CN109678500A - Yttrium stable zirconium oxide ceramic powders and its preparation method and application - Google Patents
Yttrium stable zirconium oxide ceramic powders and its preparation method and application Download PDFInfo
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Abstract
The present invention provides a kind of yttrium stable zirconium oxide ceramic powders and its preparation method and application, belong to ceramic field.Yttrium stable zirconium oxide ceramic powders, with molar percent, comprising: yttrium oxide 4-9%, zirconium oxide 89-94% and aluminium oxide 1-3%.The preparation method of yttrium stable zirconium oxide ceramic powders: zirconium oxychloride is dissolved with water, and sodium sulphate or ammonium sulfate is added, has been warming up to solid precipitation, is then cooled down, is filtered to obtain zirconium sulfate；Yttrium oxide is dissolved in hydrochloric acid solution, yttrium chloride solution is obtained；Zirconium sulfate is dissolved with water, is mixed with yttrium chloride solution, it is 10-13.1 that aqueous slkali and control system final pH, which is added dropwise, in program, is filtered, washed to obtain sediment；Dry, calcining, is added water and aluminium oxide ball milling, is spray-dried to obtain product.The application of the yttrium stable zirconium oxide ceramic powders, for manufacturing artificial tooth.The yttrium stable zirconium oxide ceramic powders that itself please be provided, crystallinity is high, performance is stable, easy-sintering.
Description
Technical field
The present invention relates to ceramic fields, in particular to a kind of yttrium stable zirconium oxide ceramic powders and preparation method thereof
And application.
Background technique
Pure zirconium oxide is monocline crystal phase at room temperature, and temperature can be transformed into tetragonal phase when rising to about 1173 DEG C, on
It is then converted into cubic phase when rising to 2370 DEG C, becomes liquid phase in 2690 DEG C.When due to pure zirconia from High-temperature cooling to low temperature,
It is converted into monoclinic crystal from quadratic crystal, violent variation occurs for volume, and the later period is caused to pass through when manufacturing other products using it
Even crack is often cracked, industry manufacture is not met and requires.It is mutually stable as adulterating that oxide is added in sterling zirconium oxide
The temperature range that zirconium dioxide is stabilized with cubic crystal can be significantly increased in agent.Yttrium oxide is that common doping is mutually stable
Agent, but single addition yttrium oxide still has that crystallinity is not high, partial size is excessive, properties of product are unstable, sintering condition is severe
The problems such as quarter.
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 yttrium stable zirconium oxide ceramic powders, and crystallinity is high, partial size is small, performance
Stablize, easy-sintering.
The second object of the present invention is to provide a kind of preparation method of yttrium stable zirconium oxide ceramic powders, easy to operate,
Industrialization production at low cost, easy to accomplish.
The third object of the present invention is to provide a kind of application of yttrium stable zirconium oxide ceramic powders, for manufacturing artificial tooth.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
A kind of yttrium stable zirconium oxide ceramic powders, with molar percent, comprising:
Yttrium oxide 4-9%, zirconium oxide 89-94% and aluminium oxide 1-3%.
Yttrium oxide and aluminium oxide are doped in zirconium oxide simultaneously, help to solve to ask existing for simple doped yttrium oxide
Topic.
Preferably, the yttrium stable zirconium oxide ceramic powders, with molar percent, further includes: silicon carbide 0.01-
0.03% and praseodymium neodymium oxide 0.05-0.1%；Preferably, the partial size of the silicon carbide is 100-200 nanometers, the praseodymium neodymium oxide
Partial size be 50-100 nanometers.
The purpose for adding silicon carbide and praseodymium neodymium oxide is to further increase the sintering character of powder and increase titanium dioxide
The temperature range that zirconium is stabilized with cubic crystal reduces later period production difficulty.Restriction to its partial size is to improve powder
The toughness of material in use, expands its use scope.
Optionally, the partial size of the yttrium stable zirconium oxide ceramic powders is 50-200 nanometers.
The partial size for controlling yttrium stable zirconium oxide ceramic powders is that sintering character in order to advanced optimize product and performance are steady
It is qualitative.
A kind of preparation method of the yttrium stable zirconium oxide ceramic powders, comprising the following steps:
Zirconium oxychloride is dissolved with water, sodium sulphate or ammonium sulfate is then added, has been warming up to solid precipitation, it is then cold
But, zirconium sulfate is obtained by filtration；
Yttrium oxide is dissolved in hydrochloric acid solution, yttrium chloride solution is obtained；
The zirconium sulfate is dissolved with water, is then mixed with the yttrium chloride solution, aqueous slkali and control volume is added dropwise in program
Be final pH be 10-13.1, be filtered, washed to obtain sediment；
By the drying precipitate, calcining, then it is proportionally added into water and the aluminium oxide carries out ball milling and obtains slurry, institute
It states slurry and is dried to obtain the yttrium stable zirconium oxide ceramic powders by spraying.
Method by the way that aqueous slkali is added in zirconium sulfate and yttrium chloride solution and controls final pH, it is steady can to obtain common ecological
The zirconium hydroxide determine, being reasonably distributed and yttrium hydroxide mixed precipitation are finally tied using calcining, aluminium oxide mixing and ball milling
Brilliant degree is high, performance is stable, easy-sintering yttrium stable zirconium oxide ceramic powders.
Preferably, aqueous slkali is added dropwise in described program are as follows:
First stage control system temperature is 30-50 DEG C, the aqueous slkali is added dropwise, system pH is made to reach 8, then stir
30-60 minutes；
Second stage control system temperature is 60-70 DEG C, the aqueous slkali is added dropwise, system pH is made to reach 9, then stir
10-30 minutes；
Phase III control system temperature is 75-78 DEG C, and the aqueous slkali is added dropwise to terminal, is then stirred 5-15 minutes.
Temperature, pH and the mixing time of system are three factors for influencing precipitating and generating, and wherein temperature and pH are two cores
Heart factor, for controlling the formation speed of precipitating and the commensalism of two kinds of precipitatings.Early period is because of material concentration height, formation speed
Fastly, so control system is needed to be under low temperature, mild alkaline conditions；With the progress of reaction, zirconium ion and ruthenium ion are dense in system
Degree reduces, then needs to provide higher temperature and more hydroxyls are reacted.Whole purpose is the reaction speed so that system
The process that rate, precipitating generate is more uniform, speed is moderate, so that the generation state of yttrium hydroxide and precipitated zirconium hydroxide can
It controls and obtains more excellent performance of doping phase zircite towards after being conducive to calcining.
Preferably, the temperature of the drying is 80-120 DEG C.
The control of drying temperature mainly has following several purposes: first, rate of drying is controlled, so that production efficiency is maintained at
In tolerance interval；Second, it avoids that the interaction and life between zirconium hydroxide and yttrium hydroxide just occurs in drying stage
At the reaction of zirconium oxide and yttrium oxide, the dry adverse effect calcined to the later period is reduced.
Preferably, the process of the calcining are as follows: initial phase is warming up to 1000-1050 DEG C in 30-60 minutes, then keeps the temperature
10-30 minutes, then in quenching in 3-5 minutes to 300-350 DEG C；Intermediate stage, 5-10 DEG C/min of heating rate of control are warming up to
1200-1300 DEG C, keep the temperature 30-50 minutes；Cooling stage, 10-15 DEG C/min of cooling rate of control are cooled to 1110 DEG C, then
1-5 DEG C/min of cooling rate of control is cooled to 1090 DEG C, then controls 10-20 DEG C/min of cooling rate and be cooled to 500-800 DEG C,
It finally controls 30-50 DEG C/min of cooling rate and is cooled to room temperature.
Means of calcination in the prior art generally takes at the uniform velocity heating, at the uniform velocity cooling or temperature programming, program to cool down
Method；There are Railway Projects for this method: first, due to material stacks when calcining, so that it is in horizontal and vertical side
To physical presence temperature difference, lead to it actually and can not achieve purpose at the uniform velocity；Second, since zirconium oxide rises in temperature
Volume change can during which occur by monocline crystal transition at tetragonal phase at about 1173 DEG C, lead at the uniform velocity that heating cannot be good
Adapt to this variation；Third, the process that zirconium hydroxide-yttrium hydroxide calcining prepares zirconia-yttria have it is several key when
Intermediate node, at the uniform velocity heating, cooling cracking can cross over these key points, prevent system in these nodes from occurring well
Effect, the material for causing calcining to obtain cannot be accomplished to adulterate well, and then product property is caused to be not sufficiently stable, and increase subsequent make
The difficulty of used time sintering.
Preferably, the process of the ball milling are as follows:
A ball milling is first carried out, the powder that partial size is 1-3 microns is dried to obtain；24-48 hours aging, then plus water carries out
Secondary ball milling obtains the slurry.
First ball milling, the powder for being dried to obtain opposite bulky grain, by aging and then again secondary ball milling obtains final slurry,
This way has some benefits: first, reduce ball milling difficulty；Second, so that being finally spray-dried the partial size point of obtained material
Cloth range is narrower, and uniformity is more preferable；Third introduces aging process in this step, so that viscosity when material adds water for ball milling,
Mobility improves, and the performance of slurry is more uniform, the stability of the powder after improving spray drying, when the later period being avoided to use
Generate micro-crack.
Optionally, when carrying out the ball milling, silicon carbide and praseodymium neodymium oxide are additionally added.
In order to improve the effect of ball milling, dispersing agent and binder can also be added.
A kind of application of the yttrium stable zirconium oxide ceramic powders, for manufacturing artificial tooth.
Compared with prior art, the invention has the benefit that
(1) crystallinity is high, performance is stable, easy-sintering；
(2) partial size is small, good toughness, and use scope is wide；
(3) micro-crack is not susceptible to when applying.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
Embodiment 1
Zirconium oxychloride is dissolved with water, sodium sulphate is then added, has been warming up to solid precipitation, then cools down, filter
To zirconium sulfate；
Yttrium oxide is dissolved in hydrochloric acid solution, yttrium chloride solution is obtained；
Zirconium sulfate is dissolved with water, is then mixed with yttrium chloride solution, first stage control system temperature is 30 DEG C, is added dropwise
Sodium hydroxide solution makes system pH reach 8, then stirs 60 minutes；Second stage control system temperature is 60 DEG C, and hydrogen is added dropwise
Sodium hydroxide solution makes system pH reach 9, then stirs 30 minutes；Phase III control system temperature is 75 DEG C, and hydrogen-oxygen is added dropwise
Changing sodium solution to system final pH is 13.1, is then stirred 5 minutes；It is filtered, washed to obtain sediment；
Will be dry at 120 DEG C of sediment, then calcined: initial phase is warming up to 1050 DEG C in 30 minutes, then keeps the temperature
10 minutes, then in quenching in 5 minutes to 300 DEG C；Intermediate stage, 10 DEG C/min of heating rate of control are warming up to 1200 DEG C, heat preservation 50
Minute；Cooling stage, 10 DEG C/min of cooling rate of control are cooled to 1110 DEG C, then control 5 DEG C/min of cooling rate coolings
It to 1090 DEG C, then controls 10 DEG C/min of cooling rate and is cooled to 800 DEG C, finally control 30 DEG C/min of cooling rate and be cooled to often
Temperature.Then it is proportionally added into water and aluminium oxide, first carries out a ball milling, is dried to obtain the powder that partial size is 3 microns；Aging 24 is small
When, then plus water carries out secondary ball milling and obtains slurry, and slurry is dried to obtain yttrium stable zirconium oxide ceramic powders by spraying.It is steady to control yttrium
Determine in zirconia ceramics powder, with molar percent, comprising: yttrium oxide 4%, zirconium oxide 94% and aluminium oxide 2%.
Embodiment 2
Zirconium oxychloride is dissolved with water, ammonium sulfate is then added, has been warming up to solid precipitation, then cools down, filter
To zirconium sulfate；
Yttrium oxide is dissolved in hydrochloric acid solution, yttrium chloride solution is obtained；
Zirconium sulfate is dissolved with water, is then mixed with yttrium chloride solution, first stage control system temperature is 50 DEG C, is added dropwise
Ammonium hydroxide makes system pH reach 8, then stirs 30 minutes；Second stage control system temperature is 70 DEG C, and it is proper that dropwise addition ammonium hydroxide makes
It is that pH reaches 9, then stirs 10 minutes；Phase III control system temperature is 78 DEG C, and it is 10 that ammonium hydroxide to system final pH, which is added dropwise,
Then it stirs 15 minutes；It is filtered, washed to obtain sediment；
Will be dry at 80 DEG C of sediment, then calcined: initial phase is warming up to 1000 DEG C in 60 minutes, then keeps the temperature
30 minutes, then in quenching in 3 minutes to 350 DEG C；Intermediate stage, 5 DEG C/min of heating rate of control are warming up to 1300 DEG C, heat preservation 30
Minute；Cooling stage, 15 DEG C/min of cooling rate of control are cooled to 1110 DEG C, then control 1 DEG C/min of cooling rate cooling
It to 1090 DEG C, then controls 20 DEG C/min of cooling rate and is cooled to 500 DEG C, finally control 50 DEG C/min of cooling rate and be cooled to often
Temperature.Then being proportionally added into water and aluminium oxide, silicon carbide and praseodymium neodymium oxide, (partial size of silicon carbide is 100 nanometers, praseodymium neodymium oxide
Partial size is 100 nanometers), a ball milling is first carried out, the powder that partial size is 1 micron is dried to obtain；Aging 48 hours, then plus water into
Row secondary ball milling obtains slurry, and slurry is dried to obtain yttrium stable zirconium oxide ceramic powders by spraying.Control yttrium stable zirconium oxide ceramics
In powder, with molar percent, comprising: yttrium oxide 9%, zirconium oxide 89.92%, aluminium oxide 1%, silicon carbide 0.03% and oxygen
Change praseodymium neodymium 0.05%.
Embodiment 3
Zirconium oxychloride is dissolved with water, sodium sulphate or ammonium sulfate is then added, has been warming up to solid precipitation, it is then cold
But, zirconium sulfate is obtained by filtration；
Yttrium oxide is dissolved in hydrochloric acid solution, yttrium chloride solution is obtained；
Zirconium sulfate is dissolved with water, is then mixed with yttrium chloride solution, first stage control system temperature is 40 DEG C, is added dropwise
Potassium hydroxide solution makes system pH reach 8, then stirs 50 minutes；Second stage control system temperature is 65 DEG C, and hydrogen is added dropwise
Potassium oxide solution makes system pH reach 9, then stirs 20 minutes；Phase III control system temperature is 76 DEG C, and hydrogen-oxygen is added dropwise
Changing potassium solution to system final pH is 11, is then stirred 10 minutes；It is filtered, washed to obtain sediment；
Will be dry at 100 DEG C of sediment, then calcined: initial phase is warming up to 1020 DEG C in 40 minutes, then keeps the temperature
20 minutes, then in quenching in 4 minutes to 320 DEG C；Intermediate stage, 8 DEG C/min of heating rate of control are warming up to 1250 DEG C, heat preservation 40
Minute；Cooling stage, 12 DEG C/min of cooling rate of control are cooled to 1110 DEG C, then control 2 DEG C/min of cooling rate coolings
It to 1090 DEG C, then controls 15 DEG C/min of cooling rate and is cooled to 700 DEG C, finally control 40 DEG C/min of cooling rate and be cooled to often
Temperature.Then being proportionally added into water and aluminium oxide, silicon carbide and praseodymium neodymium oxide, (partial size of silicon carbide is 200 nanometers, praseodymium neodymium oxide
Partial size is 50 nanometers), a ball milling is first carried out, the powder that partial size is 2 microns is dried to obtain；Aging 36 hours, then plus water into
Row secondary ball milling obtains slurry, and slurry is dried to obtain yttrium stable zirconium oxide ceramic powders by spraying.Control yttrium stable zirconium oxide ceramics
In powder, with molar percent, comprising: yttrium oxide 8%, zirconium oxide 89%, aluminium oxide 2.89%, silicon carbide 0.01% and oxygen
Change praseodymium neodymium 0.1%.
Embodiment 4
Zirconium oxychloride is dissolved with water, sodium sulphate or ammonium sulfate is then added, has been warming up to solid precipitation, it is then cold
But, zirconium sulfate is obtained by filtration；
Yttrium oxide is dissolved in hydrochloric acid solution, yttrium chloride solution is obtained；
Zirconium sulfate is dissolved with water, is then mixed with yttrium chloride solution, first stage control system temperature is 35 DEG C, is added dropwise
Aqueous slkali makes system pH reach 8, then stirs 40 minutes；Second stage control system temperature is 68 DEG C, and aqueous slkali, which is added dropwise, to be made
It obtains system pH and reaches 9, then stir 15 minutes；Phase III control system temperature is 77 DEG C, and it is final to system that aqueous slkali is added dropwise
PH is 12, is then stirred 12 minutes；It is filtered, washed to obtain sediment；
Will be dry at 90 DEG C of sediment, then calcined: initial phase is warming up to 1005 DEG C in 50 minutes, then keeps the temperature
15 minutes, then in quenching in 3 minutes to 330 DEG C；Intermediate stage, 6 DEG C/min of heating rate of control are warming up to 1220 DEG C, heat preservation 45
Minute；Cooling stage, 14 DEG C/min of cooling rate of control are cooled to 1110 DEG C, then control 4 DEG C/min of cooling rate coolings
It to 1090 DEG C, then controls 12 DEG C/min of cooling rate and is cooled to 600 DEG C, finally control 35 DEG C/min of cooling rate and be cooled to often
Temperature.Then being proportionally added into water and aluminium oxide, silicon carbide and praseodymium neodymium oxide, (partial size of silicon carbide is 150 nanometers, praseodymium neodymium oxide
Partial size is 80 nanometers), a ball milling is first carried out, the powder that partial size is 2 microns is dried to obtain；Aging 48 hours, then plus water into
Row secondary ball milling obtains slurry, and slurry is dried to obtain yttrium stable zirconium oxide ceramic powders by spraying.Control yttrium stable zirconium oxide ceramics
In powder, with molar percent, comprising: yttrium oxide 4.5%, zirconium oxide 92.4%, aluminium oxide 3%, 0.02% and of silicon carbide
Praseodymium neodymium oxide 0.08%.
Comparative example 1
Compared with Example 1, pH, direct step section to 13.1 are adjusted without using the method that program is added dropwise.
Comparative example 2
Compared with Example 2, using 5 DEG C/min of heating rate, 1300 DEG C are at the uniform velocity warming up to, keeps the temperature 30 minutes, then
Naturally cool to the method calcining of room temperature.
Comparative example 3
Compared with Example 3, without using ball milling twice, one time ball milling is completed.
The obtained material of embodiment 1-4 and comparative example 1-3 is tested for the property, as a result as shown in table 1 below.
Specific test item are as follows:
1. yttrium stable zirconium oxide ceramic powders cake of press after 1400 DEG C/3h is at porcelain, measures density；
2. being calcined 3 hours at 1020 DEG C, its specific surface area is measured using aperture and specific surface area analysis instrument；
3. being measured Rockwell hardness to material using GB/T 230.1-2009；
4. measuring breaking strength to material with omnipotent test machine SANS.CMT4104.
It is specific that test result is as follows shown in table 1:
1 test result of table
| Project | Density g/cm3 | Specific surface area m2/g | Rockwell hardness HRB | Breaking strength N |
| Embodiment 1 | 6.0 | 8 | 89.0 | 1235 |
| Embodiment 2 | 6.07 | 10.5 | 90.0 | 1255 |
| Embodiment 3 | 6.06 | 11 | 91.0 | 1251 |
| Embodiment 4 | 6.06 | 12 | 91.0 | 1256 |
| Comparative example 1 | 5.85 | 6.9 | 79.0 | 1043 |
| Comparative example 2 | 5.56 | 6.5 | 75.0 | 1062 |
| Comparative example 3 | 5.62 | 7.0 | 81.0 | 1101 |
Above-mentioned test data shows that program is added dropwise aqueous slkali, calcination procedure and ball grinding method and can stablize to resulting yttrium
Zirconia ceramics powder has an impact.
Yttrium stable zirconium oxide ceramic powders provided by the present application, crystallinity is high, performance is stable, easy-sintering；Partial size is small, toughness
Good, use scope is wide；Using when be not susceptible to micro-crack.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from of the invention
Many other change and modification can be made in the case where spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of yttrium stable zirconium oxide ceramic powders, which is characterized in that with molar percent, comprising:
Yttrium oxide 4-9%, zirconium oxide 89-94% and aluminium oxide 1-3%.
2. yttrium stable zirconium oxide ceramic powders according to claim 1, which is characterized in that with molar percent, also wrap
It includes: silicon carbide 0.01-0.03% and praseodymium neodymium oxide 0.05-0.1%；Preferably, the partial size of the silicon carbide is received for 100-200
Rice, the partial size of the praseodymium neodymium oxide are 50-100 nanometers.
3. according to claim 1 or 2 described in any item yttrium stable zirconium oxide ceramic powders, which is characterized in that the yttrium is stablized
The partial size of zirconia ceramics powder is 50-200 nanometers.
4. a kind of preparation method of yttrium stable zirconium oxide ceramic powders described in claim 1, which is characterized in that including following step
It is rapid:
Zirconium oxychloride is dissolved with water, sodium sulphate or ammonium sulfate is then added, has been warming up to solid precipitation, then cooling, mistake
Filter obtains zirconium sulfate；
Yttrium oxide is dissolved in hydrochloric acid solution, yttrium chloride solution is obtained；
The zirconium sulfate is dissolved with water, is then mixed with the yttrium chloride solution, aqueous slkali and control system is added dropwise most in program
Whole pH is 10-13.1, is filtered, washed to obtain sediment；
By the drying precipitate, calcining, then it is proportionally added into water and the aluminium oxide carries out ball milling and obtains slurry, the slurry
Material spray drying obtains the yttrium stable zirconium oxide ceramic powders.
5. the preparation method according to claim 4, which is characterized in that aqueous slkali is added dropwise in described program are as follows:
First stage control system temperature is 30-50 DEG C, the aqueous slkali is added dropwise, system pH is made to reach 8, then stir 30-60
Minute；
Second stage control system temperature is 60-70 DEG C, the aqueous slkali is added dropwise, system pH is made to reach 9, then stir 10-30
Minute；
Phase III control system temperature is 75-78 DEG C, and the aqueous slkali is added dropwise to terminal, is then stirred 5-15 minutes.
6. the preparation method according to claim 4, which is characterized in that the temperature of the drying is 80-120 DEG C.
7. the preparation method according to claim 4, which is characterized in that the process of the calcining are as follows: initial phase, 30-60
Minute is warming up to 1000-1050 DEG C, then keeps the temperature 10-30 minutes, then in quenching in 3-5 minutes to 300-350 DEG C；Intermediate stage,
5-10 DEG C/min of heating rate of control is warming up to 1200-1300 DEG C, keeps the temperature 30-50 minutes；Cooling stage controls cooling rate
10-15 DEG C/min is cooled to 1110 DEG C, then controls 1-5 DEG C/min of cooling rate and is cooled to 1090 DEG C, then controls cooling speed
10-20 DEG C/min of rate is cooled to 500-800 DEG C, finally controls 30-50 DEG C/min of cooling rate and is cooled to room temperature.
8. the preparation method according to claim 4, which is characterized in that the process of the ball milling are as follows:
A ball milling is first carried out, the powder that partial size is 1-3 microns is dried to obtain；24-48 hours aging, then plus water progress is secondary
Ball milling obtains the slurry.
9. according to the described in any item preparation methods of claim 4-8, which is characterized in that when carrying out the ball milling, be additionally added carbon
SiClx and praseodymium neodymium oxide.
10. a kind of application of yttrium stable zirconium oxide ceramic powders of any of claims 1 or 2, which is characterized in that for manufacturing vacation
Tooth.
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