CN116496100A - Hollow magnesium-based ceramic core and preparation method and application thereof - Google Patents
Hollow magnesium-based ceramic core and preparation method and application thereof Download PDFInfo
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- CN116496100A CN116496100A CN202310414742.8A CN202310414742A CN116496100A CN 116496100 A CN116496100 A CN 116496100A CN 202310414742 A CN202310414742 A CN 202310414742A CN 116496100 A CN116496100 A CN 116496100A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 103
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 56
- 239000011777 magnesium Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000012188 paraffin wax Substances 0.000 claims abstract description 81
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229920002472 Starch Polymers 0.000 claims abstract description 38
- 239000008107 starch Substances 0.000 claims abstract description 38
- 235000019698 starch Nutrition 0.000 claims abstract description 38
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 34
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims abstract description 31
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims abstract description 31
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims abstract description 31
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 30
- 239000002002 slurry Substances 0.000 claims abstract description 30
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000001816 cooling Methods 0.000 claims abstract description 25
- 238000002844 melting Methods 0.000 claims abstract description 22
- 230000008018 melting Effects 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 238000007493 shaping process Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 89
- 229910001220 stainless steel Inorganic materials 0.000 claims description 37
- 239000010935 stainless steel Substances 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 21
- 238000007711 solidification Methods 0.000 claims description 15
- 230000008023 solidification Effects 0.000 claims description 15
- 238000005495 investment casting Methods 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 235000010216 calcium carbonate Nutrition 0.000 claims description 4
- 235000012245 magnesium oxide Nutrition 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 238000007872 degassing Methods 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 18
- 239000007788 liquid Substances 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 13
- 238000004090 dissolution Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 36
- 230000000630 rising effect Effects 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- 239000007787 solid Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 238000005266 casting Methods 0.000 description 6
- 230000008901 benefit Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/067—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- C04B35/03—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
- C04B35/04—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6022—Injection moulding
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a hollow magnesium-based ceramic core, a preparation method and application thereof. Taking a proper amount of paraffin wax, melting, pouring the paraffin wax into a first die, and cooling and shaping the paraffin wax into an inner core; taking out the paraffin inner core from the first die, placing the paraffin inner core into a second die for fixation, mixing magnesium oxide powder, calcium carbonate, hydroxypropyl methylcellulose, ammonium citrate, starch and water, pouring the mixture into the second die, heating the mixture to solidify and shape the slurry, demolding, melting the paraffin inner core, recovering paraffin, and sintering at high temperature. The paraffin can be recycled in the preparation process, and is different from the existing process for preparing the ceramic core with the hollow structure by using the burnable material; the hollow structure enables the mold core and the dissolution liquid to have larger contact area, and the dissolution and collapsibility speed of the mold core is obviously accelerated.
Description
Technical Field
The invention relates to a hollow magnesium-based ceramic core, and a preparation method and application thereof, and belongs to the technical field of ceramic cores.
Background
With the progress of technology, precision casting is becoming more and more common. For example, engine turbine blades, aircraft casings, hollow blades, etc., and stainless steel is increasingly used in our daily lives because of its excellent corrosion resistance. In the field of precision casting of stainless steel, ceramic cores play a critical role in the preparation of some castings with hollow structures, and it is necessary to have the relevant properties: the mold core is not broken, bent and the like in the casting process of the molten metal so as to ensure the internal structural dimension of the casting and have proper strength; the material has proper porosity and shrinkage; has good collapsibility and is convenient for later core removal.
At present, a large number of magnesium-based ceramic cores are used in stainless steel casting, but most of the ceramic cores are of solid structures, the strength is moderate, the dissolution and collapsibility are poor, and patents on hollow ceramic cores are fewer, and CN201510569357.6 discloses that the hollow ceramic cores are prepared by taking paraffin as a plasticizer, so that the problems of mutual penetration, direct combustion of paraffin, environmental pollution and the like are easy to occur in the preparation process; CN200510047854.6 discloses that the preparation of hollow ceramics from polyethylene glycol and polyethylene has the problem that the preparation needs to be carried out by adopting a pressurized injection mode, which causes the breakage of an internal melting core; zhang Peng, li Xin, ji Huiming, etc. preparation of inner cavity melting core of multi-layer ceramic core and performance study [ J ]. University of Chongqing, 2021,44 (10): 46-54., core is prepared by using polyethylene glycol as plasticizer, and the inner core is removed by sintering, thus having low economic benefit; in addition to this, CN201410210181.0 discloses the use of metal as an internal core, electrochemical corrosion removal, which causes problems in that metal remains inside the core, affecting the quality of the core inner surface.
The hollow ceramic core has better collapsibility due to larger contact area with the dissolving liquid, and is more suitable for investment casting. Therefore, the development of the hollow magnesium-based ceramic core with simple preparation process and high economic benefit is urgently needed.
Disclosure of Invention
The invention aims to: the first object of the invention is to provide a hollow magnesium-based ceramic core, the second object of the invention is to provide a preparation method of the hollow magnesium-based ceramic core, and the third object of the invention is to provide the application of the hollow magnesium-based ceramic core in preparing stainless steel investment castings.
The technical scheme is as follows: the hollow magnesium-based ceramic core is a ceramic core with a hollow structure, and comprises a ceramic outer core of magnesium oxide and calcium oxide, wherein the inside of the ceramic outer core is provided with a hollow structure formed by through holes.
Further, the hollow structure is formed by using paraffin wax to melt, cool and shape at high temperature.
Further, the ceramic outer core comprises slurry formed by in-situ solidification of magnesia, calcium carbonate, hydroxypropyl methyl cellulose, starch, a dispersing agent and water.
Further, the weight ratio of the magnesium oxide, the calcium carbonate, the hydroxypropyl methylcellulose, the starch, the dispersing agent and the water is (85-100): (10-15): (1-2): (4-8): (1-2): (35-40).
Further, the magnesium oxide and the calcium carbonate are both powder with the granularity of 400 meshes, the viscosity of the hydroxypropyl methylcellulose is 18000-20000 mPa.s, the starch is water-soluble starch, and the dispersing agent is ammonium citrate.
The preparation method of the hollow magnesium-based ceramic core comprises the following two steps: the preparation method comprises the steps of preparing an inner core, wherein the inner core is prepared from paraffin, preparing an outer core, pouring slurry comprising magnesium oxide, calcium carbonate, hydroxypropyl methylcellulose, starch, ammonium citrate and water into the outer core, solidifying the slurry to form a blank, heating to remove the inner core of the blank, and sintering to obtain the composite material, and specifically comprises the following steps:
(1) Melting paraffin, pouring into a first mold, and cooling and shaping to obtain an inner core;
(2) Fully mixing water-soluble starch, hydroxypropyl methyl cellulose and ammonium citrate, adding a proper amount of water, stirring and uniformly mixing, adding magnesium oxide and calcium carbonate, and continuously stirring to obtain a slurry with fluidity;
(3) Placing the inner core in a second mould for fixing, pouring the slurry in the second mould, oscillating for degassing, heating the second mould, carrying out water-absorbing gelatinization and shaping on starch, removing the second mould after complete solidification to obtain a blank, and heating the blank to recover paraffin to obtain a green body;
(4) And (3) embedding the green body into alumina filler for sintering to obtain the hollow magnesium-based ceramic core.
Further, in the step (1), the melting temperature is 80-90 ℃, the melting time is 30-60min, and the stirring speed is 100-200r/min.
Further, in the step (2), the stirring speed is 200-400r/min, and the stirring time is 30-60min.
Further, in the step (3), the second mold is heated at 60-65 ℃ for 3-4 hours.
Further, in the step (4), the sintering process comprises slowly rising to 1100-1200 ℃ at a speed lower than 2 ℃/min in an air atmosphere, and preserving heat for 30min.
The invention also comprises application of the hollow magnesium-based ceramic core in preparing stainless steel investment castings.
The invention takes magnesium oxide and calcium oxide as ceramic outer cores, paraffin wax as inner cores, the inner cores utilize the characteristic of high-temperature melting, cooling and shaping of paraffin wax, the outer cores utilize the characteristic of shaping after water absorption and gelatinization of starch to prepare hollow magnesium-based ceramic core green bodies, and the hollow magnesium-based ceramic core with a hollow structure is obtained through high-temperature sintering. The prepared hollow ceramic core has good dimensional accuracy and proper strength, the hollow structure enables the core to have more contact area with the acetic acid of the dissolution liquid, the dissolution collapsibility is faster, the problem that the existing magnesium-based ceramic core is poor in collapsibility in the field of stainless steel investment casting can be well solved, the method is simple to operate, and meanwhile, the product quality is higher, so that the method meets the actual production.
The beneficial effects are that: compared with the prior art, the invention has the following remarkable advantages:
(1) The inner core part consisting of paraffin is melted and flows out after heat treatment to form a hollow structure, and meanwhile, the paraffin can be recycled, which is different from the prior process for preparing the ceramic core with the hollow structure by using the burnable material;
(2) The invention adopts the direct casting solidification technology, does not need to be pressurized, has lower requirement on a die and has simple preparation process;
(3) Starch is introduced, on one hand, the starch is shaped after being gelatinized by water absorption at 80 ℃, and on the other hand, the starch and hydroxypropyl methylcellulose are sintered to improve the porosity of the core so as to facilitate the later core-removing work;
(4) The hollow structure of the invention ensures that the mold core has larger contact area with the dissolving liquid, and the dissolving and collapsing speed is obviously accelerated.
Drawings
FIG. 1 is a schematic view of a first mold and a second mold used in the present invention;
FIG. 2 is a diagram of a green compact of a hollow magnesium-based ceramic core and a model of a green compact of a molded hollow magnesium-based ceramic core prepared by the invention;
FIG. 3 is a graph of a ceramic core prepared in example 1.
Fig. 4 is a graph showing the dissolution and collapse of the hollow ceramic core prepared in example 1 and the solid ceramic core prepared in comparative example 1.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings.
Example 1
(1) 100 parts of paraffin, 100 parts of magnesium oxide, 12 parts of calcium carbonate, 4 parts of water-soluble starch, 1 part of hydroxypropyl methyl cellulose, 1 part of ammonium citrate and 40 parts of water are respectively weighed.
(2) Placing the weighed paraffin into a stainless steel stirring tank, placing the stainless steel stirring tank at 80 ℃ for melting, setting the stirring speed to be 150r/min, stirring for 30min, pouring the paraffin into a first die 1 (see figure 1) after stirring is finished, and cooling and shaping to obtain a paraffin inner core;
(3) Placing the weighed water-soluble starch, hydroxypropyl methylcellulose and ammonium citrate in a stainless steel stirring tank, adding water, setting the stirring speed to be 400r/min, gradually adding magnesium oxide and calcium carbonate in batches after uniform mixing, and continuously stirring the mixture for 30min after all the materials are added to obtain the ceramic outer core slurry with certain fluidity;
(4) Taking out the inner core of the first die 1 in the step (2), placing the inner core in a second die 2 (see figure 1) for fixing, pouring the slurry in the step (3) into the second die 2, heating the second die 2 at the temperature of 60 ℃ for 3 hours, demolding after complete solidification to obtain a blank body, heating the blank body to 80 ℃ for recycling paraffin, and placing the blank body so that the paraffin liquid flows out from the inner cavity of the blank body to obtain a green body; as shown in fig. 2.
(5) The prepared green compact is put into a box-type furnace, and sintering is completed according to the following set procedures: slowly rising to 1100 ℃ at a speed of 2 ℃/min in an air atmosphere, and preserving heat for 30min.
And (5) naturally cooling the temperature in the box-type furnace to room temperature, and taking out the sintered ceramic core to obtain the magnesium-based ceramic core with the hollow structure. As shown in fig. 3.
The flexural strength of the magnesium-based ceramic core prepared in this example was measured by a microcomputer controlled electronic universal tester and was 1.18MPa, and at the same time, the core was immersed in a 40wt.% acetic acid solution in a 80 ℃ water bath to completely collapse within 4 hours.
Example 2
(1) 100 parts of paraffin, 98 parts of magnesium oxide, 12 parts of calcium carbonate, 5 parts of water-soluble starch, 1 part of hydroxypropyl methyl cellulose, 1 part of ammonium citrate and 38 parts of water are respectively weighed.
(2) Placing the weighed paraffin into a stainless steel stirring tank, placing the stainless steel stirring tank at 85 ℃ for melting, setting the stirring speed to be 100r/min, stirring for 40min, pouring the paraffin into a first die 1 (see figure 1) after stirring is finished, and cooling and shaping to obtain a paraffin inner core;
(3) Placing the weighed water-soluble starch, hydroxypropyl methylcellulose and ammonium citrate in a stainless steel stirring tank, adding water, setting the stirring speed to be 380r/min, gradually adding magnesium oxide and calcium carbonate in batches after uniform mixing, and continuously stirring the mixture for 40min after all the materials are added to obtain the ceramic outer core slurry with certain fluidity;
(4) Taking out the inner core of the first die 1 in the step (2), placing the inner core in a second die 2 (see figure 1) for fixing, pouring the slurry in the step (3) into the second die 2, heating the second die 2 at 65 ℃ for 3.5 hours, demolding after complete solidification to obtain a green body, heating the green body to 80 ℃ for recycling paraffin, and placing the green body so that the paraffin liquid can flow out from the inner cavity of the green body to obtain a green body;
(5) The prepared green compact is put into a box-type furnace, and sintering is completed according to the following set procedures: slowly rising to 1100 ℃ at a speed of 2 ℃/min in an air atmosphere, and preserving heat for 30min. And (5) naturally cooling the temperature in the box-type furnace to room temperature, and taking out the sintered ceramic core to obtain the magnesium-based ceramic core with the hollow structure.
The flexural strength of the magnesium-based ceramic core prepared in this example was measured by a microcomputer controlled electronic universal tester and was 1.25MPa, and at the same time, the core was immersed in a 40wt.% acetic acid solution in a 80 ℃ water bath to completely collapse within 4 hours.
Example 3
(1) 100 parts of paraffin, 96 parts of magnesium oxide, 10 parts of calcium carbonate, 5 parts of water-soluble starch, 2 parts of hydroxypropyl methyl cellulose, 1 part of ammonium citrate and 38 parts of water are weighed respectively.
(2) Placing the weighed paraffin into a stainless steel stirring tank, placing the stainless steel stirring tank at 80 ℃ for melting, setting the stirring speed to be 200r/min, stirring for 30min, pouring the paraffin into a first die 1 (see figure 1) after stirring is finished, and cooling and shaping to obtain a paraffin inner core;
(3) Placing the weighed water-soluble starch, hydroxypropyl methylcellulose and ammonium citrate in a stainless steel stirring tank, adding water, setting the stirring speed to be 360r/min, gradually adding magnesium oxide and calcium carbonate in batches after uniform mixing, and continuously stirring the mixture for 40min after all the materials are added to obtain the ceramic outer core slurry with certain fluidity;
(4) Taking out the inner core of the first die 1 in the step (2), placing the inner core in a second die 2 (see figure 1) for fixing, pouring the slurry in the step (3) into the second die 2, heating the second die 2 at 65 ℃ for 3 hours, demolding after complete solidification to obtain a blank body, heating the blank body to 80 ℃ for recovering paraffin, and placing the blank body so that the paraffin liquid can flow out from the inner cavity of the blank body to obtain a green body;
(5) The prepared green compact is put into a box-type furnace, and sintering is completed according to the following set procedures: slowly rising to 1150 ℃ at a speed of 2 ℃/min in an air atmosphere, and preserving heat for 30min.
And (5) naturally cooling the temperature in the box-type furnace to room temperature, and taking out the sintered ceramic core to obtain the magnesium-based ceramic core with the hollow structure.
The flexural strength of the magnesium-based ceramic core prepared in this example was measured by a microcomputer controlled electronic universal tester and was 1.97MPa, and at the same time, the core was immersed in a 40wt.% acetic acid solution in a 80 ℃ water bath to completely collapse within 4 hours.
Example 4
(1) 100 parts of paraffin, 95 parts of magnesium oxide, 12 parts of calcium carbonate, 4 parts of water-soluble starch, 1 part of hydroxypropyl methyl cellulose, 2 parts of ammonium citrate and 37 parts of water are respectively weighed.
(2) Placing the weighed paraffin into a stainless steel stirring tank, placing the stainless steel stirring tank at 90 ℃ for melting, setting the stirring speed to be 100r/min, stirring for 60min, pouring the paraffin into a first die 1 (see figure 1) after stirring is finished, and cooling and shaping to obtain a paraffin inner core;
(3) Placing the weighed water-soluble starch, hydroxypropyl methylcellulose and ammonium citrate in a stainless steel stirring tank, adding water, setting the stirring speed to be 360r/min, gradually adding magnesium oxide and calcium carbonate in batches after uniform mixing, and continuously stirring the mixture for 50min after all the materials are added to obtain the ceramic outer core slurry with certain fluidity;
(4) Taking out the inner core in the first die 1 in the step (2), placing the inner core in a second die 2 (see figure 1) for fixing, pouring the slurry in the step (3) into the second die 2, heating the second die 2, setting the temperature to 60 ℃, and heating the second die for 4 hours; demolding after complete solidification to obtain a green body, heating the green body to 80 ℃ to recover paraffin, and placing the green body so that the paraffin liquid can flow out from the inner cavity of the green body to obtain a green body;
(5) The prepared green compact is put into a box-type furnace, and sintering is completed according to the following set procedures: slowly rising to 1200 ℃ at a speed of 2 ℃/min in an air atmosphere, and preserving heat for 30min.
And (5) naturally cooling the temperature in the box-type furnace to room temperature, and taking out the sintered ceramic core to obtain the magnesium-based ceramic core with the hollow structure.
The flexural strength of the magnesium-based ceramic core prepared in this example was measured by a microcomputer controlled electronic universal tester and was 2.40MPa, and at the same time, the core was immersed in a 40wt.% acetic acid solution in a 80 ℃ water bath to completely collapse within 4.5 hours.
Example 5
(1) 100 parts of paraffin, 94 parts of magnesium oxide, 15 parts of calcium carbonate, 8 parts of water-soluble starch, 2 parts of hydroxypropyl methyl cellulose, 2 parts of ammonium citrate and 40 parts of water are respectively weighed.
(2) Placing the weighed paraffin into a stainless steel stirring tank, placing the stainless steel stirring tank at 80 ℃ for melting, setting the stirring speed to be 200r/min, stirring for 30min, pouring the paraffin into a first die 1 (see figure 1) after stirring is finished, and cooling and shaping to obtain a paraffin inner core;
(3) Placing the weighed water-soluble starch, hydroxypropyl methylcellulose and ammonium citrate in a stainless steel stirring tank, adding water, setting the stirring speed to be 340r/min, gradually adding magnesium oxide and calcium carbonate in batches after uniform mixing, and continuously stirring the mixture for 60min after all the materials are added to obtain the ceramic outer core slurry with certain fluidity;
(4) Taking out the inner core in the first die 1 in the step (2), placing the inner core in a second die 2 (see figure 1) for fixing, pouring the slurry in the step (3) in the second die 2, heating the second die 2, setting the temperature to 63 ℃ and the heating time to 4 hours; demolding after complete solidification to obtain a blank, heating the blank to 80 ℃ to recover paraffin, and placing the blank so that the paraffin liquid flows out of the inner cavity of the blank to obtain a green body;
(5) The prepared green compact is put into a box-type furnace, and sintering is completed according to the following set procedures: slowly rising to 1200 ℃ at a speed of 2 ℃/min in an air atmosphere, and preserving heat for 30min. And (5) naturally cooling the temperature in the box-type furnace to room temperature, and taking out the sintered ceramic core to obtain the magnesium-based ceramic core with the hollow structure.
The flexural strength of the magnesium-based ceramic core prepared in this example was measured by a microcomputer controlled electronic universal tester and was 2.45MPa, and at the same time, the core was immersed in a 40wt.% acetic acid solution in a 80 ℃ water bath to completely collapse within 4.5 hours.
Example 6
(1) 100 parts of paraffin, 92 parts of magnesium oxide, 13 parts of calcium carbonate, 6 parts of water-soluble starch, 1 part of hydroxypropyl methyl cellulose, 1 part of ammonium citrate and 36 parts of water are respectively weighed;
(2) Placing the weighed paraffin into a stainless steel stirring tank, placing the stainless steel stirring tank at 82 ℃ for melting, setting the stirring speed to be 180r/min, stirring for 40min, pouring the paraffin into a first die 1 (see figure 1) after stirring is finished, and cooling and shaping to obtain a paraffin inner core;
(3) Placing the weighed water-soluble starch, hydroxypropyl methylcellulose and ammonium citrate in a stainless steel stirring tank, adding water, setting the stirring speed to be 350r/min, gradually adding magnesium oxide and calcium carbonate in batches after uniform mixing, and continuously stirring the mixture for 60min after all the materials are added to obtain the ceramic outer core slurry with certain fluidity;
(4) Taking out the inner core in the first die 1 in the step (2), placing the inner core in the second die 2 (see figure 1) for fixing, pouring the slurry in the step (3) into the second die 2, heating the second die 2, setting the temperature to 65 ℃ and the heating time to 3 hours; demolding after complete solidification to obtain a blank, heating the blank to 80 ℃ to recover paraffin, and placing the blank so that the paraffin liquid flows out of the inner cavity of the blank to obtain a green body;
(5) The prepared green compact is put into a box-type furnace, and sintering is completed according to the following set procedures: slowly rising to 1180 ℃ at a speed of 2 ℃/min in an air atmosphere, and preserving heat for 30min. And (5) naturally cooling the temperature in the box-type furnace to room temperature, and taking out the sintered ceramic core to obtain the magnesium-based ceramic core with the hollow structure.
The flexural strength of the magnesium-based ceramic core prepared in this example was measured by a microcomputer controlled electronic universal tester and was 2.30MPa, and at the same time, the core was immersed in a 40wt.% acetic acid solution in a 80 ℃ water bath to completely collapse within 4.5 hours.
Example 7
(1) 100 parts of paraffin, 89 parts of magnesium oxide, 14 parts of calcium carbonate, 6 parts of water-soluble starch, 1 part of hydroxypropyl methyl cellulose, 2 parts of ammonium citrate and 35 parts of water are weighed respectively.
(2) Placing the weighed paraffin into a stainless steel stirring tank, placing the stainless steel stirring tank at 80 ℃ for melting, setting the stirring speed to be 200r/min, stirring for 30min, pouring the paraffin into a first die 1 (see figure 1) after stirring is finished, and cooling and shaping to obtain a paraffin inner core;
(3) Placing the weighed water-soluble starch, hydroxypropyl methylcellulose and ammonium citrate in a stainless steel stirring tank, adding water, setting the stirring speed to be 350r/min, gradually adding magnesium oxide and calcium carbonate in batches after uniform mixing, and continuously stirring the mixture for 60min after all the materials are added to obtain the ceramic outer core slurry with certain fluidity;
(4) Taking out the inner core in the first die 1 in the step (2), placing the inner core in a second die 2 (see figure 1) for fixing, pouring the slurry in the step (3) into the second die 2, heating the second die 2, setting the temperature to 63 ℃ and the heating time to 4 hours; demolding after complete solidification to obtain a blank, heating the blank to 80 ℃ to recover paraffin, and placing the blank so that the paraffin liquid flows out of the inner cavity of the blank to obtain a green body;
(5) The prepared green compact is put into a box-type furnace, and sintering is completed according to the following set procedures: slowly rising to 1160 ℃ at a speed of 2 ℃/min in an air atmosphere, and preserving heat for 30min. And (5) naturally cooling the temperature in the box-type furnace to room temperature, and taking out the sintered ceramic core to obtain the magnesium-based ceramic core with the hollow structure.
The flexural strength of the magnesium-based ceramic core prepared in this example was measured by a microcomputer controlled electronic universal tester and was 2.32MPa, and at the same time, the core was immersed in a 40wt.% acetic acid solution in a 80 ℃ water bath to completely collapse within 4 hours.
Example 8
(1) 100 parts of paraffin, 89 parts of magnesium oxide, 14 parts of calcium carbonate, 6 parts of water-soluble starch, 1 part of hydroxypropyl methyl cellulose, 2 parts of ammonium citrate and 35 parts of water are respectively weighed;
(2) Placing the weighed paraffin into a stainless steel stirring tank, placing the stainless steel stirring tank at 80 ℃ for melting, setting the stirring speed to be 200r/min, stirring for 40min, pouring the paraffin into a first die 1 (see figure 1) after stirring is finished, and cooling and shaping to obtain a paraffin inner core;
(3) Placing the weighed water-soluble starch, hydroxypropyl methylcellulose and ammonium citrate in a stainless steel stirring tank, adding water, setting the stirring speed to be 300r/min, gradually adding magnesium oxide and calcium carbonate in batches after uniform mixing, and continuously stirring the mixture for 60min after all the materials are added to obtain the ceramic outer core slurry with certain fluidity;
(4) Taking out the inner core in the first die 1 in the step (2), placing the inner core in a second die 2 (see figure 1) for fixing, pouring the slurry in the step (3) into the second die 2, heating the second die 2, setting the temperature to 63 ℃ and the heating time to 4 hours; demolding after complete solidification to obtain a blank, heating the blank to 80 ℃ to recover paraffin, and placing the blank so that the paraffin liquid flows out of the inner cavity of the blank to obtain a green body;
(4) The prepared green compact is put into a box-type furnace, and sintering is completed according to the following set procedures: slowly rising to 1120 ℃ at a speed of 2 ℃/min in an air atmosphere, and preserving the temperature for 30min. And (5) naturally cooling the temperature in the box-type furnace to room temperature, and taking out the sintered ceramic core to obtain the magnesium-based ceramic core with the hollow structure.
The flexural strength of the magnesium-based ceramic core prepared in this example was measured by a microcomputer controlled electronic universal tester and was 1.37MPa, and the core was immersed in a 40wt.% acetic acid solution in a 80℃water bath to completely collapse within 4 hours.
Example 9
(1) 100 parts of paraffin, 87 parts of magnesium oxide, 14 parts of calcium carbonate, 7 parts of water-soluble starch, 2 parts of hydroxypropyl methyl cellulose, 1 part of ammonium citrate and 39 parts of water are respectively weighed.
(2) Placing the weighed paraffin into a stainless steel stirring tank, placing the stainless steel stirring tank at 80 ℃ for melting, setting the stirring speed to be 200r/min, stirring for 30min, pouring the paraffin into a first die 1 (see figure 1) after stirring is finished, and cooling and shaping to obtain a paraffin inner core;
(3) Placing the weighed water-soluble starch, hydroxypropyl methylcellulose and ammonium citrate in a stainless steel stirring tank, adding water, setting the stirring speed to 320r/min, gradually adding magnesium oxide and calcium carbonate in batches after uniform mixing, and continuously stirring the mixture for 45min after all the materials are added to obtain the ceramic outer core slurry with certain fluidity;
(4) Taking out the inner core in the first die 1 in the step (2), placing the inner core in a second die 2 (see figure 1) for fixing, pouring the slurry in the step (3) into the second die 2, heating the second die 2, setting the temperature to 65 ℃ and the heating time to 3 hours; demolding after complete solidification to obtain a blank, heating the blank to 80 ℃ to recover paraffin, and placing the blank so that the paraffin liquid flows out of the inner cavity of the blank to obtain a green body;
(5) The prepared green compact is put into a box-type furnace, and sintering is completed according to the following set procedures: slowly rising to 1200 ℃ at a speed of 2 ℃/min in an air atmosphere, and preserving heat for 30min. And (5) naturally cooling the temperature in the box-type furnace to room temperature, and taking out the sintered ceramic core to obtain the magnesium-based ceramic core with the hollow structure.
The flexural strength of the magnesium-based ceramic core prepared in this example was measured by a microcomputer controlled electronic universal tester and was 2.50MPa, and at the same time, the core was immersed in a 40wt.% acetic acid solution in a 80 ℃ water bath to completely collapse within 4 hours.
Example 10
(1) 100 parts of paraffin, 85 parts of magnesium oxide, 15 parts of calcium carbonate, 8 parts of water-soluble starch, 1 part of hydroxypropyl methyl cellulose, 1 part of ammonium citrate and 40 parts of water are respectively weighed.
(2) Placing the weighed paraffin into a stainless steel stirring tank, melting at 88 ℃, setting the stirring speed to 200r/min, stirring for 30min, pouring into a first mold 1 (see figure 1) after stirring, and cooling and shaping to obtain a paraffin inner core;
(3) Placing the weighed water-soluble starch, hydroxypropyl methylcellulose and ammonium citrate in a stainless steel stirring tank, adding water, setting the stirring speed to be 340r/min, gradually adding magnesium oxide and calcium carbonate in batches after uniform mixing, and continuously stirring the mixture for 60min after all the materials are added to obtain the ceramic outer core slurry with certain fluidity;
(4) Taking out the inner core in the first die 1 in the step (2), placing the inner core in a second die 2 (see figure 1) for fixing, pouring the slurry in the step (3) into the second die 2, heating the second die 2, setting the temperature to 63 ℃ and the heating time to 4 hours; demolding after complete solidification to obtain a blank, heating the blank to 80 ℃ to recover paraffin, and placing the blank so that the paraffin liquid flows out of the inner cavity of the blank to obtain a green body;
(5) The prepared green compact is put into a box-type furnace, and sintering is completed according to the following set procedures: slowly rising to 1150 ℃ at a speed of 2 ℃/min in an air atmosphere, and preserving heat for 30min. And (5) naturally cooling the temperature in the box-type furnace to room temperature, and taking out the sintered ceramic core to obtain the magnesium-based ceramic core with the hollow structure.
The flexural strength of the magnesium-based ceramic core prepared in this example was measured by a microcomputer controlled electronic universal tester and was 1.98MPa, and the core was immersed in a 40wt.% acetic acid solution in a 80℃water bath to completely collapse within 4 hours.
Table 1 examples 1-10 preparation of hollow ceramic cores strength and collapsibility comparison
As can be seen from table 1, in example 7 and example 8, when the core formulations are identical, the flexural strength of the core increases with increasing sintering temperature. When the temperature reached 1200 ℃, the magnesium oxide content in the core composition was low (example 9), the collapsibility was improved.
In comparison, the core composition of example 9 was the best, the core formulation was the best, and the core composition of example 7 was the next lowest.
Comparative example 1 actual use Effect of comparative solid magnesium-based ceramic core and hollow magnesium-based ceramic core
(1) Preparation of solid ceramic cores
The procedure was as in example 1, except that no paraffin core was prepared and the prepared slurry was directly cast into the second mold 2. The whole mold core has the same composition and sintering process, and the solid magnesium-based ceramic mold core is obtained.
(2) Simulation of the heating transformation procedure of the solid magnesium-based ceramic core prepared in this comparative example and the hollow magnesium-based ceramic core prepared in example 1 during actual stainless steel casting
The solid magnesium-based ceramic core prepared in the comparative example and the hollow magnesium-based ceramic core prepared in the example 1 are both kept at 1100 ℃ for 30min, then cooled to 900 ℃ along with a furnace, then the temperature is rapidly increased to 1450 ℃ for 5min, and finally cooled to room temperature. The results are shown in FIG. 4, which are obtained by soaking in acetic acid solution at 80℃and 40wt.% concentration. FIG. 4 is a graph showing the dissolution and collapse of the hollow ceramic core prepared in example 1 and the solid ceramic core prepared in comparative example 1, wherein it can be seen from FIG. 4 that the hollow magnesium-based ceramic core prepared in example 1 collapses within 8 hours, and the mass loss rate is 100%; while the solid magnesium-based ceramic core 8h prepared in comparative example 1 had dissolved and fallen off the surface, but did not completely collapse, and the mass loss rate was 53.7%, while maintaining the matrix shape. The hollow structure of the invention can lead the mold core to have larger contact area with the dissolution liquid, and the dissolution and collapse speed of the mold core is obviously accelerated.
Claims (10)
1. The hollow magnesium-based ceramic core is characterized by being a ceramic core with a hollow structure, wherein the hollow magnesium-based ceramic core comprises a ceramic outer core of magnesium oxide and calcium oxide, and the inside of the ceramic outer core is provided with a hollow structure formed by through holes.
2. The hollow magnesium-based ceramic core according to claim 1, wherein the hollow structure is shaped by high temperature melting and cooling of paraffin wax.
3. The hollow magnesium-based ceramic core according to claim 1, wherein the ceramic outer core comprises a slurry of magnesium oxide, calcium carbonate, hydroxypropyl methylcellulose, starch, dispersant and water formed by in situ solidification.
4. A hollow magnesium-based ceramic core according to claim 3, wherein the weight ratio of magnesium oxide, calcium carbonate, hydroxypropyl methylcellulose, starch, dispersant and water is 85-100:10-15:1-2:4-8:1-2:35-40.
5. A hollow magnesium based ceramic core according to claim 3, wherein both magnesium oxide and calcium carbonate are powders with a particle size of 400 mesh, the hydroxypropyl methylcellulose has a viscosity of 18000-20000 mPa-s, the starch is a water-soluble starch, and the dispersant is ammonium citrate.
6. A method for preparing a hollow magnesium-based ceramic core according to any one of claims 1 to 5, comprising the steps of:
(1) Melting paraffin, pouring into a first mold (1) for cooling and shaping to obtain an inner core;
(2) Fully mixing water-soluble starch, hydroxypropyl methyl cellulose and ammonium citrate, adding a proper amount of water, stirring and uniformly mixing, adding magnesium oxide and calcium carbonate, and continuously stirring to obtain a slurry with fluidity;
(3) Placing the inner core in a second mould (2) for fixing, pouring the slurry in the second mould (2), oscillating for degassing, heating the second mould (2), carrying out water absorption gelatinization and shaping on starch, removing the second mould (2) after complete solidification to obtain a blank body, and heating the blank body to recover paraffin to obtain a green body;
(4) And (3) embedding the green body into alumina filler for sintering to obtain the hollow magnesium-based ceramic core.
7. The method according to claim 7, wherein in the step (1), the melting temperature is 80 to 90 ℃, the melting time is 30 to 60min, and the stirring speed is 100 to 200r/min.
8. The method according to claim 7, wherein in the step (2), the stirring speed is 200-400r/min, the stirring time is 30-60min, and in the step (3), the second mold (2) is heated at 60-65 ℃ for 3-4h.
9. The method of claim 7, wherein in step (4), the sintering process comprises slowly raising the temperature to 1100 ℃ to 1200 ℃ at a rate of less than 2 ℃/min in an air atmosphere, and maintaining the temperature for 30min.
10. Use of the hollow magnesium-based ceramic core of any of claims 1-5 in the preparation of stainless steel investment castings.
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