CN107827458A - A kind of technique for preparing zirconia ceramics using oscillation pressure sintering process - Google Patents
A kind of technique for preparing zirconia ceramics using oscillation pressure sintering process Download PDFInfo
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Abstract
The invention discloses a kind of technique that zirconia ceramics is prepared using oscillation pressure sintering process, its step is：A, Zirconium powder loads；B, protective gas is filled with after vacuumize process；C, apply precompression and be warming up to 800 DEG C with 100 DEG C/h heating rates；D, 30min is incubated for the first time；E, increase pressure is warming up to 1000 DEG C to 15MPa, while with 100 DEG C/h heating rate；F, second of insulation 30min；G, increase pressure is warming up to 1400 DEG C to 30MPa and with 50 DEG C/h heating rate；H, third time insulation 15min；I, apply oscillation pressure, and carry out the 4th insulation 45min；J, cooled with 100 DEG C/min rate of temperature fall and cool to 900 DEG C；K, pressure release and room temperature is naturally cooled to stove.The present invention can effectively suppress grain growth and promote grain boundaries to hold one's breath hole discharge, and prepared zirconia ceramics consistency and hardness are high.
Description
Technical field
The present invention relates to zirconia ceramics preparing technical field, more particularly to one kind to prepare oxygen using oscillation pressure sintering process
The technique for changing zircon ceramic.
Background technology
Conventional pressure sintering method is the method for improving powder sintering performance by applying pressure, and it mainly has hot pressing burning
Three kinds of knot, HIP sintering, discharge plasma sintering methods.Wherein, for hot-pressing sintering method, it refers to sintering
While unidirectional or two-way pressure is applied to powder, the scope of pressure can be from tens MPa to several GPa；Hot pressing at present
The pressure of sintering gradually steps up, when pressure is more than 1GPa, also known as super-pressure hot pressed sintering；Due to applying during hot pressed sintering
Higher pressure, the densification of powder can be effectively facilitated and suppress crystal grain and grown up, hot-pressing sintering method is by widely at present
Applied to ceramics, hard alloy, intermetallic compound and composite etc..For HIP sintering method, it is
Powder all directions are applied with equal pressure with inert gas, liquid or solid media in sintering, can preferably be disappeared
Except the hole in powder and suppress grain growth.For discharge plasma sintering method, it is a kind of quick, energy-conservation, ring
The material processing technology of preparing of guarantor, under distinctive electric field, stress field, temperature field action, realize various structures and performance green wood
The sintering of material；During activated sintering on the scene, broken and particle the rearrangement being applied with beneficial to reunion powder of stress, it is possible to reduce group
The a large amount of defects and stomata that aggressiveness introduces after sintering, and then obtain fine and close material；In the final stage of sintering, pressure energy promotees
Enter Plastic Flow and diffusion creep, improve the consistency of field activating sintered material, and as the increase for applying load, pressure energy carry
Height sintering driving force, advantageously reduces final sintering temperature.
Specifically, the deformation of powder is carried out under being acted on while stress and temperature during pressure sintering, thing
Matter migration can by dislocation movement by slip, climb, spread, the number of mechanisms such as diffusion creep is completed.
Above-mentioned three kinds of pressure sintering processes can substantially reduce the sintering temperature of system, shorten the sintered heat insulating time and reduce
Or without using sintering aid, while grain coarsening can also be suppressed and promote blank Densification, therefore prepared ceramic structure
Part has higher mechanical property and reliability.However, the limitation of hydraulic system causes what above-mentioned sintering method was applied at present
Pressure is all static pressure, shows as pressure value constant at pressure head；The limitation of constant pressure mainly shows in pressure sintering
：1st, before sintering starts, constant pressure can not fully realize particle re-arrangement and particle agglomeration can not abundant depolymerization；2nd, sinter
In the later stage, the residual of grain boundaries hole of holding one's breath can not effectively exclude under constant pressure, and hole of holding one's breath is limit structural Mechanical Property of Ceramics
An important factor for.
It should further be noted that when pressure sintering technology to be used for the sintering of nano ceramics, it was found that many new limitations,
Generally existing " threshold value " when nano ceramics sinters, i.e., pressure have to be larger than certain value and could promote ceramic dense at a certain temperature
Change, and the effect less than this numerical pressure can be ignored；Research shows that threshold value is relevant with crystallite dimension, and crystal grain is smaller,
Threshold value is bigger.In nano ceramics sintering process, it is difficult to effectively crush due to soft-agglomerated, in sintering process inside aggregate first
It is densified, tension force is produced between matrix, causes the appearance of crackle shape gross blow hole；Simultaneously because of the limitation of graphite jig, outside
Pressure is not enough to overcome threshold value caused by plastic flow, therefore gross blow hole can not crush, and makes the sintered density of material less than identical
At a temperature of pressureless sintering material.So to improve the sintered density of nano material, generally set about in terms of following two：One
It is to improve initial pressure, it is soft-agglomerated in powder thoroughly to crush；Second, the external pressure in sintering is improved, to promote plastic flow
Progress.But pressure sintering generally use graphite jig at present, and the stress that graphite jig can bear is limited, further
It is relatively difficult to improve external pressure.In a word, current constant pressure agglomerating plant there is no method to give full play to pressure factor and ceramics burnt
The effect of densification and grain growth during knot.
Except crystallite dimension and shape, the consistency of material is also to determine the important parameter of its mechanical property；In ceramic material
To expect in sintering process, the remnants of grain boundaries hole of holding one's breath often is difficult to discharge, therefore ceramic material can not realize complete densification, and
The hold one's breath negative effects in hole of remnants are mainly shown as：1st, the strength of materials is reduced as stress concentration point；2nd, as in light scattering
The heart and the consistency for reducing material；3rd, hinder domain wall motion and influence the ferroelectricity and magnetic of material.Prepared in polycrystalline ceramics
Cheng Zhong, stomata are present in the links of flow, and it is initially present between biscuit particle, are by between particle during original powder briquetting
Hole leave；Initial stage of sintering, when interface curvature and higher interfacial migration driving force, crystal boundary is transported with higher speed
Dynamic, stomata can not often rest on grain boundaries and enter intra-die, therefore be able to observe that in many crystal grain spilehole be present；
Grown up with the carry out crystal grain of sintering, the curvature of crystal boundary and the driving force of grain boundary are gradually reduced, then the stomata in base substrate
Crystal boundary generally can be arrived at and moved with crystal boundary, and gradually gathered on crystal grain corner, such as trident crystal boundary or four fork crystal boundaries；
For this part holes, common pressure sintering processes are often difficult to exclude.
The content of the invention
The purpose of the present invention is to solve the shortcomings of the prior art and one kind is provided and prepares oxygen using oscillation pressure sintering process
The technique for changing zircon ceramic, the technique that zirconia ceramics is prepared using oscillation pressure sintering process can effectively produce preparation oxidation
Zircon ceramic, and can effectively suppress grain growth and by crystallite dimension control in narrower size section by applying oscillation pressure
It is interior, additionally it is possible to effectively facilitate grain boundaries and hold one's breath the discharge in hole, and the prepared zirconia ceramics consistency formed is high, hardness is high.
To reach above-mentioned purpose, the present invention is achieved through the following technical solutions.
A kind of technique that zirconia ceramics is prepared using oscillation pressure sintering process, includes following processing step, specifically：
A, Zirconium powder is loaded in the graphite jig to sintering furnace, graphite jig loads zirconia powder by charging aperture
Body, the charging aperture of graphite jig are that the inner diameter values of circular port and charging aperture are 50mm；
B, after zirconium powder body to be oxidized loads, the bell of sintering furnace is closed, then by vavuum pump first to the inner chamber of sintering furnace
Vacuumize process is carried out, the inner chamber after vacuumizing toward sintering furnace is filled with protective gas；
C, the precompression of constant pressure is applied for Zirconium powder by pressure head, the pressure value of precompression is 5MPa, is opened simultaneously
The heater of dynamic sintering furnace is heated, slowly heating and 100 DEG C/h of heating rate；
D, when the temperature value for sintering furnace chamber reaches 800 DEG C, carry out first time insulation and be incubated 30min, to exclude zirconium oxide
Contained organic matter in powder；
E, after insulation terminates after first time, increase pressure head to the pressure of Zirconium powder and cause pressure of the pressure head to Zirconium powder
Power increases to 15MPa, while continues to heat with 100 DEG C/h heating rate, until the temperature of sintering furnace chamber is warming up to
1000℃；
F, when the temperature value for sintering furnace chamber reaches 1000 DEG C, it is 30min to carry out second of insulation and soaking time；
G, after second of insulation terminates, increase pressure head to the pressure of Zirconium powder and cause pressure of the pressure head to Zirconium powder
Power increases to 30MPa, while continues to heat with 50 DEG C/h heating rate, until the temperature of sintering furnace chamber is warming up to
1400℃；
H, when the temperature value for sintering furnace chamber reaches 1400 DEG C, it is 15min to carry out third time insulation and soaking time；
I, after third time insulation terminates, in the case where keeping pressure head to be 30MPa to the pressure of Zirconium powder, pressure head is applied
Add oscillation pressure, the oscillation pressure couples with above-mentioned 30MPa and collective effect is in Zirconium powder；Applying the mistake of oscillation pressure
Cheng Zhong, it is 45min to carry out the 4th insulation and soaking time；
J, after the 4th insulation terminates, sintering furnace chamber starts to be cooled with 100 DEG C/min rate of temperature fall, until cooling to
900℃；
K, when the inner chamber of sintering furnace is cooled to 900 DEG C, slow pressure release is started gradually to reduce pressure of the pressure head to zirconia ceramics
Power, and zirconia ceramics is kept into the inner chamber with sintering furnace and naturally cools to room temperature with stove.
Wherein, the protective gas is argon gas.
Wherein, load by Zirconium powder to before graphite jig, stabilizer is added in Zirconium powder, stabilizer is
Yttrium oxide powder, the addition of yttrium oxide powder are 3mol.%, and Zirconium powder be well mixed with yttrium oxide powder after filling out
It is filled in graphite jig.
Wherein, the average grain diameter D50 of the Zirconium powder is 0.08 μm, and the specific surface area of Zirconium powder is less than
10m2/g。
Beneficial effects of the present invention are：It is of the present invention a kind of to prepare zirconia ceramics using oscillation pressure sintering process
Technique, it includes following processing step, specifically：A, Zirconium powder is loaded in the graphite jig to sintering furnace, stone
Black mould loads Zirconium powder by charging aperture, and the charging aperture of graphite jig is that the inner diameter values of circular port and charging aperture are
50mm；B, after zirconium powder body to be oxidized loads, the bell of sintering furnace is closed, then by vavuum pump first to the inner chamber of sintering furnace
Vacuumize process is carried out, the inner chamber after vacuumizing toward sintering furnace is filled with protective gas；C, by pressure head to Zirconium powder
The precompression of constant pressure is applied for, the pressure value of precompression is 5MPa, while the heater for starting sintering furnace is heated,
Slowly heating and 100 DEG C/h of heating rate；D, when the temperature value for sintering furnace chamber reaches 800 DEG C, insulation for the first time is carried out simultaneously
30min is incubated, to exclude organic matter contained in Zirconium powder；E, after after first time, insulation terminates, increase pressure head is to oxygen
Change the pressure of zirconium powder body and cause pressure head to increase to 15MPa to the pressure of Zirconium powder, while with 100 DEG C/h heating rate
Continue to heat, until the temperature of sintering furnace chamber is warming up to 1000 DEG C；F, when the temperature value of sintering furnace chamber reaches 1000
DEG C when, it is 30min to carry out second insulation and soaking time；G, after second of insulation terminates, increase pressure head is to zirconia powder
The pressure of body simultaneously causes pressure head to increase to 30MPa to the pressure of Zirconium powder, at the same with 50 DEG C/h heating rate continue into
Row heating, until the temperature of sintering furnace chamber is warming up to 1400 DEG C；H, when the temperature value for sintering furnace chamber reaches 1400 DEG C, enter
Row third time is incubated and soaking time is 15min；I, after third time insulation terminates, pressure of the pressure head to Zirconium powder is being kept
In the case that power is 30MPa, apply oscillation pressure to pressure head, the oscillation pressure couples with above-mentioned 30MPa and collective effect is in oxygen
Change zirconium powder body；During oscillation pressure is applied, it is 45min to carry out the 4th insulation and soaking time；J, the 4th insulation is treated
After end, sintering furnace chamber starts to be cooled with 100 DEG C/min rate of temperature fall, until cooling to 900 DEG C；K, sintering furnace is worked as
Inner chamber when being cooled to 900 DEG C, start slow pressure release gradually to reduce pressure of the pressure head to zirconia ceramics, and zirconium oxide is made pottery
Porcelain keeps the inner chamber with sintering furnace and naturally cools to room temperature with stove.Designed by above-mentioned processing step, the present invention can be effective
Ground production prepares zirconia ceramics, and can effectively suppress grain growth and control crystallite dimension to exist by applying oscillation pressure
In narrower size section, additionally it is possible to effectively facilitate grain boundaries and hold one's breath the discharge in hole, and the prepared zirconia ceramics formed causes
Density is high, hardness is high.
Brief description of the drawings
Next below in conjunction with the accompanying drawings the present invention will be described, but the embodiment in accompanying drawing does not form the limit to the present invention
System.
Fig. 1 is that oscillation pressure couples schematic diagram.
Fig. 2 is the micro-structure diagram of the zirconia ceramics prepared by the present invention.
Embodiment
With reference to specific embodiment, the present invention will be described.
A kind of technique that zirconia ceramics is prepared using oscillation pressure sintering process, includes following processing step, specifically：
A, Zirconium powder is loaded in the graphite jig to sintering furnace, graphite jig loads zirconia powder by charging aperture
Body, the charging aperture of graphite jig are that the inner diameter values of circular port and charging aperture are 50mm；
B, after zirconium powder body to be oxidized loads, the bell of sintering furnace is closed, then by vavuum pump first to the inner chamber of sintering furnace
Vacuumize process is carried out, the inner chamber after vacuumizing toward sintering furnace is filled with protective gas；
C, the precompression of constant pressure is applied for Zirconium powder by pressure head, the pressure value of precompression is 5MPa, is opened simultaneously
The heater of dynamic sintering furnace is heated, slowly heating and 100 DEG C/h of heating rate；
D, when the temperature value for sintering furnace chamber reaches 800 DEG C, carry out first time insulation and be incubated 30min, to exclude zirconium oxide
Contained organic matter in powder；
E, after insulation terminates after first time, increase pressure head to the pressure of Zirconium powder and cause pressure of the pressure head to Zirconium powder
Power increases to 15MPa, while continues to heat with 100 DEG C/h heating rate, until the temperature of sintering furnace chamber is warming up to
1000℃；
F, when the temperature value for sintering furnace chamber reaches 1000 DEG C, it is 30min to carry out second of insulation and soaking time；
G, after second of insulation terminates, increase pressure head to the pressure of Zirconium powder and cause pressure of the pressure head to Zirconium powder
Power increases to 30MPa, while continues to heat with 50 DEG C/h heating rate, until the temperature of sintering furnace chamber is warming up to
1400℃；
H, when the temperature value for sintering furnace chamber reaches 1400 DEG C, it is 15min to carry out third time insulation and soaking time；
I, after third time insulation terminates, in the case where keeping pressure head to be 30MPa to the pressure of Zirconium powder, pressure head is applied
Add oscillation pressure（As shown in Figure 2）, the oscillation pressure couples with above-mentioned 30MPa and collective effect is in Zirconium powder；Applying
During oscillation pressure, it is 45min to carry out the 4th insulation and soaking time；
J, after the 4th insulation terminates, sintering furnace chamber starts to be cooled with 100 DEG C/min rate of temperature fall, until cooling to
900℃；
K, when the inner chamber of sintering furnace is cooled to 900 DEG C, slow pressure release is started gradually to reduce pressure of the pressure head to zirconia ceramics
Power, and zirconia ceramics is kept into the inner chamber with sintering furnace and naturally cools to room temperature with stove.
It should further be noted that protective gas is argon gas.
It is emphasized that loading by Zirconium powder to before graphite jig, stabilizer is added in Zirconium powder, surely
It is yttrium oxide powder to determine agent, and the addition of yttrium oxide powder is 3mol.%, and Zirconium powder is well mixed with yttrium oxide powder
Loading afterwards to graphite jig.
Also it is exactly that the average grain diameter D50 of Zirconium powder is 0.08 μm, and the specific surface area of Zirconium powder is less than
10m2/g。
Designed by above-mentioned processing step, the present invention effectively production can prepare zirconia ceramics, and be shaken by applying
Grain growth can effectively be suppressed and by crystallite dimension control in narrower size section by swinging pressure, additionally it is possible to effectively facilitate crystalline substance
Held one's breath at boundary the discharge in hole, and the prepared zirconia ceramics consistency formed is high, hardness is high.
Above content is only presently preferred embodiments of the present invention, for one of ordinary skill in the art, according to the present invention's
Thought, there will be changes, this specification content should not be construed as to the present invention in specific embodiments and applications
Limitation.
Claims (4)
1. a kind of technique for preparing zirconia ceramics using oscillation pressure sintering process, it is characterised in that include following technique step
Suddenly, specifically：
A, Zirconium powder is loaded in the graphite jig to sintering furnace, graphite jig loads zirconia powder by charging aperture
Body, the charging aperture of graphite jig are that the inner diameter values of circular port and charging aperture are 50mm；
B, after zirconium powder body to be oxidized loads, the bell of sintering furnace is closed, then by vavuum pump first to the inner chamber of sintering furnace
Vacuumize process is carried out, the inner chamber after vacuumizing toward sintering furnace is filled with protective gas；
C, the precompression of constant pressure is applied for Zirconium powder by pressure head, the pressure value of precompression is 5MPa, is opened simultaneously
The heater of dynamic sintering furnace is heated, slowly heating and 100 DEG C/h of heating rate；
D, when the temperature value for sintering furnace chamber reaches 800 DEG C, carry out first time insulation and be incubated 30min, to exclude zirconium oxide
Contained organic matter in powder；
E, after insulation terminates after first time, increase pressure head to the pressure of Zirconium powder and cause pressure of the pressure head to Zirconium powder
Power increases to 15MPa, while continues to heat with 100 DEG C/h heating rate, until the temperature of sintering furnace chamber is warming up to
1000℃；
F, when the temperature value for sintering furnace chamber reaches 1000 DEG C, it is 30min to carry out second of insulation and soaking time；
G, after second of insulation terminates, increase pressure head to the pressure of Zirconium powder and cause pressure of the pressure head to Zirconium powder
Power increases to 30MPa, while continues to heat with 50 DEG C/h heating rate, until the temperature of sintering furnace chamber is warming up to
1400℃；
H, when the temperature value for sintering furnace chamber reaches 1400 DEG C, it is 15min to carry out third time insulation and soaking time；
I, after third time insulation terminates, in the case where keeping pressure head to be 30MPa to the pressure of Zirconium powder, pressure head is applied
Add oscillation pressure, the oscillation pressure couples with above-mentioned 30MPa and collective effect is in Zirconium powder；Applying the mistake of oscillation pressure
Cheng Zhong, it is 45min to carry out the 4th insulation and soaking time；
J, after the 4th insulation terminates, sintering furnace chamber starts to be cooled with 100 DEG C/min rate of temperature fall, until cooling to
900℃；
K, when the inner chamber of sintering furnace is cooled to 900 DEG C, slow pressure release is started gradually to reduce pressure of the pressure head to zirconia ceramics
Power, and zirconia ceramics is kept into the inner chamber with sintering furnace and naturally cools to room temperature with stove.
2. a kind of technique that zirconia ceramics is prepared using oscillation pressure sintering process according to claim 1, its feature are existed
In：The protective gas is argon gas.
3. a kind of technique that zirconia ceramics is prepared using oscillation pressure sintering process according to claim 1, its feature are existed
In：Load by Zirconium powder to before graphite jig, stabilizer is added in Zirconium powder, stabilizer is oxidation yttrium powder
End, the addition of yttrium oxide powder are 3mol.%, and Zirconium powder be well mixed with yttrium oxide powder after loading to graphite
In mould.
4. a kind of technique that zirconia ceramics is prepared using oscillation pressure sintering process according to claim 1, its feature are existed
In：The average grain diameter D50 of the Zirconium powder is 0.08 μm, and the specific surface area of Zirconium powder is less than 10m2/g。
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