CN108751989B - A kind of zirconia ceramics and its multiple sintering preparation method - Google Patents
A kind of zirconia ceramics and its multiple sintering preparation method Download PDFInfo
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Abstract
The present invention provides a kind of zirconia ceramics and its multiple sintering preparation methods.A kind of multiple sintering preparation method of zirconia ceramics, including the following steps: zirconia ceramics green compact are heated to 1150~1400 DEG C, keep the temperature 0~5min；Then 900~1100 DEG C are cooled to, 3~10h is kept the temperature, completes first sintering；It is repeated as many times the process of the first sintering later, is repeatedly sintered, obtains product.The means that the present invention was repeatedly sintered and was reduced high-temperature temperature using circulation effectively inhibit the abnormal growth of crystal grain, provide the thermodynamic driving force of enough grain boundary decisions, therefore zirconia ceramics crystal grain obtained is thinner, tissue more evenly, consistency it is higher, mechanical performance and water resistant heat aging performance are excellent.
Description
Technical field
The present invention relates to ceramic technology fields, more particularly, to a kind of zirconia ceramics and its multiple sintering preparation method.
Background technique
Zirconia ceramics due to its good biocompatibility, wearability, transformation toughening effect etc. be widely used in dentistry,
Bone implant prosthese etc. especially obtains the extensive concern of researcher in the application of bone implant prosthese industry in recent years.
Currently, yttrium stable zirconium oxide ceramics mostly use pressureless sintering, in order to guarantee ceramic consistency and excellent machinery
Performance, the mode for generalling use high temperature sintering and long-time heat preservation carry out sintering oxidation zircon ceramic.And long-time soak is being protected
Also it can cause the abnormal growth of crystal grain while demonstrate,proving ceramic high-compactness, the direct result of abnormal grain growth is to lead to ceramic machine
Tool performance substantially reduces.In order to improve the performance of zirconia ceramics, consistency can be improved but also inhibit crystal grain different by seeking one kind
The method often grown up is most important.
Two-step sintering method is presently believed to be the effective means for inhibiting crystal grain to grow up while guaranteeing densification.Its original
Reason is: sample being first heated to a higher temperature, isothermal treatment for short time, the thermodynamics for making system obtain enough grain boundary decisions drives
Power, then fast cooling to lower temperature reaches the mesh of densification using grain boundary decision to inhibit the migration of crystal boundary
's.
In terms of two-step sintering prepares zirconia ceramics, (not smoothgoing super, Li Ning etc., two-step sintering makes pottery to dental zirconium oxide to document 1
The influence of porcelain microstructure, West China Journal of Stomatology, 31 (2013) 496-499) use a kind of two-step sintering method: first
Sample is heated to 1450-1550 DEG C, 5min is kept the temperature, so that system is obtained the thermodynamic driving force of enough grain boundary decisions, then quickly
It is reduced to 1250-1350 DEG C, keeps the temperature 300min, crystallite dimension obtained is up to 210-340nm.Two-step sintering is burnt relative to tradition
Knot, density is higher, and crystal grain is thinner, organizes conclusion more evenly.(Zhu Nannan, molding and firing temperature system are to 3Y-TZP for document 2
The research that ceramic structure and performance influence, University Of Ji'nan, 2015) 3Y-TZP ceramics are sintered using two-step sintering method,
Two-step sintering temperature is respectively 1450 DEG C, is down to 1400 DEG C, and bulk density has been made up to 6.04g/cm3Zirconia ceramics.
In the above documents, the temperature that two-step sintering uses has reached 1450 DEG C, although in order to avoid the exception of crystal grain
It grows up, hot stage soaking time is very short, but temperature is so high, the appearance of some still unavoidable abnormal growth crystal grain, from
And influence the mechanical performance of zirconia ceramics.
In view of this, the present invention is specifically proposed.
Summary of the invention
The first object of the present invention is to provide a kind of multiple sintering preparation method of zirconia ceramics, this method reduce
The temperature of soak when sintering, therefore avoid the bad problem of ceramic performance caused by conventional high-temperature is sintered.Of the invention
Second purpose is zirconia ceramics made from the above method, which compares existing product, and crystal grain is thinner, organizes more
Uniformly, consistency is higher, and mechanical performance and water resistant heat aging performance are more excellent.
In order to achieve the goal above, the present invention provides following technical schemes:
A kind of multiple sintering preparation method of zirconia ceramics, including the following steps:
Zirconia ceramics green compact are heated to 1150~1400 DEG C, keep the temperature 0~5min；Then it is cooled to 900~
1100 DEG C, 3~10h is kept the temperature, completes first sintering；
It is repeated as many times the process of the first sintering later, is repeatedly sintered, obtains product.
The characteristics of above method of the present invention is circulation repeatedly sintering, isothermal treatment for short time, therefore can be kept the temperature to avoid high temperature, overlength
Bring adverse effect, such as the problems such as avoid the abnormal growth of crystal grain, so as to improve mechanical performance and the water resistant heat of ceramics
Ageing properties.After tested, the zirconia ceramics crystallite dimension that the present invention obtains is less than 220nm；Four point bending strength is greater than
1100MPa；Bulk density is greater than 6.04g/cm3；After 134 DEG C of hydrothermal aging processing 5h, ceramic surface is without monoclinic phase.
The thermodynamic process that the present invention is repeatedly sintered is main are as follows: zirconia ceramics green compact are risen to 1150~1400 DEG C in short-term
Heat preservation, crystal boundary migration is greater than grain boundary decision rate at this time, grown up with crystal grain based on, crystal grain inner air vent plays pendulum；So
Temperature is quickly down to 900~1100 DEG C afterwards, due to the reduction of sintering activating energy, crystal boundary migration is short of power, crystal grain grow up by
Inhibit, and the thermodynamic driving force gathered at high temperature can then continue to the diffusion of crystal boundary, promote the discharge of stomata, densification
Carried out；After 900~1100 DEG C of heat preservation a period of times, temperature is increased to 1150~1400 DEG C of isothermal treatment for short time again, due to
High temperature sintering temperature of the invention is substantially less than conventional sintering and two-step sintering temperature, therefore the heat preservation of short time will not promote crystal grain
Abnormal growth, and because subsequent high temperature mainly supplement again to system promote grain boundary decision thermodynamic driving force, therefore
Subsequent soak temperature is below the holding temperature of first time high temperature.
To sum up, preparation method of the invention belongs to the sintering means of high/low temperature cycle sintering, but compared with prior art excellent
Gesture is reduction of the high-temperature temperature of sintering, has both been supplied to the driving force of grain boundary decision, and it is excessively high caused in turn avoid high-temperature temperature
The bad problem of performance.
The present invention can select to repeat the number of sintering according to densifying materials degree.
In the present invention, every time sintering when heating after heat preservation can be specific temperature spot, be also possible to range compared with
Small silicon carbide, but need to guarantee within the scope of 1150~1400 DEG C, for example, 1150 DEG C, 1200 DEG C, 1250 DEG C, 1300 DEG C,
1350 DEG C, 1400 DEG C etc..
Equally, the heat preservation to cool down when being sintered every time can be specific temperature spot, be also possible to the lesser area of range
Between temperature, but need to guarantee within the scope of 900~1100 DEG C, such as 900 DEG C, 950 DEG C, 1000 DEG C, 1050 DEG C, 1100 DEG C etc..
The soaking time of heating and cooling arbitrarily determines within the scope of 0~5min, 3~10h respectively.
Preparation method of the invention is not only applicable to common zirconia ceramics, it may also be used for prepares the zirconium oxide pottery of doping
Porcelain, such as the zirconia ceramics of different metal oxides doping.
In addition, the present invention also optimizes other process conditions of sintering, it is specific as follows.
Preferably, the rate of the heating is 2~6 DEG C/min, preferably 2~5 DEG C/min, preferably 3 when each sintering
~5 DEG C/min.
All have an impact through mechanical performance and water resistant heat aging performance of the screening discovery heating rate to ceramics, synthesis is examined
Consider, be advisable with the heating rate of 2~6 DEG C/min, such as 2 DEG C/min, 3 DEG C/min, 4 DEG C/min, 5 DEG C/min, 6 DEG C/min etc.,
Wherein preferred range be 2~5 DEG C/min, 3~5 DEG C/min.
Preferably, every time the sintering when cooling rate be 40~60 DEG C/min, preferably 40~55 DEG C/min, it is excellent
Select 45~50 DEG C/min.
All have an impact through mechanical performance and water resistant heat aging performance of the screening discovery rate of temperature fall to ceramics, synthesis is examined
Consider, be advisable with the rate of temperature fall of 40~60 DEG C/min, such as 40 DEG C/min, 45 DEG C/min, 50 DEG C/min, 55 DEG C/min, 60 DEG C/
Min etc., wherein preferred range is 40~55 DEG C/min, preferably 45~50 DEG C/min.
Preferably, every time the sintering when heating outlet temperature be 1150~1350 DEG C, preferably 1300~1350
℃。
Preferably, every time the sintering when cooling outlet temperature be 1000~1100 DEG C, preferably 1000~1070
℃。
Preferably, the holding temperature after heating up when each sintering is below the heat preservation temperature when sintering for the first time
Degree.
Since subsequent temperature-rise period is to supplement the thermodynamic driving force for promoting grain boundary decision to system, for as far as possible
The abnormal growth of crystal grain is avoided, soaking time when improving mechanical performance, preferably each sintering after heating is less than the last time
Soaking time after heating up when the sintering.
Preferably, the duplicate number is 3 times~10 times.
Preferably, soaking time when each sintering after heating is 0~4min, preferably 1~3min.
Preferably, soaking time when each sintering after cooling is 3~6h, preferably 5~6h.
To sum up, compared with prior art, invention achieves following technical effects:
(1) sintering process reduced using high-temperature temperature, not only solves the process bands such as high temperature sintering, overlength heat preservation sintering
The bad problem of the ceramic performance come, improves product quality, and also save energy consumption；
(2) critical craft has been screened, the mechanical performance and water resistant heat aging performance of product are further improved.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is the grain morphology figure for the ceramics that the embodiment of the present invention 1 provides；
Fig. 2 is the four point bending strength figure for the ceramics that the embodiment of the present invention 1 provides；
Fig. 3 is XRD test chart after the ceramic hydrothermal aging that the embodiment of the present invention 1 provides.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with the drawings and specific embodiments, but
Be it will be understood to those of skill in the art that it is following described embodiments are some of the embodiments of the present invention, rather than it is whole
Embodiment is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.Based on the embodiments of the present invention, ability
Domain those of ordinary skill every other embodiment obtained without making creative work, belongs to guarantor of the present invention
The range of shield.The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions.Agents useful for same
Or production firm person is not specified in instrument, is the conventional products that can be obtained by commercially available purchase.
Embodiment 1
Be 4 DEG C/min by heating rate, in 1350 DEG C of progresss first sinterings, heat preservation 3min, heat preservation terminates, with 50 DEG C/
Min is down to 1050 DEG C, is warming up to 1300 DEG C by 4 DEG C/min after heat preservation 6h and carries out second of sintering, keeps the temperature 3min, and heat preservation terminates,
1050 DEG C are down to 50 DEG C/min, keeps the temperature 6h, heat preservation terminates, and repeats second of sintering process and carries out third, the 4th sintering, obtains
To zirconia ceramics.
Embodiment 2
The difference from embodiment 1 is that the maximum temperature of third time sintering and the 4th sintering reduces, it is specific as follows.
Be 4 DEG C/min by heating rate, in 1350 DEG C of progresss first sinterings, heat preservation 3min, heat preservation terminates, with 50 DEG C/
Min is down to 1050 DEG C, is warming up to 1300 DEG C by 4 DEG C/min after heat preservation 6h and carries out second of sintering, keeps the temperature 3min, and heat preservation terminates,
1050 DEG C are down to 50 DEG C/min, keeps the temperature 6h, and heat preservation terminates, and is down to 1050 DEG C with 50 DEG C/mi, keeps the temperature after 6h according to 4 DEG C/min
1270 DEG C of progress third time sintering are warming up to, 3min is kept the temperature, heat preservation terminates, and is down to 1070 DEG C with 50 DEG C/min, keeps the temperature 6h, repeats
Third step sintering process carries out the sintering of the 4th step, obtains zirconia ceramics.
Embodiment 3
The difference from embodiment 1 is that the maximum temperature of first sintering reduces, it is specific as follows.
3min is kept the temperature, heat preservation terminates, with 50 DEG C/min in 1330 DEG C of progress first sinterings by 4 DEG C/min of heating rate
1070 DEG C are down to, 1300 DEG C is risen to by 4 DEG C/min after heat preservation 6h and carries out second of sintering, keep the temperature 3min, heat preservation terminates, with 50
DEG C/min is down to 1070 DEG C, it keeps the temperature and is warming up to 1300 DEG C of progresss third time sintering according to 4 DEG C/min after 6h, keep the temperature 3min, keep the temperature
Terminate, be down to 1050 DEG C with 50 DEG C/min, keep the temperature 6h, repeats third step sintering process and carry out the sintering of the 4th step, obtain zirconium oxide
Ceramics.
Embodiment 4
Difference with embodiment 3 is that third time is sintered and the maximum temperature of the 4th sintering reduces, specific as follows.
3min is kept the temperature in 1330 DEG C of progress first sinterings by 4 DEG C/min of heating rate, heat preservation terminates, 50 DEG C/min drop
To 1070 DEG C, keep the temperature after 6h to rise to 1300 DEG C by 4 DEG C/min and carry out second and be sintered, heat preservation 3min, heat preservation terminates, with 50 DEG C/
Min is down to 1050 DEG C, keeps the temperature and is warming up to 1270 DEG C of progresss third time sintering according to 4 DEG C/min after 6h, keeps the temperature 3min, heat preservation is tied
Beam is down to 1050 DEG C with 50 DEG C/min, keeps the temperature 6h, repeats third step sintering process and carries out the sintering of the 4th step, obtains zirconium oxide pottery
Porcelain.
Embodiment 5
Difference with embodiment 4 is to be sintered the minimum temperature reduction after cooling every time, specific as follows.
3min is kept the temperature, heat preservation terminates, with 50 DEG C/min in 1330 DEG C of progress first sinterings by 4 DEG C/min of heating rate
1020 DEG C are down to, 1300 DEG C is risen to by 4 DEG C/min after heat preservation 6h and carries out second of sintering, keep the temperature 3min, heat preservation terminates, with 50
DEG C/min is down to 1020 DEG C, it keeps the temperature and is warming up to 1270 DEG C of progresss third time sintering according to 4 DEG C/min after 6h, keep the temperature 3min, keep the temperature
Terminate, be down to 1000 DEG C with 50 DEG C/min, keep the temperature 6h, repeats third step sintering process and carry out the sintering of the four, the 5th steps, obtain oxygen
Change zircon ceramic.
Embodiment 6
The difference from embodiment 1 is that the heating rate being sintered every time is different.
Be 2 DEG C/min by heating rate, in 1350 DEG C of progresss first sinterings, heat preservation 3min, heat preservation terminates, with 50 DEG C/
Min is down to 1050 DEG C, is warming up to 1300 DEG C by 2 DEG C/min after heat preservation 6h and carries out second of sintering, keeps the temperature 3min, and heat preservation terminates,
1050 DEG C are down to 50 DEG C/min, keeps the temperature 6h, heat preservation terminates, and repeats second of sintering process and carries out third, the 4th sintering, obtains
To zirconia ceramics.
Embodiment 7
The difference from embodiment 1 is that the heating rate being sintered every time is different.
Be 6 DEG C/min by heating rate, in 1350 DEG C of progresss first sinterings, heat preservation 3min, heat preservation terminates, with 50 DEG C/
Min is down to 1050 DEG C, is warming up to 1300 DEG C by 6 DEG C/min after heat preservation 6h and carries out second of sintering, keeps the temperature 3min, and heat preservation terminates,
1050 DEG C are down to 50 DEG C/min, keeps the temperature 6h, heat preservation terminates, and repeats second of sintering process and carries out third, the 4th sintering, obtains
To zirconia ceramics.
Embodiment 8
The difference from embodiment 1 is that the rate of temperature fall being sintered every time is different.
Be 4 DEG C/min by heating rate, in 1350 DEG C of progresss first sinterings, heat preservation 3min, heat preservation terminates, with 40 DEG C/
Min is down to 1050 DEG C, is warming up to 1300 DEG C by 4 DEG C/min after heat preservation 6h and carries out second of sintering, keeps the temperature 3min, and heat preservation terminates,
1050 DEG C are down to 40 DEG C/min, keeps the temperature 6h, heat preservation terminates, and repeats second of sintering process and carries out third, the 4th sintering, obtains
To zirconia ceramics.
Embodiment 9
The difference from embodiment 1 is that the rate of temperature fall being sintered every time is different.
Be 4 DEG C/min by heating rate, in 1350 DEG C of progresss first sinterings, heat preservation 3min, heat preservation terminates, with 60 DEG C/
Min is down to 1050 DEG C, is warming up to 1300 DEG C by 4 DEG C/min after heat preservation 6h and carries out second of sintering, keeps the temperature 3min, and heat preservation terminates,
1050 DEG C are down to 60 DEG C/min, keeps the temperature 6h, heat preservation terminates, and repeats second of sintering process and carries out third, the 4th sintering, obtains
To zirconia ceramics.
Embodiment 10
The difference from embodiment 1 is that the maximum temperature after first sintering heating is 1400 DEG C.
Be 4 DEG C/min by heating rate, in 1400 DEG C of progresss first sinterings, heat preservation 3min, heat preservation terminates, with 50 DEG C/
Min is down to 1050 DEG C, is warming up to 1300 DEG C by 4 DEG C/min after heat preservation 6h and carries out second of sintering, keeps the temperature 3min, and heat preservation terminates,
1050 DEG C are down to 50 DEG C/min, keeps the temperature 6h, heat preservation terminates, and repeats second of sintering process and carries out third, the 4th sintering, obtains
To zirconia ceramics.
Embodiment 11
Difference with embodiment 5 is that the minimum temperature after the last cooling of sintering three times reduces, specific as follows.
3min is kept the temperature, heat preservation terminates, with 50 DEG C/min in 1330 DEG C of progress first sinterings by 4 DEG C/min of heating rate
1020 DEG C are down to, 1300 DEG C is risen to by 4 DEG C/min after heat preservation 6h and carries out second of sintering, keep the temperature 3min, heat preservation terminates, with 50
DEG C/min is down to 1020 DEG C, it keeps the temperature and is warming up to 1270 DEG C of progresss third time sintering according to 4 DEG C/min after 6h, keep the temperature 3min, keep the temperature
Terminate, be down to 900 DEG C with 50 DEG C/min, keep the temperature 6h, repeats third step sintering process and carry out the sintering of the four, the 5th steps, obtain oxygen
Change zircon ceramic.
Ceramic performance made from above-described embodiment is as shown in table 1.
The performance of 1 ceramics of table
In addition, the present invention has also listed the electron microscope of the gained ceramics of embodiment 1, as shown in Figure 1, four point bending strength is such as
Shown in Fig. 2, XRD test is as shown in Figure 3 after 134 DEG C of hydrothermal aging processing 5h.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (15)
1. a kind of multiple sintering preparation method of zirconia ceramics, characterized in that it comprises the following steps:
Zirconia ceramics green compact are heated to 1150~1400 DEG C, keep the temperature 0~5min；Then 900~1100 DEG C are cooled to,
3~10h is kept the temperature, first sintering is completed；
It is repeated as many times the process of the first sintering later, is repeatedly sintered, obtains product；
The rate of the heating is 2~6 DEG C/min when each sintering；
The rate of the cooling is 40~60 DEG C/min when each sintering；
Holding temperature when each sintering after heating is below the holding temperature when sintering for the first time.
2. multiple sintering preparation method according to claim 1, which is characterized in that heating when each sintering
Rate is 2~5 DEG C/min.
3. multiple sintering preparation method according to claim 2, which is characterized in that heating when each sintering
Rate is 3~5 DEG C/min.
4. multiple sintering preparation method according to claim 1, which is characterized in that cooling when each sintering
Rate is 40~55 DEG C/min.
5. multiple sintering preparation method according to claim 4, which is characterized in that cooling when each sintering
Rate is 45~50 DEG C/min.
6. multiple sintering preparation method according to claim 1, which is characterized in that heating when each sintering
Outlet temperature is 1150-1350 DEG C.
7. multiple sintering preparation method according to claim 6, which is characterized in that heating when each sintering
Outlet temperature is 1300-1350 DEG C.
8. multiple sintering preparation method according to claim 1, which is characterized in that cooling when each sintering
Outlet temperature is 1000~1100 DEG C.
9. multiple sintering preparation method according to claim 8, which is characterized in that cooling when each sintering
Outlet temperature is 1000~1070 DEG C.
10. multiple sintering preparation method according to claim 1, which is characterized in that the duplicate number is 3 times~10
It is secondary.
11. multiple sintering preparation method according to claim 1, which is characterized in that when each sintering after heating
Soaking time is 1~4min.
12. multiple sintering preparation method according to claim 11, which is characterized in that when each sintering after heating
Soaking time is 1~3min.
13. multiple sintering preparation method according to claim 1, which is characterized in that when each sintering after cooling
Soaking time is 3~6h.
14. multiple sintering preparation method according to claim 1, which is characterized in that when each sintering after cooling
Soaking time is 5~6h.
15. a kind of zirconia ceramics, which is characterized in that use the described in any item multiple sintering preparation methods of claim 1-14
It is made.
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