CN109553414A - A kind of zirconia ceramics plastic processing method of DC electric field auxiliary - Google Patents
A kind of zirconia ceramics plastic processing method of DC electric field auxiliary Download PDFInfo
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Abstract
The invention discloses a kind of zirconia ceramics plastic processing methods of DC electric field auxiliary, comprising the following steps: step 1: using Y2O3Stablize ZrO2Powder obtains 3YSZ sample after being molded, being sintered；Step 2: sample being heated to 600~900 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 30 min；Step 3: under the conditions of 600~900 DEG C of temperature, applying current density at sample both ends is 50~400mA/mm2DC electric field, keep 5min after sample is stretched, complete plastic processing；The present invention assists lower electro plastic effect and electrocaloric effect using DC electric field, and while environment temperature to be offered needed for improving rate of deformation, reducing plastic processing, resistance of deformation in reduction plastic processing improves the elongation percentage of plastic processing.
Description
Technical field
The present invention relates to ceramic material Technology of Plastic Processing fields, and in particular to a kind of zirconium oxide pottery of DC electric field auxiliary
Porcelain plastic processing method.
Background technique
Zirconium oxide (ZrO2) be it is a kind of have high rigidity, low heat conductivity, high tenacity, good wear resistance and corrosion resistance and high temperature from
The ceramic material of subconductivity；Since zirconia ceramics and its composite material have certain unique performances at different conditions
(such as semiconductive, functionality of sensitive and increasing tougheness)；Therefore with the development of electronics and new material industry, zirconia ceramics is main
It has become the past as application to refractory；Electronic ceramics, function ceramics and in terms of application rapidly develop；But
It is that the property of the distinctive structure of zirconia ceramics and chemical bond determines that it is a kind of intrinsic brittle material, it is difficult to use tradition
Plastic processing method manufacture complex-shaped and large-scale ceramic component, therefore greatly limit their application range.
At present about the research of zirconia ceramics plastic processing generally be directed to Ultra-fine Grained zirconia ceramics in higher deformation
The plastic deformation of temperature and lower rate of deformation；This is because it is tiny to realize that zirconia ceramics superplasticity needs to meet crystallite dimension
(1 μm of usual <) and deformation temperature T > 0.5Tm(TmFor fusing point) condition；Such as " The high temperature
Mechanical characteristics of superplastic 3mol%yttria stabilized zirconia
1998,46 (2): [J] .Acta Materialia teaches zirconia ceramics in a series of rates of deformation, temperature in 667-679. "
Deformation in degree and grain size range, maximum strain rate is 10-4s-1The order of magnitude, sample maximum extension rate is only 65%；
Such low strain rate and limited elongation percentage are difficult to meet the industrial application demand of zirconia ceramics plastic processing；Such as
“Microstructural examination in high-strain-rate superplastically deformed
tetragonal ZrO2Dispersed with 30vol%MgAl2O4spinel[J].Journal of Materials
2007,22 (03): Research mentions height of the magnesium aluminate spinel doped zirconia complex phase ceramic at 1500 DEG C in 801-813. "
Mild 10-4~10-1s-1It is deformed under strain rate, sample maximum extension rate is up to 600%, but deficiency present in it is to be formed again
Phase zircite ceramics change the one-component of zirconia material, are not suitable for processing pure zirconia material, because without
Generality；Secondly as the characteristic of multiphase structure, the metaplasia of spinelle observed in sample after deformation, and
Stomata is attached along the direction perpendicular to load, so the intensity of material cannot be guaranteed after deformation；"Effect of
Prestraining on cavity morphology in a superplastic 3mol%Yttria-stabilized
Tetragonal zirconia (3Y-TZP) [J] .Scripta Materialia, 1998,39 (1): is mentioned in 119-124. "
3YSZ ceramics are at 1400 DEG C and 10-3s-1Strain rate under reach 130% prestrain after, then with 10-4s-1Strain rate into
Row deformation, can achieve 280% elongation percentage；Although experiments have shown that introducing prestrain can effectively reduce after deforming in sample
Stomata helps to ensure that the intensity of material after deformation；But the process that prestrain increases plastic processing is introduced, increase energy
Consumption, and the strain rate of further plastic working is still very low, is unfavorable for plastic processing high efficiency.
Existing zirconia ceramics plastic processing method is often in the presence of deformation required temperature is high, rate of deformation is low, deformation is anti-
The disadvantages of power is big, elongation percentage is not high, and the strength of materials substantially reduces and changes material component after deformation, significantly limits
The application and development of zirconia ceramics.
Summary of the invention
The present invention provides a kind of electro plastic effect and electrocaloric effect under assisting using DC electric field, improves deformation speed
While environment temperature to be offered needed for rate, reduction plastic processing, resistance of deformation in plastic processing is reduced, is greatly improved
The DC electric field assisted oxidation zircon ceramic plastic processing method of plastic processing elongation percentage.
The technical solution adopted by the present invention is that: a kind of zirconia ceramics plastic processing method of DC electric field auxiliary, including
Following steps:
Step 1: using Y2O3Stablize ZrO2Powder obtains 3YSZ sample after being molded, being sintered；
Step 2: sample being heated to 600~900 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 30min；
Step 3: under the conditions of 600~900 DEG C of temperature, applying current density at sample both ends is 50~400mA/mm2's
DC electric field stretches sample after keeping 5min, completes plastic processing.
Further, it is less than≤10 in strain rate in the step 3-1s-1Or under the conditions of load >=1MPa to sample into
Row stretches.
Further, further comprising the steps of:
A circular hole is respectively set at sample both ends, connects respectively in the circular hole of circular hole interior surface conductive coating, sample both ends
Connect DC power supply positive and negative anodes.
Further, Y in the step 12O3Stablize ZrO2It is raw that powder keeps 60s to be prepared into sample under the molding of 10MPa
Base, pressureless sintering 2h obtains fine and close 3YSZ sample under the conditions of 1550 DEG C.
The beneficial effects of the invention are as follows；
(1) present invention can be realized zirconia ceramics under the conditions of 600~900 DEG C by applying DC electric field with≤10- 1s-1Strain rate carry out plastic processing；
(2) of the invention since the deformation in plastic processing can be greatly lowered in electro plastic effect and electrothermal effect
Drag, so that sample homogeneous deformation in process, effectively reduces the defect inside processed sample；Elongation percentage reaches
450% or more, still there is 98% or more consistency after deflection reaches 200%, can guarantee the intensity of material after processing
It cannot destroy；
(3) present invention reduces plastic processing temperature, processing speed is improved, effectively shortens the process-cycle, is conducive to
It realizes the highly-efficient processing of zirconia ceramics, reduces energy consumption, improve production efficiency, reduce production cost.
Detailed description of the invention
Fig. 1 is specimen clamping and the structural schematic diagram connecting with DC power supply in the present invention.
Fig. 2 is the load-deformation curve of zirconia ceramics plastic processing in the embodiment of the present invention.
Fig. 3 is strain-time graph of zirconia ceramics plastic processing in the embodiment of the present invention.
Fig. 4 is the scanning electron microscope in the embodiment of the present invention after zirconia ceramics plastic processing to certain deformation
(SEM) figure；It (a) is the SEM figure of zirconia ceramics plastic processing to 100% in embodiment 4；It (b) is zirconium oxide pottery in embodiment 2
Porcelain carving is machined to 200% SEM figure.
In figure: 1- temperature control heating furnace, the upper transmission rod of 2-, transmission rod under 3-, 4- sample, 5- pin, 6- platinum filament, 7- direct current
Source.
Specific embodiment
The present invention will be further described in the following with reference to the drawings and specific embodiments.
A kind of zirconia ceramics plastic processing method of DC electric field auxiliary, comprising the following steps:
Step 1: using Y2O3Stablize ZrO2Powder obtains 3YSZ sample after being molded, being sintered；
By commercial high-purity 3mol%Y2O3Stablize ZrO2Bar shaped drawing is made in (3YSZ) powder pressure maintaining 60s under the molding of 60MPa
Stretch sample green compact；By it, pressureless sintering 2h obtains fine and close 3YSZ sample 4 under the conditions of 1550 DEG C.
Respectively on the inside of the circular hole at 4 both ends of sample and for power transmission and conductive ZrO2Coat one layer of platinum in 4 surface of pin
Slurry is to increase electric conductivity；The upper transmission rod 2 and lower transmission rod 3 of 4 both ends circular hole of sample and universal testing machine are inserted by pin 5
Circular hole in realize connection between sample 4 and upper and lower transmission rod；It places it in temperature control heating furnace 1,5 surface of pin is logical
Cross the positive and negative anodes that platinum filament 6 connects DC power supply 7.
Step 2: sample being heated to 600~900 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 30min；
Sample is heated to 600~900 DEG C with the heating rate of 10 DEG C/min by temperature control heating furnace 1, keeps the temperature 30min.
Step 3: under the conditions of 600~900 DEG C of temperature, applying current density at sample both ends is 50~400mA/mm2's
DC electric field stretches sample after keeping 5min, completes plastic processing.
Under the conditions of 600~900 DEG C of temperature, DC power supply 7 is connected, applies a DC electric field, direct current at 4 both ends of sample
Electric field density is 50~400mA/mm2, stablize 5min after current density reaches setting value, by universal testing machine in constant strain
Rate (≤10-1s-1) or constant load (>=1MPa) under the conditions of to 3YSZ carry out plastic processing.
When carrying out plastic processing to zirconia ceramics by the method for the invention, elongation percentage can achieve 450% or more, become
Shape amount still has 98% or more consistency after reaching 200%.
Embodiment 1
Fine and close 3YSZ zirconia ceramics sample is put into temperature control heating furnace 1, is heated to the heating rate of 10 DEG C/min
700 DEG C, 30min is kept the temperature at this temperature, it is ensured that furnace temperature and specimen temperature reach balance；Apply 240mA/mm at 4 both ends of sample2
DC current, stablize 5min after current density reaches setting value, it is ensured that the stabilization of electric current and temperature it is uniform；Pass through ten thousand
Energy testing machine is with 10-3s-1Constant strain rate to sample carry out stretching plastic processing；Guarantee examination in entire plastic processing
Sample constant current density is 240mA/mm2, until plastic processing terminates, 250% elongation percentage can be obtained.
Embodiment 2
Fine and close 3YSZ zirconia ceramics sample is put into temperature control heating furnace 1, is heated to the heating rate of 10 DEG C/min
900 DEG C, 30min is kept the temperature at this temperature, it is ensured that furnace temperature and specimen temperature reach balance；Apply 200mA/mm at 4 both ends of sample2
DC current, stablize 5min after current density reaches setting value, it is ensured that the stabilization of electric current and temperature it is uniform；Pass through ten thousand
Energy testing machine is with 10-2s-1Constant strain rate to sample carry out stretching plastic processing；Guarantee examination in entire plastic processing
Sample constant current density is 200mA/mm2, until plastic processing terminates, 360% elongation percentage can be obtained.
Embodiment 3
Fine and close 3YSZ zirconia ceramics sample is put into temperature control heating furnace 1, is heated to the heating rate of 10 DEG C/min
900 DEG C, 30min is kept the temperature at this temperature, it is ensured that furnace temperature and specimen temperature reach balance；Apply 200mA/mm at 4 both ends of sample2
DC current, stablize 5min after current density reaches setting value, it is ensured that the stabilization of electric current and temperature it is uniform；Pass through ten thousand
Energy testing machine is with 10-3s-1Constant strain rate to sample carry out stretching plastic processing；Guarantee examination in entire plastic processing
Sample constant current density is 200mA/mm2, until plastic processing terminates, 450% elongation percentage can be obtained.
Embodiment 4
Fine and close 3YSZ zirconia ceramics sample is put into temperature control heating furnace 1, is heated to the heating rate of 10 DEG C/min
900 DEG C, 30min is kept the temperature at this temperature, it is ensured that furnace temperature and specimen temperature reach balance；Apply 200mA/mm at 4 both ends of sample2
DC current, stablize 5min after current density reaches setting value, it is ensured that the stabilization of electric current and temperature it is uniform；Pass through ten thousand
Energy testing machine carries out stretching plastic processing to sample with the constant load of 1.5MPa；Guarantee sample electricity in entire plastic processing
Constant current density is 200mA/mm2, until plastic processing terminates, 250% steady state creep strain rate can be obtained.
Embodiment 5
Fine and close 3YSZ zirconia ceramics sample is put into temperature control heating furnace 1, is heated to the heating rate of 10 DEG C/min
900 DEG C, 30min is kept the temperature at this temperature, it is ensured that furnace temperature and specimen temperature reach balance；Apply 200mA/mm at 4 both ends of sample2
DC current, stablize 5min after current density reaches setting value, it is ensured that the stabilization of electric current and temperature it is uniform；Pass through ten thousand
Energy testing machine carries out stretching plastic processing to sample with the constant load of 2.5MPa；Guarantee sample electricity in entire plastic processing
Constant current density is 200mA/mm2, until plastic processing terminates, 170% steady state creep strain rate can be obtained.
Fig. 2 be the embodiment of the present invention in zirconia ceramics plastic processing load-deformation curve, Fig. 3 be strain-when
Half interval contour；It can be seen from the figure that being assisted by DC electric field, the stretching plastic carried out under the conditions of low temperature and high strain rate
In process, flow stress is less than 10MPa, and has obtained very high elongation percentage；Under the conditions of low temperature and low load into
In capable stretching plastic process, sample deformation is stable and secondary creep rates are greater than 10-3s-1, there is very high stable state
Creep rate.
Fig. 4 is the scanning electron microscope in the embodiment of the present invention after zirconia ceramics plastic processing to certain deformation
(SEM) figure；It (a) is the SEM figure of zirconia ceramics plastic processing to 100% in embodiment 4；It (b) is zirconium oxide pottery in embodiment 2
Porcelain carving is machined to 200% SEM figure；It can be seen from the figure that being assisted by DC electric field, in low temperature and quickly stretching modeling
Property processing after, sample internal modification is uniform, does not generate the internal flaws such as stomata and crackle, and sample consistency is high, ensure that material
The intensity of material.
The present invention uses the zirconia ceramics plastic processing method under electric field-assisted, can in a low temperature of 600~900 DEG C
Realize zirconia ceramics with≤10-1s-1Strain rate carry out quick plastic processing, not only greatly reduce needed for provide
Environment temperature also improves processing speed, effectively shortens the process-cycle, is advantageously implemented the highly-efficient processing of zirconia ceramics,
Energy consumption is reduced, production efficiency is improved, reduces production cost；It can significantly be dropped using electro plastic effect and electrothermal effect
Resistance of deformation in inductile process, so that sample homogeneous deformation in process, thus effectively reduce processed
Defect inside sample, elongation percentage can achieve 450% or more, still have 98% or more cause after deflection reaches 200%
Density can guarantee the intensity of material after processing, great industrial application value.
Claims (4)
1. a kind of zirconia ceramics plastic processing method of DC electric field auxiliary, which comprises the following steps:
Step 1: using Y2O3Stablize ZrO2Powder obtains 3YSZ sample after being molded, being sintered；
Step 2: sample being heated to 600~900 DEG C with the heating rate of 10 DEG C/min, keeps the temperature 30min；
Step 3: under the conditions of 600~900 DEG C of temperature, applying current density at sample both ends is 50~400mA/mm2Direct current
, sample is stretched after keeping 5min, completes plastic processing.
2. a kind of zirconia ceramics plastic processing method of DC electric field auxiliary according to claim 1, which is characterized in that
It is less than≤10 in strain rate in the step 3-1s-1Or sample is stretched under the conditions of load >=1MPa.
3. a kind of zirconia ceramics plastic processing method of DC electric field auxiliary according to claim 1, which is characterized in that
It is further comprising the steps of:
A circular hole is respectively set at sample both ends, in circular hole interior surface conductive coating, the circular hole at sample both ends is separately connected directly
Flow power positive cathode.
4. a kind of zirconia ceramics plastic processing method of DC electric field auxiliary according to claim 1, which is characterized in that
Y in the step 12O3Stablize ZrO2Powder keeps 60s to be prepared into sample green compact under the molding of 60MPa, under the conditions of 1550 DEG C
Pressureless sintering 2h obtains fine and close 3YSZ sample.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109932388A (en) * | 2019-04-04 | 2019-06-25 | 西北工业大学 | A kind of Electroplastic fuel factor and non-thermal effect decouple separation method |
| CN111426574A (en) * | 2020-03-25 | 2020-07-17 | 国网河南省电力公司电力科学研究院 | Method and system for testing electro-plastic deformation of converter transformer conductor material |
| CN112051144A (en) * | 2020-08-13 | 2020-12-08 | 北京航空航天大学 | Pure electro-plasticity auxiliary thermal forming process for hard-material-state high-strength aluminum alloy |
| CN114394852A (en) * | 2022-01-06 | 2022-04-26 | 长安大学 | Preparation method of ceramic material with grain size in gradient distribution |
| CN115536437A (en) * | 2022-01-18 | 2022-12-30 | 武汉位错科技有限公司 | High-temperature rolling processing method and processing device and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109932388A (en) * | 2019-04-04 | 2019-06-25 | 西北工业大学 | A kind of Electroplastic fuel factor and non-thermal effect decouple separation method |
| CN111426574A (en) * | 2020-03-25 | 2020-07-17 | 国网河南省电力公司电力科学研究院 | Method and system for testing electro-plastic deformation of converter transformer conductor material |
| CN112051144A (en) * | 2020-08-13 | 2020-12-08 | 北京航空航天大学 | Pure electro-plasticity auxiliary thermal forming process for hard-material-state high-strength aluminum alloy |
| CN114394852A (en) * | 2022-01-06 | 2022-04-26 | 长安大学 | Preparation method of ceramic material with grain size in gradient distribution |
| CN114394852B (en) * | 2022-01-06 | 2022-10-28 | 长安大学 | Preparation method of ceramic material with grain size in gradient distribution |
| CN115536437A (en) * | 2022-01-18 | 2022-12-30 | 武汉位错科技有限公司 | High-temperature rolling processing method and processing device and application thereof |
| CN115536437B (en) * | 2022-01-18 | 2023-09-08 | 武汉位错科技有限公司 | High-temperature rolling processing method, processing device and application thereof |
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