CN112239369A - Gradient hollow ceramic core and preparation method thereof - Google Patents
Gradient hollow ceramic core and preparation method thereof Download PDFInfo
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- CN112239369A CN112239369A CN202011127400.0A CN202011127400A CN112239369A CN 112239369 A CN112239369 A CN 112239369A CN 202011127400 A CN202011127400 A CN 202011127400A CN 112239369 A CN112239369 A CN 112239369A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 148
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000005350 fused silica glass Substances 0.000 claims abstract description 69
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000002002 slurry Substances 0.000 claims abstract description 31
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 29
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 29
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 29
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000005642 Oleic acid Substances 0.000 claims abstract description 29
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 29
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 29
- 239000012188 paraffin wax Substances 0.000 claims abstract description 29
- 239000004698 Polyethylene Substances 0.000 claims abstract description 28
- 235000013871 bee wax Nutrition 0.000 claims abstract description 28
- 239000012166 beeswax Substances 0.000 claims abstract description 28
- -1 polyethylene Polymers 0.000 claims abstract description 28
- 229920000573 polyethylene Polymers 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 229920001169 thermoplastic Polymers 0.000 claims abstract description 25
- 239000004416 thermosoftening plastic Substances 0.000 claims abstract description 25
- 229910052845 zircon Inorganic materials 0.000 claims abstract description 21
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 238000007731 hot pressing Methods 0.000 claims abstract description 17
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001723 curing Methods 0.000 claims abstract description 9
- 238000009740 moulding (composite fabrication) Methods 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 238000002347 injection Methods 0.000 claims description 34
- 239000007924 injection Substances 0.000 claims description 34
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 26
- 239000011812 mixed powder Substances 0.000 claims description 24
- 239000001993 wax Substances 0.000 claims description 22
- 238000001746 injection moulding Methods 0.000 claims description 20
- 238000004321 preservation Methods 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 17
- 239000011819 refractory material Substances 0.000 claims description 17
- 239000010410 layer Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 15
- 239000011230 binding agent Substances 0.000 claims description 10
- 239000004014 plasticizer Substances 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000006082 mold release agent Substances 0.000 claims description 8
- 239000002344 surface layer Substances 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims 1
- 239000011162 core material Substances 0.000 description 151
- 238000004519 manufacturing process Methods 0.000 description 16
- 239000002245 particle Substances 0.000 description 8
- 238000005266 casting Methods 0.000 description 6
- 238000005495 investment casting Methods 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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Abstract
The invention discloses a gradient hollow ceramic core, which consists of the following components in percentage by mass, 65-75% of fused quartz; 10 to 30 percent of zircon; 5% -30% of white paraffin; 0.5 to 5 percent of diethyl phthalate; 0.5 to 5 percent of beeswax; 0.05 to 1 percent of polyethylene; 0.05 to 1 percent of oleic acid; 5-10% of high-temperature resistant silica sol, and the total amount is 100%. The invention also discloses a preparation method of the gradient hollow ceramic core, which comprises the following steps: weighing each component in advance according to mass percentage; step 1: preparing thermoplastic ceramic slurry; step 2: hot-pressing and injecting to obtain a formed ceramic core blank; and step 3: sintering, heating, curing and forming. The method solves the problems of long ceramic core removing time and low core removing efficiency, and has the advantages of low cost, simple preparation process and convenient popularization.
Description
Technical Field
The invention belongs to the technical field of precision casting, relates to a gradient hollow ceramic core and also relates to a preparation method of the gradient hollow ceramic core.
Background
With the rapid development of aviation, aerospace and industrial gas turbine technologies, the gas temperature of turbine engines is increasing, thus requiring an increasing ability of turbine blades to withstand high temperatures. In view of this, superalloy turbine blades are slowly being transformed from solid to hollow in construction to accommodate the application of air cooling technology. Investment casting of high temperature alloys is one of the major techniques currently used to manufacture hollow turbine blades, and the prerequisite for this technique is the production of ceramic cores and shells with good performance.
At present, high-temperature alloy with higher price is generally adopted for investment casting in the manufacturing of high-temperature turbine blades, and the structure is usually a hollow structure. The whole production process from core pressing to the final casting finished product is longer, the manufacturing difficulty is greatly increased, the blade qualification rate is relatively low, and in addition, the number of single turbine blades is large, so that the requirement on high-temperature turbine blade castings in the engine development process is large, and the delivery of high-temperature turbine blades becomes one of bottlenecks in the engine development process.
Meanwhile, the ceramic core can generate thermal interaction and certain mechanical impact in production links such as investment casting wax pattern pressing, shell coating, pouring and the like, and if the strength and the size precision of the core can not meet the requirements, cracks can occur, so that the problems of core breaking and core deviation can occur. The bearing condition of the casting mold is generally 1100-1350 ℃, and higher requirements on the core material and the structure should be met. Therefore, the ceramic core meeting the requirement of the casting process of the turbine blade is prepared, and the casting yield of the blade is improved. On one hand, a large amount of waste loss and development cost can be saved, and on the other hand, the development period of the model of the aero-engine can be effectively shortened.
Accordingly, there is an urgent need to develop a gradient hollow ceramic core having a more complex shape and superior performance so as to greatly facilitate the application of high performance cast high temperature alloys to gas turbine blades.
Disclosure of Invention
The invention aims to provide a gradient hollow ceramic core, which solves the problems of long ceramic core removing time and low core removing efficiency in the prior art.
The invention also aims to provide a preparation method of the gradient hollow ceramic core, which solves the technical problem in the aspect of ceramic core preparation in the prior art.
The technical scheme adopted by the invention is that the gradient hollow ceramic core comprises the following components in percentage by mass, namely 65-75% of fused quartz; 10 to 30 percent of zircon; 5% -30% of white paraffin; 0.5 to 5 percent of diethyl phthalate; 0.5 to 5 percent of beeswax; 0.05 to 1 percent of polyethylene; 0.05 to 1 percent of oleic acid; 5-10% of high-temperature resistant silica sol, and the total amount is 100%.
The invention adopts another technical scheme that the preparation method of the gradient hollow ceramic core is implemented according to the following steps:
the preparation method comprises the following steps: weighing the following components in percentage by mass: 65% -75% of fused quartz; 10-30% of zircon; 5-30% of white paraffin; 0.5 to 5 percent of diethyl phthalate; 0.5-5% of beeswax; 0.05 to 1 percent of polyethylene; 0.05 to 1 percent of oleic acid; 5-10% of high-temperature resistant silica sol, the total amount is 100%; 10% of the total fused quartz is divided into square fused quartz, 10% of the total fused quartz is divided into refractory materials, and the rest 80% of the fused quartz is used for preparing fused quartz powder;
step 1: preparation of thermoplastic ceramic slurry
1.1) putting white paraffin, diethyl phthalate, beeswax and polyethylene into a stirrer, heating to 50-200 ℃, and preparing a wax core after the white paraffin, the diethyl phthalate, the beeswax and the polyethylene are completely melted;
1.2) taking fused quartz powder, zircon powder and square fused quartz, sequentially putting the three raw materials into a ball milling tank for ball milling, and putting the mixed powder into an oven to dry for 0.5-5h at the temperature of 100-; taking out the mixed powder in the oven, and uniformly mixing the mixed powder with the melted plasticizer and the melted oleic acid; controlling the stirring speed to be 100-600r/min, and stirring for 5-20h to obtain thermoplastic ceramic slurry; 5-10% of high-temperature resistant silica sol is used as a binder to ensure that each layer of gradient structure of the ceramic core is compact;
step 2: hot-pressing and injecting to obtain a formed ceramic core blank,
extruding a refractory material with the grain diameter of 300-600 meshes into the surface layer of the thermoplastic ceramic slurry for preforming, performing a pressing process by using a ceramic core high-pressure injection molding machine, putting the ceramic core high-pressure injection molding machine into a charging basket of a hot-pressing injection molding machine, heating the ceramic core high-pressure injection molding machine to a molten state at the temperature of 50-200 ℃, and performing injection molding by using oleic acid as a mold release agent; putting the wet core which is just demoulded into a correction mould under the wet condition, and pressurizing by a press machine to correct the size to obtain a ceramic core blank;
and step 3: sintering, heating, curing and forming
And (3) loading the prepared ceramic core blank into a ceramic groove, performing gradient temperature rise and heat preservation on the melting points corresponding to different components, wherein the heat preservation time is different according to different component contents to obtain the gradient hollow ceramic core, and thus obtaining the ceramic core.
The beneficial effects of the invention are that the invention comprises the following aspects:
1) the silica-based core is used, so that the core forming rate is low, the silica-based core is not deformed, displaced or cracked, the shrinkage rate is low, the high-temperature strength is good, the high-temperature thermal stability is good, the dimensional accuracy is high, a thin-wall casting with a complex cavity channel can be manufactured, the wall thickness is uniform, and the silica-based core is particularly suitable for manufacturing high-temperature-resistant gas turbine blades.
2) By adopting the gradient hollow ceramic core structure, the problems of long ceramic core removing time and low core removing efficiency are solved, so that the production efficiency of the precision casting is greatly improved.
3) The ceramic powder is bonded by using the binder, and the surface of the core is coated with the small-particle-size refractory material, so that the defects of surface cracks, short shots, white stubbles and the like of the core can be avoided, the bending strength and the toughness of the core are improved, and the surface of the core is densified and smoothed. The selected raw materials are wide in source, low in cost, simple in preparation process and convenient to popularize.
Drawings
FIG. 1 is a schematic view of the state during the production by the process of the present invention.
In the figure, 1 is a wax core, 2 is a bonding layer, 3 is a gradient hollow ceramic core, and 4 is a wax hole row.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The gradient hollow ceramic core disclosed by the invention comprises the following components in percentage by mass: 65% -75% of fused quartz; 10 to 30 percent of zircon; 5% -30% of white paraffin; 0.5 to 5 percent of diethyl phthalate; 0.5 to 5 percent of beeswax; 0.05 to 1 percent of polyethylene; 0.05 to 1 percent of oleic acid; 5-10% of high-temperature resistant silica sol, and the total amount is 100%.
Wherein, the fused quartz is used as the powder of the core substrate; white paraffin and diethyl phthalate as plasticizers; zircon was used as the sintering catalyst. Oleic acid is used as one of release agents, high-temperature-resistant silica sol is used as one of binders, and during sintering, a plasticizer begins to volatilize at a low-temperature stage, so that a large number of holes are generated inside the ceramic core, the porosity of the core is improved, and the core stripping rate of the core is accelerated.
The preparation method of the gradient hollow ceramic core is implemented according to the following steps:
the preparation method comprises the following steps: weighing the following components in percentage by mass: 65% -75% of fused quartz; 10-30% of zircon; 5-30% of white paraffin; 0.5 to 5 percent of diethyl phthalate; 0.5-5% of beeswax; 0.05 to 1 percent of polyethylene; 0.05 to 1 percent of oleic acid; 5-10% of high-temperature resistant silica sol, the total amount is 100%; 10% of the total fused quartz is divided into square fused quartz, 10% of the total fused quartz is divided into refractory materials, and the rest 80% of the fused quartz is used for preparing fused quartz powder;
step 1: preparation of thermoplastic ceramic slurry
1.1) putting white paraffin, diethyl phthalate, beeswax and polyethylene into a stirrer, heating to 50-200 ℃, and preparing a wax core after the white paraffin, the diethyl phthalate, the beeswax and the polyethylene are completely melted; the wax core is used for being placed in the inner layer of the ceramic core.
1.2) taking fused quartz powder, zircon powder and square fused quartz with different particle diameters, sequentially putting the three raw materials into a ball milling tank, adding zirconia balls with the diameter of 5-30mm, wherein the mass ratio of the three raw materials to the zirconia balls is 3: 2, after fully ball-milling for 0.5-5h at room temperature, putting the mixed powder into an oven to be dried for 0.5-5h at the temperature of 100-; taking out the mixed powder in the oven, uniformly mixing the mixed powder with the melted plasticizer and the melted oleic acid, and manufacturing the outer layer of the ceramic core in a gradient manner; controlling the stirring speed to be 100-600r/min, and stirring for 5-20h to ensure that the slurry components are uniform, and the core performance is stable to obtain the thermoplastic ceramic slurry; 5-10% of high-temperature-resistant silica sol is used as a binder, so that each layer of gradient structure of the ceramic core is compact and obvious in distinction;
step 2: hot-pressing and injecting to obtain a formed ceramic core blank,
extruding a refractory material with the grain diameter of 300-600 meshes into the surface layer of the thermoplastic ceramic slurry for preforming, performing a pressing process by using a ceramic core high-pressure injection molding machine, putting the ceramic core high-pressure injection molding machine into a charging basket of a hot-pressing injection molding machine, heating the ceramic core high-pressure injection molding machine to a molten state at 50-200 ℃, performing injection molding, and adopting oleic acid as a mold release agent, wherein the injection pressure is 0.5-5MPa, the pressure maintaining time is 5-50s, and the injection temperature is room temperature; and (3) putting the wet core which is just stripped into a correcting mould under the wet condition, and pressurizing by using a press machine to correct the size so as to ensure that the wet core has good size and does not generate phenomena of short shot and crack, thereby obtaining a ceramic core blank.
And step 3: sintering, heating, curing and forming
Placing the prepared ceramic core blank into a ceramic groove, performing gradient temperature rise and heat preservation on melting points corresponding to different components, keeping the temperature rise speed at 200 ℃/h according to different component contents, and preserving the heat for 10-20min after continuously raising the temperature for 1 h; when the temperature is raised to 600 ℃, preserving the heat for 2 hours to ensure that the wax core in the ceramic core is completely removed and becomes a hollow gradient structure; when the temperature is raised to 1400 ℃ to reach the final sintering temperature, the mixture is sintered for 4 hours in a heat preservation way; and then cooling to 200-500 ℃ at the speed of 100 ℃/h, and then cooling along with the furnace until the temperature reaches room temperature, and taking out to obtain the gradient hollow ceramic core with the densified and smoothed surface.
Referring to fig. 1, a schematic diagram of a state in the manufacturing process of the method of the present invention is shown, wherein an adhesive layer 2 is arranged between a gradient hollow ceramic core 3 and a wax core 1, and the wax core 1 is dewaxed and then discharged from a wax discharge hole 4, so as to form the hollow ceramic core.
Example 1
The preparation method comprises the following steps: weighing the following components in percentage by mass: 65% of fused quartz; 12% of white paraffin; 2% of diethyl phthalate; 2% of beeswax; 1% of polyethylene; 17% of zircon; 1% of oleic acid; the total amount is 100%. 10% of the total fused quartz is divided into square fused quartz, 10% of the total fused quartz is divided into refractory materials, and the rest 80% of the fused quartz is used for preparing fused quartz powder;
step 1: preparation of thermoplastic ceramic slurry
1.1) putting white paraffin, diethyl phthalate, beeswax and polyethylene into a stirrer, heating to 120 ℃, and preparing a wax core after the white paraffin, the diethyl phthalate, the beeswax and the polyethylene are completely melted;
1.2) taking fused quartz powder, zircon powder and square fused quartz with different particle diameters, sequentially putting the three raw materials into a ball milling tank, adding zirconia balls with the diameter of 10mm, wherein the mass ratio of the three raw materials to the zirconia balls is 3: 2, after fully ball-milling for 1h at room temperature, putting the mixed powder into an oven to dry for 2h at the temperature of 200 ℃; taking out the mixed powder in the oven, uniformly mixing the mixed powder with the melted plasticizer and the melted oleic acid, and manufacturing the outer layer of the ceramic core in a gradient manner; controlling the stirring speed to be 400r/min, and stirring for 12h to ensure that the slurry components are uniform, and the core performance is stable to obtain the thermoplastic ceramic slurry; 8% of high-temperature resistant silica sol is used as a binder, so that each layer of gradient structure of the ceramic core is compact and obvious in distinction;
step 2: hot-pressing and injecting to obtain a formed ceramic core blank,
extruding a refractory material with the particle size of 300 meshes into a surface layer of thermoplastic ceramic slurry for preforming, performing a pressing process by using a ceramic core high-pressure injection machine, putting the ceramic core high-pressure injection machine into a charging basket of a hot-pressing injection molding machine, heating the ceramic core high-pressure injection machine to a molten state at 90 ℃, performing injection, and taking oleic acid as a mold release agent, wherein the injection pressure is 3MPa, the pressure maintaining time is 30s, and the injection temperature is room temperature; and (3) putting the wet core which is just stripped into a correcting mould under the wet condition, and pressurizing by using a press machine to correct the size so as to ensure that the wet core has good size and does not generate phenomena of short shot and crack, thereby obtaining a ceramic core blank.
And step 3: sintering, heating, curing and forming
Loading the prepared ceramic core blank into a ceramic groove, performing gradient temperature rise and heat preservation on melting points corresponding to different components, keeping the temperature rise speed at 150 ℃/h according to different component contents, and preserving heat for 15min after continuously raising the temperature for 1 h; when the temperature is raised to 600 ℃, preserving the heat for 2 hours to ensure that the wax core in the ceramic core is completely removed and becomes a hollow gradient structure; when the temperature is raised to 1400 ℃ to reach the final sintering temperature, the mixture is sintered for 4 hours in a heat preservation way; and then cooling to 400 ℃ at the speed of 100 ℃/h, then cooling along with the furnace until the temperature reaches room temperature, and taking out to obtain the gradient hollow ceramic core with the densified and smoothed surface.
Example 2
The preparation method comprises the following steps: weighing the following components in percentage by mass: 67% of fused quartz; 13% of white paraffin; 2% of diethyl phthalate; 2% of beeswax; 0.05% of polyethylene; 18% of zircon; oleic acid 0.05%; the total amount is 100%. 10% of the total fused quartz is divided into square fused quartz, 10% of the total fused quartz is divided into refractory materials, and the rest 80% of the fused quartz is used for preparing fused quartz powder;
step 1: preparation of thermoplastic ceramic slurry
1.2) putting white paraffin, diethyl phthalate, beeswax and polyethylene into a stirrer, heating to 60 ℃, and preparing a wax core after the white paraffin, the diethyl phthalate, the beeswax and the polyethylene are completely melted;
1.2) taking fused quartz powder, zircon powder and square fused quartz with different particle diameters, sequentially putting the three raw materials into a ball milling tank, adding zirconia balls with the diameter of 5mm, wherein the mass ratio of the three raw materials to the zirconia balls is 3: 2, after fully ball-milling for 0.5h at room temperature, putting the mixed powder into an oven to dry for 5h at 120 ℃; taking out the mixed powder in the oven, uniformly mixing the mixed powder with the melted plasticizer and the melted oleic acid, and manufacturing the outer layer of the ceramic core in a gradient manner; controlling the stirring speed to be 100r/min, and stirring for 20h to ensure that the slurry components are uniform, and the core performance is stable to obtain the thermoplastic ceramic slurry; 5% of high-temperature resistant silica sol is used as a binder, so that each layer of gradient structure of the ceramic core is compact and obvious in distinction;
step 2: hot-pressing and injecting to obtain a formed ceramic core blank,
extruding a refractory material with the grain diameter of 400 meshes into a surface layer of thermoplastic ceramic slurry for preforming, performing a pressing process by using a ceramic core high-pressure injection machine, putting the ceramic core high-pressure injection machine into a charging basket of a hot-pressing injection molding machine, heating the ceramic core high-pressure injection machine to a molten state at 60 ℃, performing injection, and adopting oleic acid as a mold release agent, wherein the injection pressure is 1MPa, the pressure maintaining time is 40s, and the injection temperature is room temperature; and (3) putting the wet core which is just stripped into a correcting mould under the wet condition, and pressurizing by using a press machine to correct the size so as to ensure that the wet core has good size and does not generate phenomena of short shot and crack, thereby obtaining a ceramic core blank.
And step 3: sintering, heating, curing and forming
Loading the prepared ceramic core blank into a ceramic groove, performing gradient temperature rise and heat preservation on melting points corresponding to different components, keeping the temperature rise speed at 120 ℃/h according to different component contents, and preserving heat for 20min after continuously raising the temperature for 1 h; when the temperature is raised to 600 ℃, preserving the heat for 2 hours to ensure that the wax core in the ceramic core is completely removed and becomes a hollow gradient structure; when the temperature is raised to 1400 ℃ to reach the final sintering temperature, the mixture is sintered for 4 hours in a heat preservation way; and then cooling to 200 ℃ at the speed of 100 ℃/h, then cooling along with the furnace until the temperature reaches room temperature, and taking out to obtain the gradient hollow ceramic core with the densified and smoothed surface.
Example 3
The preparation method comprises the following steps: weighing the following components in percentage by mass: 68% of fused quartz; 14% of white paraffin; 1% of diethyl phthalate; 1% of beeswax; 0.05% of polyethylene; 15% of zircon; oleic acid 0.05%; the total amount is 100%. 10% of the total fused quartz is divided into square fused quartz, 10% of the total fused quartz is divided into refractory materials, and the rest 80% of the fused quartz is used for preparing fused quartz powder;
step 1: preparation of thermoplastic ceramic slurry
1.3) putting white paraffin, diethyl phthalate, beeswax and polyethylene into a stirrer, heating to 150 ℃, and preparing a wax core after the white paraffin, the diethyl phthalate, the beeswax and the polyethylene are completely melted;
1.2) taking fused quartz powder, zircon powder and square fused quartz with different particle diameters, sequentially putting the three raw materials into a ball milling tank, adding zirconia balls with the diameter of 15mm, wherein the mass ratio of the three raw materials to the zirconia balls is 3: 2, after fully ball-milling for 4 hours at room temperature, putting the mixed powder into an oven to dry for 2 hours at the temperature of 250 ℃; taking out the mixed powder in the oven, uniformly mixing the mixed powder with the melted plasticizer and the melted oleic acid, and manufacturing the outer layer of the ceramic core in a gradient manner; controlling the stirring speed to be 500r/min, and stirring for 8h to ensure that the slurry components are uniform, and the core performance is stable to obtain the thermoplastic ceramic slurry; the 10% high-temperature resistant silica sol is used as a binder, so that each layer of gradient structure of the ceramic core is compact and obvious in distinction;
step 2: hot-pressing and injecting to obtain a formed ceramic core blank,
extruding a refractory material with the grain diameter of 600 meshes into a surface layer of thermoplastic ceramic slurry for preforming, performing a pressing process by using a ceramic core high-pressure injection machine, putting the ceramic core high-pressure injection machine into a charging basket of a hot-pressing injection molding machine, heating the ceramic core high-pressure injection machine to a molten state at 160 ℃, performing injection, and adopting oleic acid as a mold release agent, wherein the injection pressure is 4MPa, the pressure maintaining time is 30s, and the injection temperature is room temperature; and (3) putting the wet core which is just stripped into a correcting mould under the wet condition, and pressurizing by using a press machine to correct the size so as to ensure that the wet core has good size and does not generate phenomena of short shot and crack, thereby obtaining a ceramic core blank.
And step 3: sintering, heating, curing and forming
Loading the prepared ceramic core blank into a ceramic groove, performing gradient temperature rise and heat preservation on melting points corresponding to different components, keeping the temperature rise speed at 180 ℃/h according to different component contents, and preserving heat for 15min after continuously raising the temperature for 1 h; when the temperature is raised to 600 ℃, preserving the heat for 2 hours to ensure that the wax core in the ceramic core is completely removed and becomes a hollow gradient structure; when the temperature is raised to 1400 ℃ to reach the final sintering temperature, the mixture is sintered for 4 hours in a heat preservation way; and then cooling to 500 ℃ at the speed of 100 ℃/h, then cooling along with the furnace until the temperature reaches room temperature, and taking out to obtain the gradient hollow ceramic core with the densified and smoothed surface.
Example 4
The preparation method comprises the following steps: weighing the following components in percentage by mass: 65% of fused quartz; 18% of white paraffin; 3% of diethyl phthalate; 2% of beeswax; 1% of polyethylene; 10% of zircon; 1% of oleic acid; the total amount is 100%. 10% of the total fused quartz is divided into square fused quartz, 10% of the total fused quartz is divided into refractory materials, and the rest 80% of the fused quartz is used for preparing fused quartz powder;
step 1: preparation of thermoplastic ceramic slurry
1.4) putting white paraffin, diethyl phthalate, beeswax and polyethylene into a stirrer, heating to 200 ℃, and preparing a wax core after the white paraffin, the diethyl phthalate, the beeswax and the polyethylene are completely melted;
1.2) taking fused quartz powder, zircon powder and square fused quartz with different particle diameters, sequentially putting the three raw materials into a ball milling tank, adding zirconia balls with the diameter of 30mm, wherein the mass ratio of the three raw materials to the zirconia balls is 3: 2, after fully ball-milling for 0.5h at room temperature, putting the mixed powder into an oven to dry for 0.5h at the temperature of 300 ℃; taking out the mixed powder in the oven, uniformly mixing the mixed powder with the melted plasticizer and the melted oleic acid, and manufacturing the outer layer of the ceramic core in a gradient manner; controlling the stirring speed to be 600r/min, and stirring for 5 hours to ensure that the slurry components are uniform, and the core performance is stable to obtain the thermoplastic ceramic slurry; 9% of high-temperature resistant silica sol is used as a binder, so that each layer of gradient structure of the ceramic core is compact and obvious in distinction;
step 2: hot-pressing and injecting to obtain a formed ceramic core blank,
extruding a refractory material with the particle size of 300 meshes into a surface layer of thermoplastic ceramic slurry for preforming, performing a pressing process by using a ceramic core high-pressure injection machine, putting the ceramic core high-pressure injection machine into a charging basket of a hot-pressing injection molding machine, heating the ceramic core high-pressure injection machine to a molten state at the temperature of 200 ℃, performing injection, and taking oleic acid as a mold release agent, wherein the injection pressure is 5MPa, the pressure maintaining time is 10s, and the injection temperature is room temperature; and (3) putting the wet core which is just stripped into a correcting mould under the wet condition, and pressurizing by using a press machine to correct the size so as to ensure that the wet core has good size and does not generate phenomena of short shot and crack, thereby obtaining a ceramic core blank.
And step 3: sintering, heating, curing and forming
Loading the prepared ceramic core blank into a ceramic groove, performing gradient temperature rise and heat preservation on melting points corresponding to different components, keeping the temperature rise speed at 200 ℃/h according to different component contents, and preserving heat for 10min after continuously raising the temperature for 1 h; when the temperature is raised to 600 ℃, preserving the heat for 2 hours to ensure that the wax core in the ceramic core is completely removed and becomes a hollow gradient structure; when the temperature is raised to 1400 ℃ to reach the final sintering temperature, the mixture is sintered for 4 hours in a heat preservation way; and then cooling to 450 ℃ at the speed of 100 ℃/h, then cooling along with the furnace until the temperature reaches room temperature, and taking out to obtain the gradient hollow ceramic core with the densified and smoothed surface.
Example 5
The preparation method comprises the following steps: weighing the following components in percentage by mass: fused quartz 75%; 5% of white paraffin; 5% of diethyl phthalate; 4.9 percent of beeswax; 0.05% of polyethylene; 10% of zircon; oleic acid 0.05%; the total amount is 100%. 10% of the total fused quartz is divided into square fused quartz, 10% of the total fused quartz is divided into refractory materials, and the rest 80% of the fused quartz is used for preparing fused quartz powder;
step 1: preparation of thermoplastic ceramic slurry
1.5) putting white paraffin, diethyl phthalate, beeswax and polyethylene into a stirrer, heating to 80 ℃, and preparing a wax core after the white paraffin, the diethyl phthalate, the beeswax and the polyethylene are completely melted;
1.2) taking fused quartz powder, zircon powder and square fused quartz with different particle diameters, sequentially putting the three raw materials into a ball milling tank, adding zirconia balls with the diameter of 25mm, wherein the mass ratio of the three raw materials to the zirconia balls is 3: 2, after fully ball-milling for 0.5h at room temperature, putting the mixed powder into an oven to dry for 0.5h at the temperature of 280 ℃; taking out the mixed powder in the oven, uniformly mixing the mixed powder with the melted plasticizer and the melted oleic acid, and manufacturing the outer layer of the ceramic core in a gradient manner; controlling the stirring speed to be 120r/min, and stirring for 18h to ensure that the components of the slurry are uniform, and the performance of the mold core is stable to obtain the thermoplastic ceramic slurry; 7% of high-temperature resistant silica sol is used as a binder, so that each layer of gradient structure of the ceramic core is compact and obvious in distinction;
step 2: hot-pressing and injecting to obtain a formed ceramic core blank,
extruding a refractory material with the grain diameter of 500 meshes into a surface layer of thermoplastic ceramic slurry for preforming, performing a pressing process by using a ceramic core high-pressure injection machine, putting the ceramic core high-pressure injection machine into a charging basket of a hot-pressing injection molding machine, heating the ceramic core high-pressure injection machine to a molten state at 60 ℃, performing injection, and taking oleic acid as a mold release agent, wherein the injection pressure is 0.5MPa, the pressure maintaining time is 50s, and the injection temperature is room temperature; and (3) putting the wet core which is just stripped into a correcting mould under the wet condition, and pressurizing by using a press machine to correct the size so as to ensure that the wet core has good size and does not generate phenomena of short shot and crack, thereby obtaining a ceramic core blank.
And step 3: sintering, heating, curing and forming
Loading the prepared ceramic core blank into a ceramic groove, performing gradient temperature rise and heat preservation on melting points corresponding to different components, keeping the temperature rise speed at 150 ℃/h according to different component contents, and preserving heat for 12min after continuously raising the temperature for 1 h; when the temperature is raised to 600 ℃, preserving the heat for 2 hours to ensure that the wax core in the ceramic core is completely removed and becomes a hollow gradient structure; when the temperature is raised to 1400 ℃ to reach the final sintering temperature, the mixture is sintered for 4 hours in a heat preservation way; and then cooling to 250 ℃ at the speed of 100 ℃/h, then cooling along with the furnace until the temperature reaches room temperature, and taking out to obtain the gradient hollow ceramic core with the densified and smoothed surface.
Referring to fig. 1, the gradient hollow ceramic core manufactured by the method of the present invention according to the above five embodiments has the advantages of more compact structure gradient, good high temperature strength, good high temperature thermal stability, and surface densification and smoothing of the core. The problems of long ceramic core removing time and low core removing efficiency are effectively solved, and the ceramic core removing efficiency is greatly improved.
Claims (5)
1. A gradient hollow ceramic core, characterized in that: the material consists of the following components in percentage by mass, 65-75% of fused quartz; 10 to 30 percent of zircon; 5% -30% of white paraffin; 0.5 to 5 percent of diethyl phthalate; 0.5 to 5 percent of beeswax; 0.05 to 1 percent of polyethylene; 0.05 to 1 percent of oleic acid; 5-10% of high-temperature resistant silica sol, and the total amount is 100%.
2. The preparation method of the gradient hollow ceramic core is characterized by comprising the following steps of:
the preparation method comprises the following steps: weighing the following components in percentage by mass: 65% -75% of fused quartz; 10-30% of zircon; 5-30% of white paraffin; 0.5 to 5 percent of diethyl phthalate; 0.5-5% of beeswax; 0.05 to 1 percent of polyethylene; 0.05 to 1 percent of oleic acid; 5-10% of high-temperature resistant silica sol, the total amount is 100%; 10% of the total fused quartz is divided into square fused quartz, 10% of the total fused quartz is divided into refractory materials, and the rest 80% of the fused quartz is used for preparing fused quartz powder;
step 1: preparation of thermoplastic ceramic slurry
1.1) putting white paraffin, diethyl phthalate, beeswax and polyethylene into a stirrer, heating to 50-200 ℃, and preparing a wax core after the white paraffin, the diethyl phthalate, the beeswax and the polyethylene are completely melted;
1.2) taking fused quartz powder, zircon powder and square fused quartz, sequentially putting the three raw materials into a ball milling tank for ball milling, and putting the mixed powder into an oven to dry for 0.5-5h at the temperature of 100-; taking out the mixed powder in the oven, and uniformly mixing the mixed powder with the melted plasticizer and the melted oleic acid; controlling the stirring speed to be 100-600r/min, and stirring for 5-20h to obtain thermoplastic ceramic slurry; 5-10% of high-temperature resistant silica sol is used as a binder to ensure that each layer of gradient structure of the ceramic core is compact;
step 2: hot-pressing and injecting to obtain a formed ceramic core blank,
extruding a refractory material with the grain diameter of 300-600 meshes into the surface layer of the thermoplastic ceramic slurry for preforming, performing a pressing process by using a ceramic core high-pressure injection molding machine, putting the ceramic core high-pressure injection molding machine into a charging basket of a hot-pressing injection molding machine, heating the ceramic core high-pressure injection molding machine to a molten state at the temperature of 50-200 ℃, and performing injection molding by using oleic acid as a mold release agent; putting the wet core which is just demoulded into a correction mould under the wet condition, and pressurizing by a press machine to correct the size to obtain a ceramic core blank;
and step 3: sintering, heating, curing and forming
And (3) loading the prepared ceramic core blank into a ceramic groove, performing gradient temperature rise and heat preservation on the melting points corresponding to different components, wherein the heat preservation time is different according to different component contents to obtain the gradient hollow ceramic core, and thus obtaining the ceramic core.
3. The method for preparing the gradient hollow ceramic core according to claim 2, wherein in the step 1.2), zirconia balls with the diameter of 5-30mm are added, and the mass ratio of the three raw materials to the zirconia balls is 3: 2, fully ball-milling for 0.5-5h at room temperature.
4. The method for preparing the gradient hollow ceramic core according to claim 3, wherein in the step 1.2), the injection pressure is 0.5-5MPa, the dwell time is 5-50s, and the injection temperature is room temperature.
5. The method for preparing the gradient hollow ceramic core according to claim 3, wherein in the step 3, the specific processes of gradient temperature rise and heat preservation are that the temperature rise speed is kept at 120-; when the temperature is raised to 600 ℃, preserving the heat for 2 hours to ensure that the wax core in the ceramic core is completely removed and becomes a hollow gradient structure; when the temperature is raised to 1400 ℃ to reach the final sintering temperature, the mixture is sintered for 4 hours in a heat preservation way; then cooling to 200-500 ℃ at the speed of 100 ℃/h, and then taking out when the temperature is up to room temperature along with furnace cooling.
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