CN106830973A - A kind of new A l2O3/ZrO2(Y2O3) complex phase ceramic preparation method - Google Patents

A kind of new A l2O3/ZrO2(Y2O3) complex phase ceramic preparation method Download PDF

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CN106830973A
CN106830973A CN201710070381.4A CN201710070381A CN106830973A CN 106830973 A CN106830973 A CN 106830973A CN 201710070381 A CN201710070381 A CN 201710070381A CN 106830973 A CN106830973 A CN 106830973A
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porous ceramics
zro
complex phase
phase ceramic
new
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许小静
李平
王帅
徐泽跃
郭文飞
陆丽芳
伦文山
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JIANGSU PROV CERAMIC RESEARCH INST Co Ltd
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JIANGSU PROV CERAMIC RESEARCH INST Co Ltd
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Abstract

The invention discloses a kind of new A l2O3/ZrO2(Y2O3) complex phase ceramic preparation method.First by Al2O3Powder is made Al2O3Porous ceramics, then under vacuum conditions by the Al2O3Porous ceramics is immersed in containing Zr4+、Y3+Liquid in, liquid is filled into Al2O3In the hole of porous ceramics, then by hydro-thermal reaction, make the Zr in liquid4+、Y3+Solidification is attached to Al2O3Particle surface, finally by drying and be fired into a kind of new Al2O3/ZrO2(Y2O3) complex phase ceramic.The present invention can make ZrO2、Y2O3It is dispersed in complex phase ceramic, it is to avoid to reunite, the second relative effect for improving material mechanical performance, and preparation process is simple are enhanced, convenient to carry out and popularization can be in existing Al2O3Mass production is carried out on ceramic production line.

Description

A kind of new A l2O3/ZrO2(Y2O3) complex phase ceramic preparation method
Technical field
The invention belongs to high-temperature structural ceramics technical field, it is related to a kind of Al2O3/ZrO2(Y2O3) complex phase ceramic and its preparation Method.
Background technology
Al2O3The ceramic material spy such as have high temperature resistant, resistant to chemical etching, anti-oxidant, wear-resisting, high mechanical strength, insulating properties high Property, it is most widely used high temperature resistant structure ceramicses.But, the Al obtained by our actual productions2O3The machinery of ceramic material Performance and theoretical values have larger gap, and a main cause is, Al2O3Ceramic material is original when high temperature burns till Al2O3Particle can form larger size, Al by grain growth2O3Crystallite dimension increase can cause under the mechanical performance of material Drop.By in Al2O3ZrO is introduced in material2Multiphase structure is formed, can not only effectively suppress Al2O3Life of the crystal grain when burning till It is long, also with toughening effect, effectively increase the mechanical performance of material.
In Al2O3The conventional method of the second phase is introduced in material, is that the raw material of the second phase will be formed in dispensing according to design Proportioning add it is well mixed, then according to Al2O3The production technology of ceramics, the blank containing the second phase constituent is fabricated into Required complex phase ceramic product.This is a kind of relatively easy and relatively inexpensive method, but the major defect for existing is system The Al for producing2O3/ZrO2(Y2O3) the second phase crystal grain phenomenon pockety easily occurs in complex phase ceramic.What phenomenon was produced Reason is mainly the second phase crystal grain and easily reunites in Feedstock treating.Therefore, second how is allowed mutually to be evenly distributed in Al2O3It is brilliant It is to improve Al between grain2O3/ZrO2(Y2O3) complex phase ceramic mechanical performance one of key technology.
The content of the invention
The invention provides a kind of new A l2O3/ZrO2(Y2O3) complex phase ceramic preparation method, can effectively by second Phase ZrO2It is evengranular to be distributed in Al2O3Between particle, Al is improve2O3/ZrO2(Y2O3) complex phase ceramic mechanical performance.This Invention first using conventional Production Technique of Alumina Ceramics, Al is produced by easy fired2O3Porous ceramics, then in vacuum By the Al under environment2O3Porous ceramics is immersed in and contains the second phase constituent Zr4+、Y3+Liquid in, liquid is filled into Al2O3It is many In the hole of hole ceramics, then by hydro-thermal reaction, make the Zr in liquid4+、Y3+Be converted into solid, and by repeated impregnations and Adjustment strength of fluid controls the content of the second phase, the Al after final impregnating treatment2O3Porous ceramics is by drying and being fired into one Plant the Al of the new uniform excellent performance of the second distributed mutually2O3/ZrO2(Y2O3) complex phase ceramic.
To realize the object of the invention, there is provided following technical scheme：A kind of new A l2O3/ZrO2(Y2O3) complex phase ceramic Preparation method, comprises the following steps, first by Al2O3Powder is made Al2O3Porous ceramics, then under vacuum conditions should Al2O3Porous ceramics is immersed in containing Zr4+、Y3+Liquid in, liquid is filled into Al2O3In the hole of porous ceramics, then pass through Hydro-thermal reaction, makes the Zr in liquid4+、Y3+Solidification is attached to Al2O3Particle surface, then it is heat-treated after repeat above-mentioned dipping Journey, to improve two kinds of contents of composition of Zr elements and Y element, finally by drying and be fired into finished product.
Preferably, containing Zr4+、Y3+Liquid components by percentage to the quality：Zirconium nitrate（Zr(NO3)4·3H2O）35.0~ 45.8wt%, yttrium nitrate（Y(NO3)3·6H2O）2.2 ~ 2.8wt%, 36.7 ~ 51.6wt% of deionized water, 11.2 ~ 14.7wt% of urea.
Preferably, containing Zr4+、Y3+Liquid preparation method：Zirconium nitrate, yttrium nitrate and deionized water are weighed in proportion, 80 ~ 85 DEG C of constant temperature water baths are simultaneously stirred, and solution are cooled into 20 ~ 30 DEG C after zirconium nitrate, yttrium nitrate are completely dissolved, then claim in proportion Amount urea is added, stirring and dissolving.
Preferably, Al2O3Porous ceramics is immersed in containing Zr4+、Y3+The specific steps of liquid include：By Al2O3Porous pottery Porcelain is put into closed container, and 10 ~ 15min is kept under vacuum≤10Pa, is continued to keep vacuum state and is noted to closed container Enter containing Zr4+、Y3+Liquid, to Al2O3Porous ceramics is totally submerged by liquid, and 10 ~ 15min is persistently submerged under vacuum；Will dipping Al afterwards2O3Porous ceramics takes out and carries out hydro-thermal reaction, then heating, drying, obtains containing Zr elements and Y element composition Al2O3Porous ceramics；The porous ceramics for impregnating drying is heated, is then increased by repeating above-mentioned dipping process Two kinds of contents of composition of Zr elements and Y element, number of repetition 0 ~ 4 time in material.By controlling the concentration of solution secondary with dipping Count to control Al2O3/ZrO2(Y2O3) ZrO in complex phase ceramic2And Y2O3Content.
Preferably, that burns till concretely comprises the following steps：By the Al after impregnation process2O3Porous ceramics is placed in high temperature kiln roasting, 1700 ~ 1750 DEG C are warmed up to the speed of 0.5 ~ 1 DEG C/min, and in maximum temperature 2 ~ 5h of constant temperature, furnace cooling is obtained to room temperature Al of the present invention2O3/ZrO2(Y2O3) complex phase ceramic.
Preferably, Al2O3Porous ceramics preparation process：α-Al are weighed in proportion2O3、CaCO3、Y2O3、MgCO3, kaolinite Soil, 10%PVA solution and deionized water, add ball mill 16 ~ 36h of wet-milling, obtain aqueous slurry of the average grain diameter at 1.6 ~ 4.7 μm Material, is processed into dry-pressing formed blank, and obtain so that the pressure of 100 ~ 120MPa is compressing by water paste by mist projection granulating The Al of required geomery2O3Green compact are dried 12 ~ 24h by ceramic green in 60 ~ 80 DEG C of temperature, make green compact moisture content≤ 1wt%, is finally putting into kiln, and 1300 ~ 1400 DEG C are warmed up to the speed of 0.5 ~ 1 DEG C/min, and in maximum temperature 2 ~ 3h of constant temperature, Furnace cooling obtains Al to room temperature2O3Porous ceramics.
Preferably, the component of the water paste is by percentage to the quality：α-Al2O351.54 ~ 56.72wt%, CaCO30.00 ~ 0.10wt%, Y2O30.00 ~ 0.17wt%, MgCO30.00 ~ 0.11wt%'s, kaolin 0.00 ~ 0.36wt%, 10% 3 ~ 7wt% of PVA solution, 38 ~ 41wt% of deionized water.Wherein α-Al2O3 、Y2O3It is by 400 mesh fine powders, CaCO3、MgCO3And height Ridge soil is by 250 targeted fine powders.
Preferably, hydro-thermal reaction is specially：By the Al after dipping2O3Porous ceramics is placed in climatic chamber, thermostat temperature It is 80 ~ 90 DEG C, constant humidity humidity >=98%, 4 ~ 8h of constant temperature and humidity time.
Preferably, heating is specially：By the Al after hydro-thermal reaction2O3Porous ceramics is placed in 90 ~ 100 DEG C of constant temperature 6 ~ 12h in drying box, then be put into kiln and be warmed up to 600 DEG C with the speed of 0.5 ~ 1 DEG C/min, 2 ~ 3h of constant temperature, furnace cooling is arrived Room temperature.
Beneficial effect of the present invention：Invention utilizes hydro-thermal reaction by the ZrO of the second phase2Separated out with nano particle and be coated on Al2O3Particle surface, realizes ZrO2It is dispersed；Meanwhile, micron order Al2O3The gap that particle packing is formed constitutes submicron order Masterplate, can effectively limit ZrO2The reunion of nano particle, makes ZrO2Second in Al2O3In it is dispersed, cause according to Al prepared by the present invention2O3/ZrO2(Y2O3) complex phase ceramic has more preferable mechanical performance.
Specific embodiment
The present invention is done with reference to embodiment is further explained, the following example is merely to illustrate the present invention, but It is not used to limit use scope of the invention.
Embodiment 1：
（1）Weigh α-Al2O351.54wt%、CaCO30.10wt%、MgCO30.10wt%, kaolin 0.26wt%, 10%PVA solution 3wt%, deionized water 45wt%, wherein α-Al2O3It is by 400 mesh fine powders, CaCO3、MgCO3, kaolin be by 250 purposes Fine powder, adds ball mill wet-milling 36h, obtains average grain diameter in 1.6 μm of water paste, and water paste is added by mist projection granulating Work into dry-pressing formed blank, and with the compressing Al for obtaining required geomery of the pressure of 120MPa2O3Ceramic green, by life Base dries 12h in 80 DEG C of temperature, makes green compact moisture content≤1wt%, is finally putting into kiln, is warmed up to the speed of 0.5 DEG C/min 1300 DEG C, and in maximum temperature constant temperature 3h, furnace cooling obtains Al to room temperature2O3Porous ceramics.
（2）Zirconium nitrate 45.8wt%, yttrium nitrate 2.8wt%, deionized water 36.7wt% are weighed, 80 DEG C of constant temperature water baths are simultaneously stirred, Solution is cooled to 20 DEG C after zirconium nitrate, yttrium nitrate are completely dissolved, 14.7wt% urea is added, is soaked after stirring and dissolving Stain liquid.
（3）By step（1）Gained Al2O3Porous ceramics is put into closed container, and 15min is kept under vacuum≤10Pa, Continue to keep vacuum state and to closed container implantation step（2）Gained steeping liq, to Al2O3Porous ceramics is complete by liquid Submergence, and continue to impregnate 15min；By the Al after dipping2O3Porous ceramics takes out and is placed in climatic chamber, and thermostat temperature is 90 DEG C, Constant humidity humidity >=98%, constant temperature and humidity time 4h.Hydro-thermal reaction is carried out, then by the Al after hydro-thermal reaction2O3Porous ceramics is placed in 6h in 100 DEG C of freeze-day with constant temperature, then 600 DEG C, freeze-day with constant temperature 2h are warmed up to the speed of 0.5 DEG C/min.Heating, drying, is contained There is the Al of Zr elements and Y element composition2O3Porous ceramics.
（4）By step（3）Al after treatment2O3Porous ceramics is placed in high temperature kiln roasting, with the speed liter of 1.0 DEG C/min Temperature is to 1700 DEG C, and in maximum temperature constant temperature 2h, furnace cooling obtains Al of the present invention to room temperature2O3/ZrO2(Y2O3) multiple Phase ceramics.
The bulk density of the diphase ceramic material is 3.89g/cm3, three-point bending resistance intensity is 291 MPa.
Embodiment 2：
（1）Weigh α-Al2O352.53wt%、Y2O30.11wt%, kaolin 0.36wt%, 10%PVA solution 7wt%, deionized water 40wt%, wherein α-Al2O3 、Y2O3It is by 400 mesh fine powders, CaCO3, kaolin be by 250 targeted fine powders, to add ball mill Wet-milling 16h, obtains water paste of the average grain diameter at 4.7 μm, and water paste is processed into dry-pressing formed base by mist projection granulating Material, and with the compressing Al for obtaining required geomery of the pressure of 100MPa2O3Ceramic green, by green compact in 70 DEG C of temperature Drying 18h, makes green compact moisture content≤1wt%, is finally putting into kiln, and 1350 DEG C are warmed up to the speed of 0.8 DEG C/min, and most High-temperature constant temperature 2h, furnace cooling obtains Al to room temperature2O3Porous ceramics.
（2）Zirconium nitrate 42.0wt%, yttrium nitrate 2.6wt%, deionized water 41.9wt% are weighed, 85 DEG C of constant temperature water baths are simultaneously stirred, Solution is cooled to 20 DEG C after zirconium nitrate, yttrium nitrate are completely dissolved, 13.5wt% urea is added, is soaked after stirring and dissolving Stain liquid.
（3）By step（1）Gained Al2O3Porous ceramics is put into closed container, and 15min is kept under vacuum≤10Pa, Continue to keep vacuum state and to closed container implantation step（2）Gained steeping liq, to Al2O3Porous ceramics is complete by liquid Submergence, and continue to impregnate 10min；By the Al after dipping2O3Porous ceramics takes out and is placed in climatic chamber, and thermostat temperature is 85 DEG C, Constant humidity humidity >=98%, constant temperature and humidity time 6h.Hydro-thermal reaction is carried out, then by the Al after hydro-thermal reaction2O3Porous ceramics is placed in 8h in 95 DEG C of freeze-day with constant temperature, then 600 DEG C, freeze-day with constant temperature 3h are warmed up to the speed of 0.8 DEG C/min.Heating, drying, is contained There is the Al of Zr elements and Y element composition2O3Porous ceramics.
（4）By step（3）Al after treatment2O3Porous ceramics repeat step（3）, to increase by two kinds of contents of component of Zr, Y, Number of repetition 1 time.
（5）By step（4）Al after treatment2O3Porous ceramics is placed in high temperature kiln roasting, with the speed liter of 0.8 DEG C/min Temperature is to 1720 DEG C, and in maximum temperature constant temperature 3h, furnace cooling obtains Al of the present invention to room temperature2O3/ZrO2(Y2O3) multiple Phase ceramics.
The bulk density of the diphase ceramic material is 3.93g/cm3, three-point bending resistance intensity is 342MPa.
Embodiment 3：
（1）Weigh α-Al2O356.72wt%、Y2O30.17wt%、MgCO30.11wt%, 10%PVA solution 5wt%, deionized water 38wt%, wherein α-Al2O3 、Y2O3It is by 400 mesh fine powders, MgCO3It is, by 250 targeted fine powders, to add ball mill wet-milling 24h, obtains water paste of the average grain diameter at 3.1 μm, and water paste is processed into dry-pressing formed blank by mist projection granulating, and With the compressing Al for obtaining required geomery of the pressure of 120MPa2O3Ceramic green, green compact are dried in 60 DEG C of temperature 24h, makes green compact moisture content≤1wt%, is finally putting into kiln, and 1400 DEG C are warmed up to the speed of 1.0 DEG C/min, and in the highest temperature Degree constant temperature 2h, furnace cooling obtains Al to room temperature2O3Porous ceramics.
（2）Zirconium nitrate 35.0wt%, yttrium nitrate 2.2wt%, deionized water 51.6wt% are weighed, 85 DEG C of constant temperature water baths are simultaneously stirred, Solution is cooled to 30 DEG C after zirconium nitrate, yttrium nitrate are completely dissolved, 11.2wt% urea is added, is soaked after stirring and dissolving Stain liquid.
（3）By step（1）Gained Al2O3Porous ceramics is put into closed container, and 10min is kept under vacuum 10Pa, after Continuation of insurance holds vacuum state and to closed container implantation step（2）Gained steeping liq, to Al2O3Porous ceramics is soaked completely by liquid Not yet, and continue impregnate 15min；By the Al after dipping2O3Porous ceramics takes out and is placed in climatic chamber, and thermostat temperature is 80 DEG C, permanent Humidity >=98%, constant temperature and humidity time 8h.Hydro-thermal reaction is carried out, then by the Al after hydro-thermal reaction2O3Porous ceramics is placed in 90 DEG C freeze-day with constant temperature in 12h, then 600 DEG C, freeze-day with constant temperature 3h are warmed up to the speed of 0.5 DEG C/min.Heating, drying, is contained The Al of Zr elements and Y element composition2O3Porous ceramics.
（4）By step（3）Al after treatment2O3Porous ceramics repeat step（3）, to increase by two kinds of contents of component of Zr, Y, Number of repetition 3 times.
（5）By step（4）Al after treatment2O3Porous ceramics is placed in high temperature kiln roasting, with the speed liter of 0.5 DEG C/min Temperature is to 1750 DEG C, and in maximum temperature constant temperature 5h, furnace cooling obtains Al of the present invention to room temperature2O3/ZrO2(Y2O3) multiple Phase ceramics.
The bulk density of the diphase ceramic material is 4.01g/cm3, three-point bending resistance intensity 418MPa.

Claims (10)

1. a kind of new A l2O3/ZrO2(Y2O3) complex phase ceramic preparation method, it is characterised in that comprise the following steps：First will Al2O3Powder is made Al2O3Porous ceramics, then under vacuum conditions by the Al2O3Porous ceramics is immersed in containing Zr4+、Y3+Liquid In body, liquid is set to be filled into Al2O3In the hole of porous ceramics, then by hydro-thermal reaction, make the Zr in liquid4+、Y3+Solidification is attached In Al2O3Particle surface, finally by drying and be fired into finished product.
2. a kind of new A l according to claim 12O3/ZrO2(Y2O3) complex phase ceramic preparation method, it is characterised in that Containing Zr4+、Y3+Liquid components by percentage to the quality：Zirconium nitrate（Zr(NO3)4·3H2O）35.0 ~ 45.8wt%, yttrium nitrate（Y (NO3)3·6H2O）2.2 ~ 2.8wt%, 36.7 ~ 51.6wt% of deionized water, 11.2 ~ 14.7wt% of urea.
3. a kind of new A l according to claim 22O3/ZrO2(Y2O3) complex phase ceramic preparation method, it is characterised in that Containing Zr4+、Y3+Liquid preparation method：Zirconium nitrate, yttrium nitrate and deionized water are weighed in proportion, and 80 ~ 85 DEG C of constant temperature water baths are simultaneously Stirring, 20 ~ 30 DEG C are cooled to after zirconium nitrate, yttrium nitrate are completely dissolved by solution, then weigh urea addition in proportion, are stirred molten Solution.
4. a kind of new A l according to claim 12O3/ZrO2(Y2O3) complex phase ceramic preparation method, it is characterised in that Al2O3Porous ceramics is immersed in containing Zr4+、Y3+The specific steps of liquid include：By Al2O3Porous ceramics is put into closed container, 10 ~ 15min is kept under vacuum≤10Pa, is continued to keep vacuum state and is contained Zr to closed container injection4+、Y3+Liquid, To Al2O3Porous ceramics is totally submerged by liquid, and 10 ~ 15min is persistently submerged under vacuum；By the Al after dipping2O3Porous ceramics takes Go out to carry out hydro-thermal reaction, then heating, drying, obtain the Al containing Zr elements and Y element composition2O3Porous ceramics；Dipping is dried Dry porous ceramics is heated, and Zr elements and Y element two in material are then increased by repeating above-mentioned dipping process Plant the content of composition, number of repetition 0 ~ 4 time.
5. a kind of new A l according to claim 12O3/ZrO2(Y2O3) complex phase ceramic preparation method, it is characterised in that That burns till concretely comprises the following steps：By the Al after impregnation process2O3Porous ceramics is placed in high temperature kiln roasting, with the speed of 0.5 ~ 1 DEG C/min Degree is warmed up to 1700 ~ 1750 DEG C, and in maximum temperature 2 ~ 5h of constant temperature, furnace cooling obtains Al of the present invention to room temperature2O3/ ZrO2(Y2O3) complex phase ceramic.
6. a kind of new A l according to claim 12O3/ZrO2(Y2O3) complex phase ceramic preparation method, it is characterised in that Al2O3Porous ceramics preparation process：α-Al are weighed in proportion2O3、CaCO3、Y2O3、MgCO3, kaolin, 10%PVA solution and go Ionized water, adds ball mill 16 ~ 36h of wet-milling, obtains average grain diameter in 1.6 ~ 4.7 μm of water paste, and water paste is passed through Mist projection granulating is processed into dry-pressing formed blank, and with the compressing Al for obtaining required geomery of the pressure of 100 ~ 120MPa2O3 Green compact are dried 12 ~ 24h by ceramic green in 60 ~ 80 DEG C of temperature, make green compact moisture content≤1wt%, are finally putting into kiln, with The speed of 0.5 ~ 1 DEG C/min is warmed up to 1300 ~ 1400 DEG C, and in maximum temperature 2 ~ 3h of constant temperature, furnace cooling is obtained to room temperature Al2O3Porous ceramics.
7. a kind of new A l according to claim 62O3/ZrO2(Y2O3) complex phase ceramic preparation method, it is characterised in that The component of the water paste is by percentage to the quality：α-Al2O351.54 ~ 56.72wt%, CaCO30.00 ~ 0.10wt%, Y2O30.00 ~ 0.17wt%, MgCO30.00 ~ 0.11wt%, kaolin 0.00 ~ 0.36wt%, 10% 3 ~ 7wt% of PVA solution, go from Sub- 38 ~ 41wt% of water.
8. wherein α-Al2O3 、Y2O3It is by 400 mesh fine powders, CaCO3、MgCO3It is by 250 targeted fine powders with kaolin.
9. a kind of new A l according to claim 42O3/ZrO2(Y2O3) complex phase ceramic preparation method, it is characterised in that Hydro-thermal reaction is specially：By the Al after dipping2O3Porous ceramics is placed in climatic chamber, and thermostat temperature is 80 ~ 90 DEG C, and constant humidity is wet Degree >=98%, 4 ~ 8h of constant temperature and humidity time.
10. a kind of new A l according to claim 42O3/ZrO2(Y2O3) complex phase ceramic preparation method, it is characterised in that Heating is specially：By the Al after hydro-thermal reaction2O3Porous ceramics is placed in 6 ~ 12h in 90 ~ 100 DEG C of thermostatic drying chamber, then puts 600 DEG C, 2 ~ 3h of constant temperature, furnace cooling to room temperature are warmed up to the speed of 0.5 ~ 1 DEG C/min in kiln.
CN201710070381.4A 2017-02-09 2017-02-09 A kind of new A l2O3/ZrO2(Y2O3) complex phase ceramic preparation method Pending CN106830973A (en)

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Application publication date: 20170613