CN111018501A - Preparation method of ZTA ceramic - Google Patents
Preparation method of ZTA ceramic Download PDFInfo
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- CN111018501A CN111018501A CN201911233795.XA CN201911233795A CN111018501A CN 111018501 A CN111018501 A CN 111018501A CN 201911233795 A CN201911233795 A CN 201911233795A CN 111018501 A CN111018501 A CN 111018501A
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Abstract
The invention relates to a preparation method of ZTA ceramic, which is characterized by comprising the following steps: step 1, preparing a 3Y-ZrO2 precursor xerogel; step 2, preparing a premixed solution: preparing a premixed solution from the precursor xerogel; step 3, mixing and ball milling: mixing the premixed liquid and performing ball milling to obtain slurry; step 4, defoaming the slurry: de-foaming the slurry; and 5, injection molding: injecting the defoaming slurry obtained in the step 4 into a model; step 6, demoulding and drying; and 7, sintering. The ZTA ceramic prepared by the invention has high strength, high density, controllable crystal grain and excellent performance.
Description
Technical Field
The invention relates to the field of ceramics, in particular to a preparation method of ZTA ceramics.
Background
The ZTA complex phase ceramic has the characteristics of high fracture toughness, high wear resistance, high mechanical strength, high chemical stability and the like, and is widely applied to the industries of electronics, automobiles, mineral development, metallurgy and the like. However, because the ZTA complex-phase ceramic has the characteristics of complex formula, complex powder property and the like, the existing preparation process has the defects of difficult preparation of composite powder, uneven mixing, high sintering temperature, difficult process design, various production types, difficult post-processing and the like in the preparation process. When the ceramic is used as high-performance industrial ceramic, parts with complex shapes, high dimensional accuracy, high mechanical performance and no internal defects are required to be prepared, the existing dry pressing process, cold isostatic pressing process, hot die casting process, injection molding process and the like have certain limitations, and certain difficulty is caused when the high-performance ZTA complex phase ceramic is prepared. Therefore, the water system gel film-injection method for forming complex shapes and avoiding introducing high-content toxic organic matters is one of the key technologies for preparing ZTA complex-phase ceramics.
Conventionally, the ZTA complex phase ceramic is prepared by adding ZrO2 powder into Al2O3 powder, mechanically mixing, granulating, molding, sintering and post-processing. Although the preparation process is mature, the problems of agglomeration caused by uneven particle dispersion, manifested by uneven distribution of the second phase after firing, abnormal growth of partial main crystal phase particles and the like exist, and the performance of the ZTA complex phase ceramic is greatly reduced due to phase separation defects (such as over-firing of partial area and easy occurrence of residual internal stress among crystal grains). In addition, the traditional gel injection molding method has the problems of high toxicity of the additive, difficult operation, easy cracking of green bodies and the like, and is difficult to carry out batch industrial production. Therefore, the preparation of the complex phase ceramic with uniform second phase distribution and strong process operability is also one of the key technical problems to be solved by the industrial ceramic.
Disclosure of Invention
In order to solve the technical problem, the invention provides a preparation method of ZTA ceramic, which is characterized by comprising the following steps: step 1, preparing a 3Y-ZrO2 precursor xerogel; step 2, preparing a premixed solution: preparing a premixed solution from the precursor xerogel; step 3, mixing and ball milling: mixing the premixed liquid and performing ball milling to obtain slurry; step 4, defoaming the slurry: de-foaming the slurry; and 5, injection molding: injecting the defoaming slurry obtained in the step 4 into a model; step 6, demoulding and drying; and 7, sintering.
Further, in the step 1, the preparation of the 3Y-ZrO2 precursor xerogel comprises the following steps: weighing a certain amount of Zr (NO3) 4.3H 2O and Y (NO3) 3.6H 2O, adding into deionized water, and uniformly stirring to obtain a zirconium oxide precursor solution; adding strong ammonia water to obtain 3Y-ZrO2 precursor gel solution; and filtering, washing and drying the gel solution to obtain the 3Y-ZrO2 precursor xerogel.
Further, in the step 2, the preparation of the premix comprises the following steps: weighing methacrylamide polymer powder, polyacrylamide, 3Y-ZrO2 precursor xerogel and deionized water, adding into a planetary ball mill, and ball-milling to obtain a premixed solution.
Further, the step 3 comprises: and (3) weighing a certain amount of alumina powder and a small amount of deionized water, adding the alumina powder and the deionized water into the premixed liquid prepared in the step (2) according to the solid content or the fixed volume ratio, and performing rapid ball milling until the granularity reaches the required value to obtain the slurry for gel injection molding.
Further, the step 4 comprises: and (4) transferring the slurry obtained in the step (3) to a vacuum device, and stirring and degassing in vacuum until bubbles disappear.
Further, the step 5 comprises: and (4) injecting the slurry obtained in the step (4) into a prepared model, and curing the model in an environment with certain relative humidity and temperature until the slurry is solidified.
Further, the step 6 comprises: and (5) demolding the blank obtained in the step (5), transferring the blank into a temperature and humidity adjusting box, setting the temperature and the relative humidity, and drying.
Further, the step 7 includes: and (4) transferring the dried green body obtained in the step (6) to a high-temperature kiln to sinter the ZTA ceramic.
The ZTA ceramic prepared by the invention has high strength, high density, controllable crystal grain and excellent performance.
Detailed Description
The invention is further described with reference to specific examples.
The preparation method of ZTA ceramic comprises the following steps:
step 1, preparing a 3Y-ZrO2 precursor xerogel: weighing a certain amount of Zr (NO3) 4.3H 2O and Y (NO3) 3.6H 2O, adding into deionized water, and uniformly stirring to obtain a zirconium oxide precursor solution; (b) adding strong ammonia water to obtain 3Y-ZrO2 precursor gel solution; (c) filtering, washing and drying the gel solution to obtain a 3Y-ZrO2 precursor xerogel;
step 2, preparing a premixed solution, namely weighing methacrylamide polymer powder, polyacrylamide, 3Y-ZrO2 precursor xerogel and deionized water, adding the weighed methacrylamide polymer powder, polyacrylamide, 3Y-ZrO2 precursor xerogel and deionized water into a planetary ball mill, and ball-milling to obtain the premixed solution;
step 3, mixing and ball milling: weighing a certain amount of alumina powder and a small amount of deionized water, adding the alumina powder and the small amount of deionized water into the premixed liquid prepared in the step 2 according to the solid content or the fixed volume ratio, and performing rapid ball milling until the granularity reaches a required value to obtain slurry for gel injection molding;
step 4, defoaming the slurry: transferring the slurry obtained in the step (3) to a vacuum device, and carrying out vacuum stirring and degassing until bubbles disappear;
and 5, injection molding: injecting the slurry obtained in the step (4) into a prepared model, and curing the model in an environment with certain relative humidity and temperature until the slurry is solidified;
step 6, demoulding and drying: demolding the blank obtained in the step 5, transferring the blank into a temperature and humidity adjusting box, setting the temperature and the relative humidity, and drying;
step 7, sintering: and (4) transferring the dried blank obtained in the step (6) to a high-temperature kiln for sintering to obtain the ZTA ceramic prepared by the invention.
The specific preparation process of the complex phase ceramic comprises the following steps:
step 1, preparing a dry gel of the 3Y-ZrO2 precursor: weighing 4.3H 2O 16-37 parts of Zr (NO3) and 3.6H 2O 2O 9-22 parts of Y (NO3) into 33-60 parts of deionized water, and stirring and dissolving to obtain a mixed solution; adding ammonia water with the concentration of 25 wt% to generate a precipitate, and stirring and standing to form sol; filtering, washing and drying to obtain a dried gel of the 3Y-ZrO2 precursor;
step 2, preparing a premixed solution: weighing 0.35-0.4 part of methacrylamide polymer powder, 0.1-0.25 part of polyacrylamide and 31-25 parts of deionized water, mixing, stirring and dissolving; adding 5-18.4 parts of 3Y-ZrO2 precursor dry gel; grinding at high speed for 10min in a planetary mill;
step 3, preparing alumina slurry: weighing 100 parts of Al2O3 with the particle size D50 of 0.8 mu m, adding the Al2O3 into the premixed liquid, carrying out rapid ball milling until the particle size D50 reaches 0.65-0.75 mu m, and pouring out the slurry for later use;
step 4, defoaming the slurry: transferring the slurry obtained in the step 3 into a vacuum device, and carrying out vacuum stirring and degassing for 10-20 min until bubbles disappear;
and 5, injection molding: injecting the slurry obtained in the step (4) into a prepared model, and curing for 1-2 hours in an environment with the relative humidity of 80-95% and the temperature of 10-30 ℃ until the slurry is solidified;
step 6, demoulding and drying: demolding the blank obtained in the step 5, and transferring the blank into a temperature and humidity adjusting box, wherein the temperature is 80 ℃, and the relative humidity change range is 95-10%, and drying for 2-12 hours;
step 7, sintering: and (3) transferring the dried blank obtained in the step (6) into a high-temperature kiln to be fired, keeping the temperature at the maximum temperature of 1600-1720 ℃ for 0.5-5 h, and cooling to room temperature along with the kiln to obtain the ZTA ceramic prepared by the invention.
Example 1:
step 1, weighing Zr (NO3) 4.3H 2O 98.7.7 g and Y (NO3) 3.6H 2O 5.77.77 g, adding into 987ml of deionized water, stirring and dissolving to obtain a mixed solution, and adding excessive concentrated ammonia water to adjust the pH value to 11. And 3Y-ZrO2 precursor sol is generated. Filtering and drying the sol to obtain a 3Y-ZrO2 precursor xerogel;
step 2, weighing 3.76g of methacrylamide polymer powder, 2.5g of polyacrylamide and 249ml of deionized water, adding the weighed materials and the xerogel prepared in the previous step into a ball milling tank of a planetary ball mill, setting the rotation speed to 600rpm, and carrying out rapid ball milling for 10min to obtain a premixed solution;
step 3, weighing 1000g of alumina powder, adding the alumina powder into a ball milling tank of the premixed liquid, setting the rotating speed at 600RPM, and carrying out rapid ball milling for 10min to obtain alumina slurry with the viscosity of 1890mPa & s;
step 4, transferring the slurry obtained in the step 3 to a vacuum stirrer, and stirring for 20min in vacuum to obtain defoamed slurry;
step 5, injecting the slurry obtained in the step 4 into a grinding tool, standing at room temperature for 100min for forming, and demolding to obtain a wet blank;
step 6, transferring the wet blank into a temperature-adjusting debugging box, and respectively drying for 2 hours at the relative humidity of 95%, 75%, 50% and 20% at 60 ℃ to obtain a dry blank;
and 7, sintering the dry blank in a high-temperature furnace at 1620 ℃ to obtain the ZTA complex-phase ceramic, wherein the bulk density of the material is 3.95g/cm3, and the breaking strength is 498 MPa.
Example 2:
step 1, weighing 168.1g of Zr (NO3) 4.3H 2O and 9.83g of Y (NO3) 3.6H 2O, adding into 1681ml of deionized water, and stirring to dissolve to obtain a mixed solution; excess concentrated ammonia was added to adjust the pH to 11. And 3Y-ZrO2 precursor sol is generated. And filtering and drying the sol to obtain the 3Y-ZrO2 precursor xerogel.
Step 2, weighing 3.76g of methacrylamide polymer powder, 2.5g of polyacrylamide and 333ml of deionized water, adding the weighed materials and the xerogel prepared in the previous step into a ball milling tank of a planetary ball mill, setting the rotating speed to 600RPM, and carrying out rapid ball milling for 10min to obtain a premixed liquid;
step 3, weighing 1000g of alumina powder, adding the alumina powder into a ball milling tank of the premixed liquid, setting the rotation speed to 600rpm, and performing rapid ball milling for 10min to obtain alumina slurry with the viscosity of 1830mPa & s;
step 4, transferring the slurry obtained in the step 3 to a vacuum stirrer, and stirring for 20min in vacuum to obtain defoamed slurry;
step 5, injecting the defoamed slurry obtained in the step 4 into a grinding tool, standing at room temperature for 100min for forming, and demolding to obtain a wet blank;
step 6, transferring the wet blank into a temperature-adjusting debugging box, and respectively drying for 2 hours at the relative humidity of 95%, 75%, 50% and 20% at the temperature of 60 ℃ to obtain a dry blank with certain strength;
and 7, sintering the dry blank in a high-temperature furnace at 1620 ℃ to obtain the ZTA complex-phase ceramic, wherein the bulk density of the material is 3.97g/cm3, and the breaking strength is 511 MPa.
Example 3:
step 1, weighing 277.6g of Zr (NO3) 4.3H 2O and 16.2g of Y (NO3) 3.6H 2O, adding the weighed materials into 2776ml of deionized water, and stirring and dissolving to obtain a mixed solution; excess concentrated ammonia was added to adjust the pH to 11. Generating 3Y-ZrO2 precursor sol, filtering and drying the sol to obtain 3Y-ZrO2 precursor xerogel;
step 2, weighing 3.76g of methacrylamide polymer powder, 2.5g of polyacrylamide and 244ml of deionized water, adding the weighed materials and the xerogel prepared in the previous step into a ball milling tank of a planetary ball mill, setting the rotating speed at 600RPM, and carrying out rapid ball milling for 10min to obtain a premixed solution;
step 3, weighing 1000g of alumina powder, adding the alumina powder into a ball milling tank of the premixed liquid, setting the rotation speed to 600rpm, and performing rapid ball milling for 10min to obtain alumina slurry with the viscosity of 1970mPa & s;
step 4, transferring the alumina slurry obtained in the step 3 to a vacuum stirrer, and stirring for 20min in vacuum to obtain defoamed slurry;
step 5, injecting the defoamed slurry obtained in the step 4 into a grinding tool, standing at room temperature for 100min for forming, and demolding to obtain a wet blank;
step 6, transferring the wet blank into a temperature-adjusting debugging box, and drying the wet blank for 2 hours at the relative humidity of 95%, 75%, 50% and 20% at 60 ℃ respectively to obtain a dry blank;
and 7, sintering the dry blank in a high-temperature furnace at 1620 ℃ to obtain the ZTA complex-phase ceramic, wherein the bulk density of the material is 3.98g/cm3, and the breaking strength is 561 MPa.
Example 4:
step 1, weighing 355g of Zr (NO3) 4.3H 2O and 20.75g of Y (NO3) 3.6H 2O, adding the weighed materials into 3550ml of deionized water, and stirring to dissolve the materials to obtain a mixed solution; excess concentrated ammonia was added to adjust the pH to 11. Generating 3Y-ZrO2 precursor sol, filtering and drying the sol to obtain 3Y-ZrO2 precursor xerogel;
step 2, weighing 3.73g of methacrylamide polymer powder, 2.5g of polyacrylamide and 242ml of deionized water, adding the weighed materials and the xerogel prepared in the previous step into a ball milling tank of a planetary ball mill, setting the rotating speed to 600RPM, and carrying out rapid ball milling for 10min to obtain a premixed liquid;
step 3, weighing 1000g of alumina powder, adding the alumina powder into a ball milling tank of the premixed liquid, setting the rotating speed to 600rpm, and carrying out rapid ball milling for 10min to obtain alumina slurry with the viscosity of 1870mPa & s;
step 4, transferring the slurry obtained in the step 3 to a vacuum stirrer, and stirring for 20min in vacuum to obtain defoamed slurry;
step 5, injecting the slurry obtained in the step 4 into a grinding tool, standing at room temperature for 100min for forming, and demolding to obtain a wet blank;
step 6, transferring the wet blank into a temperature-adjusting debugging box, and respectively drying for 2 hours at the relative humidity of 95%, 75%, 50% and 20% at 60 ℃ to obtain a dry blank;
and 7, sintering the dry blank in a high-temperature furnace at 1620 ℃ to obtain the ZTA complex-phase ceramic, wherein the bulk density of the material is 4.01g/cm3, and the flexural strength is 547 MPa.
Example 5:
step 1, weighing 355g of Zr (NO3) 4.3H 2O and 20.75g of Y (NO3) 3.6H 2O, adding the weighed materials into 3550ml of deionized water, and stirring to dissolve the materials to obtain a mixed solution; excess concentrated ammonia was added to adjust the pH to 11. Generating 3Y-ZrO2 precursor sol, filtering and drying the sol to obtain 3Y-ZrO2 precursor xerogel;
step 2, weighing 3.81g of methacrylamide polymer powder, 2.54g of polyacrylamide and 292ml of deionized water, adding the weighed materials and the xerogel prepared in the previous step into a ball milling tank of a planetary ball mill, setting the rotating speed to 600RPM, and carrying out rapid ball milling for 10min to obtain a premixed solution;
step 3, weighing 1000g of alumina powder, adding the alumina powder into a ball milling tank of the premixed liquid, setting the rotating speed to 600rpm, and performing rapid ball milling for 10min to obtain alumina slurry with the viscosity of 1910mPa & s;
step 4, transferring the alumina slurry obtained in the step 3 to a vacuum stirrer, and stirring for 20min in vacuum to obtain defoamed slurry;
step 5, injecting the defoamed slurry obtained in the step 4 into a grinding tool, standing at room temperature for 100min for forming, and demolding to obtain a wet blank;
step 6, transferring the wet blank into a temperature-adjusting debugging box, and respectively drying for 2 hours at the relative humidity of 95%, 75%, 50% and 20% at 60 ℃ to obtain a dry blank;
and 7, sintering the dry blank in a high-temperature furnace at 1620 ℃ to obtain the ZTA complex-phase ceramic, wherein the bulk density of the material is 3.93g/cm3, and the breaking strength is 428 MPa.
Example 6:
step 1, weighing 355g of Zr (NO3) 4.3H 2O and 20.75g of Y (NO3) 3.6H 2O, adding the weighed materials into 3550ml of deionized water, and stirring to dissolve the materials to obtain a mixed solution; excess concentrated ammonia was added to adjust the pH to 11. Generating 3Y-ZrO2 precursor sol, filtering and drying the sol to obtain 3Y-ZrO2 precursor xerogel;
step 2, weighing 3.89g of methacrylamide polymer powder, 2.59g of polyacrylamide and 292ml of deionized water, adding the weighed materials and the xerogel prepared in the previous step into a ball milling tank of a planetary ball mill, setting the rotating speed to 600RPM, and carrying out rapid ball milling for 10min to obtain a premixed solution;
step 3, weighing 1000g of alumina powder, adding the alumina powder into a ball milling tank of the premixed liquid, setting the rotation speed to be 600rpm, and carrying out rapid ball milling for 10min to obtain alumina slurry with the viscosity of 1920mPa & s;
step 4, transferring the slurry obtained in the step 3 to a vacuum stirrer, and stirring for 20min in vacuum to obtain defoamed slurry;
step 5, injecting the slurry obtained in the step 4 into a grinding tool, standing at room temperature for 100min for forming, and demolding to obtain a wet blank;
step 6, transferring the wet blank into a temperature-adjusting debugging box, and respectively drying for 2 hours at the relative humidity of 95%, 75%, 50% and 20% at 60 ℃ to obtain a dry blank;
and 7, sintering the dry blank in a high-temperature furnace at 1620 ℃ to obtain the ZTA complex-phase ceramic, wherein the bulk density of the material is 3.95g/cm3, and the breaking strength is 521 MPa.
Example 7:
step 1, weighing 355g of Zr (NO3) 4.3H 2O and 20.75g of Y (NO3) 3.6H 2O, adding the weighed materials into 3550ml of deionized water, and stirring to dissolve the materials to obtain a mixed solution; excess concentrated ammonia was added to adjust the pH to 11. Generating 3Y-ZrO2 precursor sol, filtering and drying the sol to obtain 3Y-ZrO2 precursor xerogel;
step 2, weighing 3.96g of methacrylamide polymer powder, 2.64g of polyacrylamide and 316ml of deionized water, adding the weighed materials and the xerogel prepared in the previous step into a ball milling tank of a planetary ball mill, setting the rotating speed at 600RPM, and carrying out rapid ball milling for 10min to obtain a premixed liquid;
step 3, weighing 1000g of alumina powder, adding the alumina powder into a ball milling tank of the premixed liquid, setting the rotating speed to 600rpm, and performing rapid ball milling for 10min to obtain alumina slurry with the viscosity of 1980mPa & s;
step 4, transferring the alumina slurry obtained in the step 3 to a vacuum stirrer, and stirring for 20min in vacuum to obtain defoamed slurry;
step 5, injecting the defoamed slurry obtained in the step 4 into a grinding tool, standing at room temperature for 100min for forming, and demolding to obtain a wet blank;
step 6, transferring the wet blank into a temperature-adjusting debugging box, and respectively drying for 2 hours at the relative humidity of 95%, 75%, 50% and 20% at 60 ℃ to obtain a dry blank;
and 7, sintering the dry blank in a high-temperature furnace at 1620 ℃ to obtain the ZTA complex-phase ceramic, wherein the bulk density of the material is 3.92g/cm3, and the breaking strength is 409 MPa.
The invention provides a preparation method of ZTA complex phase ceramic, which can realize the preparation of parts with complex shapes, greatly reduce the use amount of organic additives, effectively avoid the glue discharging problems of cracking, surface peeling and the like in the glue discharging process, and prepare the high-performance complex phase ceramic with uniformly distributed second phase particles in a submicron form.
According to the invention, the zirconia precursor gel is introduced as the zirconia source and the gel reinforcing agent in the preparation stage of the premixed solution, the 3Y-ZrO2 is synthesized in situ in the sintering process, the uniform dispersion of ZrO2 in alumina is effectively realized, the effects of dispersion toughening and alumina grain growth inhibition are achieved, and the problems of giant crystal generation and uneven distribution of the second phase in the preparation of ZTA ceramic are solved. The method adopts the methacrylamide polymer aqueous solution as a gelling agent, and adds alumina to prepare gel slurry, so that the low-organic-content gel injection molding of the ZTA ceramic is realized, the prepared green body is easy to discharge gel, and the fired ZTA ceramic has the ZTA complex phase ceramic with high strength, high density, controllable crystal grains and excellent performance.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (8)
1. A preparation method of ZTA ceramic is characterized by comprising the following steps: step 1, preparing a 3Y-ZrO2 precursor xerogel; step 2, preparing a premixed solution: preparing a premixed solution from the precursor xerogel; step 3, mixing and ball milling: mixing the premixed liquid and performing ball milling to obtain slurry; step 4, defoaming the slurry: de-foaming the slurry; and 5, injection molding: injecting the defoaming slurry obtained in the step 4 into a model; step 6, demoulding and drying; and 7, sintering.
2. The method of claim 1, wherein the step 1 of preparing a xerogel of 3Y-ZrO2 precursor comprises the steps of: weighing a certain amount of Zr (NO3) 4.3H 2O and Y (NO3) 3.6H 2O, adding into deionized water, and uniformly stirring to obtain a zirconium oxide precursor solution; adding strong ammonia water to obtain 3Y-ZrO2 precursor gel solution; and filtering, washing and drying the gel solution to obtain the 3Y-ZrO2 precursor xerogel.
3. The method of claim 1 or 2, wherein in step 2, the premix is prepared by the steps of: weighing methacrylamide polymer powder, polyacrylamide, 3Y-ZrO2 precursor xerogel and deionized water, adding into a planetary ball mill, and ball-milling to obtain a premixed solution.
4. The method of claim 3, wherein step 3 comprises: and (3) weighing a certain amount of alumina powder and a small amount of deionized water, adding the alumina powder and the deionized water into the premixed liquid prepared in the step (2) according to the solid content or the fixed volume ratio, and performing rapid ball milling until the granularity reaches the required value to obtain the slurry for gel injection molding.
5. The method of claim 4, wherein step 4 comprises: and (4) transferring the slurry obtained in the step (3) to a vacuum device, and stirring and degassing in vacuum until bubbles disappear.
6. The method of claim 5, wherein step 5 comprises: and (4) injecting the slurry obtained in the step (4) into a prepared model, and curing the model in an environment with certain relative humidity and temperature until the slurry is solidified.
7. The method of claim 6, wherein step 6 comprises: and (5) demolding the blank obtained in the step (5), transferring the blank into a temperature and humidity adjusting box, setting the temperature and the relative humidity, and drying.
8. The method of claim 7, wherein step 7 comprises: and (4) transferring the dried green body obtained in the step (6) to a high-temperature kiln to sinter the ZTA ceramic.
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