CN110746196A - Hafnium oxide based ceramic core and preparation method thereof - Google Patents
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Abstract
The hafnium oxide-based ceramic core consists of hafnium oxide-based ceramic core powder and a plasticizer, wherein the hafnium oxide-based ceramic core powder consists of rare earth metal oxide, zirconium oxide, yttrium oxide, silicon oxide and hafnium oxide. The preparation method of the hafnium oxide-based ceramic core comprises the following steps: 1) preparing hafnium oxide-based ceramic core powder; 2) preparing a hafnium oxide-based ceramic core blank; 3, melting; 4) pressure injection; 5) and (4) roasting. The hafnium oxide based ceramic core and the preparation method thereof solve the problems that the existing silicon-based and aluminum-based ceramic cores have low high-temperature performance, impurities are introduced in the casting process and the like in the precision casting process of the alloy containing high-activity elements, so that the hafnium oxide based ceramic core with high temperature resistance and high purity is obtained.
Description
Technical Field
The invention belongs to the technical field of investment precision casting, and particularly relates to a hafnium oxide based ceramic core and a preparation method thereof.
Background
The development of aero-engines stems from the continuous breakthrough of new materials and new technologies. The improvement of the temperature bearing capability of the special metal turbine blade is urgent. In the prior art, for an active metal alloy casting process with high melting point and strong chemical activity, the existing silicon oxide and aluminum oxide can not be applied, and the hafnium oxide-based ceramic core has better high temperature resistance when the metal alloy is cast.
The invention provides a hafnium oxide-based ceramic core and a preparation method thereof, which can solve the problem of active metal alloy casting with high melting point and strong chemical activity, and the hafnium oxide can be dissolved in hydrofluoric acid and has good dissolution property in nitric acid, and simultaneously solves the related performances of the ceramic core in superalloy orientation and single crystal casting or eutectic alloy orientation casting.
Disclosure of Invention
Aiming at the problems that the high-temperature-resistant alloy of a hollow blade is more and more complex in the investment casting production technology in the prior precision casting, and a common material ceramic core cannot meet various physical and chemical properties in the alloy casting process, the scheme provides a hafnium oxide-based ceramic core and a preparation method thereof, aiming at solving the problems that the high-temperature properties of the prior silicon-based and aluminum-based ceramic cores are low, impurities are introduced in the casting process and the like in the alloy precision casting process containing high-activity elements, so that the hafnium oxide-based ceramic core with high temperature resistance and high purity is obtained, and the specific technical scheme is as follows:
the invention relates to a hafnium oxide-based ceramic core, which consists of hafnium oxide-based ceramic core powder and a plasticizer, wherein the mass ratio of the hafnium oxide-based ceramic core powder to the plasticizer is (12-18) of 100, the hafnium oxide-based ceramic core powder consists of rare earth metal oxide, zirconium oxide, yttrium oxide, silicon oxide and hafnium oxide, and the mass percentages are as follows: 5-20% of rare earth metal oxide, 10-20% of zirconium oxide, 10-25% of yttrium oxide, 2-10% of silicon oxide and the balance of hafnium oxide;
the rare earth metal oxide is a mixture of two or more of neodymium oxide, dysprosium oxide, erbium oxide, ytterbium oxide and cerium oxide;
the plasticizer is a mixture of more than three of paraffin, liquid paraffin, butyl stearate and PVB;
the particle size of the neodymium oxide, the dysprosium oxide, the erbium oxide, the ytterbium oxide and the cerium oxide is more than 120 meshes;
the particle size of the zirconium oxide, the silicon oxide and the yttrium oxide is 270-600 meshes;
the particle size of the hafnium oxide is 150-800 meshes;
the preparation method of the hafnium oxide based ceramic core comprises the following steps:
step 1, preparing hafnium oxide-based ceramic core powder:
weighing raw material powder of rare earth metal oxide, zirconium oxide, yttrium oxide, silicon oxide and hafnium oxide according to the proportion, premixing the rare earth metal oxide powder for 3-5 h, premixing the zirconium oxide and yttrium oxide powder for 3-5 h, adding the mixed rare earth metal oxide powder into the hafnium oxide powder for mixing for 4-8 h, then adding the silicon oxide powder for mixing for 2-5 h, finally adding the premixed mixture of zirconium oxide and yttrium oxide, and dispersing and mixing by using a mixer for 3-8 h to form hafnium oxide-based ceramic core powder for later use;
step 2, preparing a hafnium oxide-based ceramic core blank:
weighing hafnium oxide-based ceramic core powder and a plasticizer according to the mass ratio of the hafnium oxide-based ceramic core powder to the plasticizer of 100 (12-18), firstly putting the plasticizer into an oil bath cylinder with a stirring function, heating to 80-90 ℃ for melting, then stirring for 3-6h at the stirring speed of 80-100 rpm, then adding the hafnium oxide-based ceramic core powder into the melted plasticizer three times, stirring for 8-20h at 85-125 ℃, taking out the slurry and dishing, and cooling to room temperature to form a hafnium oxide-based ceramic core blank for later use;
and step 3, melting:
placing the hafnium oxide-based ceramic core blank in an oil bath charging barrel, heating to 75-110 ℃, melting, and stirring at the stirring speed of 50-250 rpm;
step 4, pressure injection:
performing injection molding by using a ceramic core injection molding machine according to the required product size structure to form a hafnium oxide-based ceramic core blank;
and step 5, roasting:
embedding the hafnium oxide-based ceramic core blank into a high-temperature-resistant mixed filler, roasting at a final sintering temperature of 1500-;
the preparation method of the hafnium oxide based ceramic core comprises the following steps:
in the step 5, the high-temperature resistant mixed filler is a mixture of zirconia powder and chopped zirconia ceramic fibers.
Compared with the prior art, the hafnium oxide based ceramic core and the preparation method thereof have the beneficial effects that:
firstly, for the casting of active metal alloy with high melting point and strong chemical activity, the existing silicon oxide and aluminum oxide can not be applied, and the hafnium oxide-based ceramic core has better high temperature resistance when the metal alloy is cast.
Secondly, the development of the hafnium oxide based ceramic core can solve the problem of active metal alloy casting with high melting point and strong chemical activity, and meanwhile, the hafnium oxide is soluble in hydrofluoric acid and has good dissolution in nitric acid. At the same time, HfO2The melting point is as high as 2850 ℃, the temperature is far above 1600 ℃, the linear expansion coefficient is small, and the tracer can also be used as a tracer of a ceramic core material, so that the flaw detection of a precise metal piece is facilitated.
And thirdly, the hafnium oxide based ceramic core can solve the relevant performance of the ceramic core in the process of superalloy orientation and single crystal casting or oriented casting of eutectic alloy.
Fourthly, the process flow is simple, the hot-pressing injection molding mode is adopted, waste products generated in the injection molding process can be recycled, and waste of high-price raw materials is avoided.
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to these examples.
Example 1
The hafnium oxide-based ceramic core comprises hafnium oxide-based ceramic core powder and a plasticizer, wherein the mass ratio of the hafnium oxide-based ceramic core powder to the plasticizer is 100:12, the hafnium oxide-based ceramic core powder comprises rare earth metal oxide, zirconium oxide, yttrium oxide, silicon oxide and hafnium oxide, and the mass percentages are as follows: 5% of rare earth metal oxide, 20% of zirconium oxide, 25% of yttrium oxide, 7% of silicon oxide and 43% of hafnium oxide;
the rare earth metal oxide is a mixture of ytterbium oxide and cerium oxide, and the mass ratio of ytterbium oxide to cerium oxide is 1: 1.5;
the plasticizer is a mixture of paraffin and liquid paraffin, and the mass ratio of the paraffin to the liquid paraffin is 2: 1;
the granularity of the ytterbium oxide and the cerium oxide is 150 meshes;
the granularity of the zirconium oxide, the silicon oxide and the yttrium oxide is 350 meshes;
the particle size of the hafnium oxide is 250 meshes;
a method of making a hafnium oxide based ceramic core, comprising the steps of:
step 1, preparing hafnium oxide-based ceramic core powder:
weighing 50g of rare earth metal oxide, 200g of zirconium oxide, 250g of yttrium oxide, 70g of silicon oxide and 430g of hafnium oxide according to a ratio, premixing 3h of rare earth metal oxide powder, premixing 3.5h of zirconium oxide and yttrium oxide powder, adding the mixed rare earth metal oxide powder into hafnium oxide powder, mixing for 5.5h, adding silicon oxide powder, mixing for 4h, adding the premixed zirconium oxide and yttrium oxide mixture, and dispersing and mixing by using a mixer for 4h to form a hafnium oxide-based ceramic powder core for later use;
step 2, preparing a hafnium oxide-based ceramic core blank:
weighing 1000g of hafnium oxide-based ceramic core powder and 120g of plasticizer according to the proportion, firstly putting the plasticizer into an oil bath cylinder with a stirring function, heating to 80 ℃ for melting, then stirring for 4h at a stirring speed of 80rpm, then adding the hafnium oxide-based ceramic core powder into the melted plasticizer three times, stirring for 10h at 100 ℃ at a stirring speed of 90rpm, finally taking out slurry and dishing, and cooling to room temperature to form a hafnium oxide-based ceramic core blank for later use;
and step 3, melting:
placing the hafnium oxide-based ceramic core blank in an oil bath charging barrel, heating to 90 ℃, melting, and stirring at the stirring speed of 150 rpm;
step 4, pressure injection:
performing injection molding by using a ceramic core injection molding machine according to the required product size structure to form a hafnium oxide-based ceramic core blank;
and step 5, roasting:
embedding the hafnium oxide-based ceramic core blank into a high-temperature-resistant mixed filler, roasting at a final sintering temperature of 1700 ℃, keeping the temperature for 3.5 hours, and cooling to room temperature to obtain a hafnium oxide-based ceramic core;
the test is carried out according to the requirement of the HB5353.3 standard method, and the high-temperature breaking strength of the sample can reach more than 20MPa under the condition of 1540 ℃/20 min.
Example 2
The hafnium oxide-based ceramic core comprises hafnium oxide-based ceramic core powder and a plasticizer, wherein the mass ratio of the hafnium oxide-based ceramic core powder to the plasticizer is 100:15, the hafnium oxide-based ceramic core powder comprises rare earth metal oxide, zirconium oxide, yttrium oxide, silicon oxide and hafnium oxide, and the mass percentages are as follows: 10% of rare earth metal oxide, 15% of zirconium oxide, 23% of yttrium oxide, 8% of silicon oxide and 44% of hafnium oxide;
the rare earth metal oxide is a mixture of neodymium oxide, dysprosium oxide and cerium oxide, and the mass ratio of the neodymium oxide to the dysprosium oxide to the cerium oxide is 0.5:1.5: 2;
the plasticizer is a mixture of paraffin, liquid paraffin and butyl stearate, and the mass ratio of the paraffin to the liquid paraffin to the butyl stearate is 7:3: 5;
the particle size of the neodymium oxide, the dysprosium oxide and the cerium oxide is 200 meshes;
the granularity of the zirconium oxide, the silicon oxide and the yttrium oxide is 300 meshes;
the particle size of the hafnium oxide is 350 meshes;
a method of making a hafnium oxide based ceramic core, comprising the steps of:
step 1, preparing hafnium oxide-based ceramic core powder:
weighing 100g of rare earth metal oxide, 150g of zirconium oxide, 230g of yttrium oxide, 80g of silicon oxide and 440g of hafnium oxide according to the proportion, premixing 4h of rare earth metal oxide powder, premixing 4h of zirconium oxide and yttrium oxide powder, adding the mixed rare earth metal oxide powder into hafnium oxide powder, mixing for 6h, adding silicon oxide powder, mixing for 3h, adding the premixed zirconium oxide and yttrium oxide mixture, and dispersing and mixing by using a mixer for 5h to form hafnium oxide-based ceramic core powder for later use;
step 2, preparing a hafnium oxide-based ceramic core blank:
weighing 1000g of hafnium oxide-based ceramic core powder and 150g of plasticizer according to the ratio, firstly putting the plasticizer into an oil bath cylinder with a stirring function, heating to 85 ℃ for melting, then stirring for 5h at a stirring speed of 90rpm, then adding the hafnium oxide-based ceramic core powder into the melted plasticizer three times, stirring for 9h at 85 ℃ at a stirring speed of 100rpm, finally taking out the slurry, dishing, and cooling to room temperature to form a hafnium oxide-based ceramic core blank for later use;
and step 3, melting:
placing the hafnium oxide-based ceramic core blank in an oil bath charging barrel, heating to 100 ℃, melting, and stirring at the stirring speed of 150 rpm;
step 4, pressure injection:
performing injection molding by using a ceramic core injection molding machine according to the required product size structure to form a hafnium oxide-based ceramic core blank;
and step 5, roasting:
embedding the hafnium oxide-based ceramic core blank into a high-temperature-resistant mixed filler, roasting at a final sintering temperature of 1650 ℃, keeping the temperature for 5 hours, and cooling to room temperature to obtain the hafnium oxide-based ceramic core;
according to the requirement of the HB5353.3 standard method, the high-temperature breaking strength of the sample can reach more than 20MPa under the condition of 1540 ℃/20 min.
Example 3
The hafnium oxide-based ceramic core comprises hafnium oxide-based ceramic core powder and a plasticizer, wherein the mass ratio of the hafnium oxide-based ceramic core powder to the plasticizer is 100:18, the hafnium oxide-based ceramic core powder comprises rare earth metal oxide, zirconium oxide, yttrium oxide, silicon oxide and hafnium oxide, and the mass percentages are as follows: 20% of rare earth metal oxide, 10% of zirconium oxide, 18% of yttrium oxide, 10% of silicon oxide and 42% of hafnium oxide;
the rare earth metal oxide is a mixture of erbium oxide, ytterbium oxide and cerium oxide, and the mass ratio of erbium oxide to ytterbium oxide to cerium oxide is 2:2: 3.5;
the plasticizer is a mixture of paraffin, liquid paraffin, butyl stearate and PVB, and the mass ratio of the paraffin to the liquid paraffin to the butyl stearate to the PVB is 9:5:2: 2;
the grain sizes of the erbium oxide, the ytterbium oxide and the cerium oxide are 200 meshes;
the granularity of the zirconium oxide, the silicon oxide and the yttrium oxide is 350 meshes;
the particle size of the hafnium oxide is 250 meshes;
a method of making a hafnium oxide based ceramic core, comprising the steps of:
step 1, preparing hafnium oxide-based ceramic core powder:
weighing 50g of rare earth metal oxide, 200g of zirconium oxide, 250g of yttrium oxide, 70g of silicon oxide and 430g of hafnium oxide according to a ratio, premixing 5h of rare earth metal oxide powder, premixing 4.5h of zirconium oxide and yttrium oxide powder, adding the mixed rare earth metal oxide powder into hafnium oxide powder, mixing for 7h, adding silicon oxide powder, mixing for 3.5h, adding the premixed zirconium oxide and yttrium oxide mixture, and dispersing and mixing by using a mixer for 6h to form a hafnium oxide-based ceramic powder core for later use;
step 2, preparing a hafnium oxide-based ceramic core blank:
weighing 1000g of hafnium oxide-based ceramic core powder and 180g of plasticizer according to the ratio, firstly putting the plasticizer into an oil bath cylinder with a stirring function, heating to 80 ℃ for melting, then stirring for 4h at a stirring speed of 80rpm, then adding the hafnium oxide-based ceramic core powder into the melted plasticizer three times, stirring for 10h at 100 ℃ at a stirring speed of 90rpm, finally taking out slurry and dishing, and cooling to room temperature to form a hafnium oxide-based ceramic core blank for later use;
and step 3, melting:
placing the hafnium oxide-based ceramic core blank in an oil bath charging barrel, heating to 100 ℃, melting, and stirring at the stirring speed of 120 rpm;
step 4, pressure injection:
performing injection molding by using a ceramic core injection molding machine according to the required product size structure to form a hafnium oxide-based ceramic core blank;
and step 5, roasting:
embedding the hafnium oxide-based ceramic core blank into a high-temperature-resistant mixed filler, roasting at a final sintering temperature of 1550 ℃, keeping the temperature for 6 hours, and cooling to room temperature to obtain a hafnium oxide-based ceramic core;
according to the requirement of the HB5353.3 standard method, the high-temperature breaking strength of the sample can reach more than 20MPa under the condition of 1540 ℃/20 min.
Claims (8)
1. The hafnium oxide-based ceramic core comprises, by mass, 100 parts (12-18) of hafnium oxide-based ceramic core powder and a plasticizer, wherein the hafnium oxide-based ceramic core powder comprises, by mass: 5-20% of rare earth metal oxide, 10-20% of zirconium oxide, 10-25% of yttrium oxide, 2-10% of silicon oxide and the balance of hafnium oxide.
2. The hafnium oxide-based ceramic core of claim 1, wherein the rare earth metal oxide is a mixture of two or more of neodymium oxide, dysprosium oxide, erbium oxide, ytterbium oxide, and cerium oxide.
3. The hafnium oxide based ceramic core of claim 1, wherein the plasticizer is a mixture of three or more of paraffin wax, liquid paraffin wax, butyl stearate, and PVB.
4. The hafnium oxide based ceramic core of claim 1, wherein the neodymium oxide, dysprosium oxide, erbium oxide, ytterbium oxide, cerium oxide have a particle size of 120 mesh or larger.
5. The hafnium oxide based ceramic core of claim 1, wherein the zirconia, silica, yttria have a particle size of 270 to 600 mesh.
6. The hafnium oxide based ceramic core of claim 1, wherein the hafnium oxide has a particle size of 150 to 800 mesh.
7. The method of making the hafnium oxide based ceramic core of claim 1, comprising the steps of:
step 1, preparing hafnium oxide-based ceramic core powder:
weighing raw material powder of rare earth metal oxide, zirconium oxide, yttrium oxide, silicon oxide and hafnium oxide according to the proportion, premixing the rare earth metal oxide powder for 3-5 h, premixing the zirconium oxide and yttrium oxide powder for 3-5 h, adding the mixed rare earth metal oxide powder into the hafnium oxide powder for mixing for 4-8 h, then adding the silicon oxide powder for mixing for 2-5 h, finally adding the premixed mixture of zirconium oxide and yttrium oxide, and dispersing and mixing by using a mixer for 3-8 h to form hafnium oxide-based ceramic core powder for later use;
step 2, preparing a hafnium oxide-based ceramic core blank:
weighing hafnium oxide-based ceramic core powder and a plasticizer according to the mass ratio of the hafnium oxide-based ceramic core powder to the plasticizer of 100 (12-18), firstly putting the plasticizer into an oil bath cylinder with a stirring function, heating to 80-90 ℃ for melting, then stirring for 3-6h at the stirring speed of 80-100 rpm, then adding the hafnium oxide-based ceramic core powder into the melted plasticizer three times, stirring for 8-20h at 85-125 ℃, taking out the slurry and dishing, and cooling to room temperature to form a hafnium oxide-based ceramic core blank for later use;
and step 3, melting:
placing the hafnium oxide-based ceramic core blank in an oil bath charging barrel, heating to 75-110 ℃, melting, and stirring at the stirring speed of 50-250 rpm;
step 4, pressure injection:
performing injection molding by using a ceramic core injection molding machine according to the required product size structure to form a hafnium oxide-based ceramic core blank;
and step 5, roasting:
embedding the hafnium oxide-based ceramic core blank into a high-temperature-resistant mixed filler, roasting at a final sintering temperature of 1500-1750 ℃, preserving heat for 3.5-7 h, and cooling to room temperature to obtain the hafnium oxide-based ceramic core.
8. The method of claim 7, wherein in step 5, the refractory hybrid filler is a mixture of zirconia powder and chopped zirconia ceramic fibers.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111423230A (en) * | 2020-06-11 | 2020-07-17 | 长沙华脉新材料有限公司 | Multiple rare earth co-doped toughened hafnium oxide ceramic material and preparation method thereof |
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| CN114478004A (en) * | 2021-12-31 | 2022-05-13 | 重庆材料研究院有限公司 | Preparation method of hafnium oxide ceramic product |
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