temperature without annealing
Degree characteristic, the dielectric constant of the sample of annealed process is apparently higher than the sample for annealed process.
Before and after accompanying drawing 5a and 5b illustrates the nano barium phthalate ceramics sample annealing of the present invention, detected electric hysteresis returns
Line, cannot present ferroelectric hysteresis loop substantially without the nano barium phthalate pottery of annealing, and the sample of annealed process
It is observed that ferroelectric hysteresis loop clearly.
Accompanying drawing 6 illustrates the annealed process of nano barium phthalate ceramics sample and the leakage current without annealing, from figure
Above it is apparent that the leakage current of the sample of annealed process significantly reduces, it is in extremely low in whole voltage range
Level.
From above comparative example it can be seen that the performance of nano barium titanate titanate ceramics is had by the stepped annelaing program of the present invention
Significantly improve.
Claims (5)
1. the method preparing high density nano barium titanate titanate ceramics, comprises the steps:
1), at room temperature, by steel mold, nanometer barium titanate powder is pressed into thin with the unidirectional pressurization of the pressure of 8Mpa on tablet machine
Sheet, the dwell time is 6-10 minute；
2), annealing the thin slice pressed in step 1), concrete annealing steps is as follows:
(1) the nano barium phthalate thin slice suppressed is put on the specimen holder of annealing furnace, closed annealing stove, it is passed through in annealing furnace
Oxygen；
(2) use accurate temperature controller, with the heating rate of 2 DEG C/min, the sample in annealing furnace is heated to 120 DEG C, be incubated 2h,
Sample in annealing furnace is heated to 400 DEG C by the heating rate using accurate temperature controller 5-10 DEG C/min, is incubated 1h；Then use
Sample in annealing furnace is heated to 600 DEG C with the heating rate of 2-4 DEG C/min by accurate temperature controller, is incubated 6h；
(3) close accurate temperature controller, make annealing furnace be naturally cooling to room temperature；
3), from annealing furnace, take out nano barium phthalate chip sample, sample native silver wrapped, is then placed in boron nitride tube,
Being put into by boron nitride tube in hollow plumbago post, boron nitride tube two ends boron nitride post is blocked again, and is loaded by hollow plumbago post afterwards
Being equipped with in the pyrophyllite in lumps in hole, hollow plumbago post two ends put graphite flake and molybdenum sheet successively, and last whole pyrophyllite hole is with there being aluminium foil
The steel loop (filling up with pyrophyllite fragment in ring) wrapped blocks, and pyrophyllite makees transmission medium, and heating furnace is used as by hollow plumbago post, will
The pyrophyllite installed is put in cubic hinge press and is pressurized to 6GPa, begins to warm up after reaching pressure, and being heated to temperature is 900
～1100 DEG C, heating rate 200～250 DEG C/min, under the conditions of this high pressure-temperature, then it is incubated 5～15min, then starts
Blood pressure lowering, pressure is down to 3GPa, pressurize 10min, is started release of lowering the temperature, and is down to atmospheric pressure and room temperature, takes out sample, then peels off
Native silver on sample, i.e. available fine and close nano barium titanate titanate ceramics.
2. the method for claim 1, it is characterised in that in annealing steps (2), sample is heated to the intensification speed of 400 DEG C
Rate is 7-8 DEG C/min.
3. the method for claim 1, it is characterised in that in annealing steps (2), sample is heated to the intensification speed of 600 DEG C
Rate is 3 DEG C/min.
4. the method for claim 1, it is characterised in that in step 3), the 6GPa lower dwell time is 10min.
5. the method for claim 1, it is characterised in that in step 3), under 6GPa, pressurize temperature is 1000 DEG C.
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| CN101182201A (en) * | 2007-11-27 | 2008-05-21 | 清华大学 | Nano doping dielectric material for preparing base-metal inner-electrode multi-layer ceramic sheet type capacitor |
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