CN107021771B - A method for manufacturing calcium oxide-based ceramic casting mold based on 3D printing technology - Google Patents
A method for manufacturing calcium oxide-based ceramic casting mold based on 3D printing technology Download PDFInfo
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Abstract
本发明公开了一种基于3D打印技术的氧化钙基陶瓷铸型制造方法，该方法通过对颗粒级配后的氧化钙陶瓷粉末进行有机化处理后，再加入适量的烧结助剂和增强短纤维混合均匀制成3D打印用氧化钙基陶瓷粉末；然后利用光固化粘接剂与有机化处理后的氧化钙基陶瓷粉末进行3D打印，实现氧化钙基陶瓷铸型素坯的成形；再对氧化钙基陶瓷铸型进行脱脂、反应熔渗以及高温强化烧结，最终得到高强度的氧化钙基陶瓷铸型，并对制备的陶瓷铸型进行表面防水化处理。本方法提高了氧化钙基陶瓷铸型的抗水化性；本发明制得的氧化钙基陶瓷铸型具有优良的高温综合性能，可满足更高温度合金和高温化学性质活泼金属的铸造要求，且型芯易于脱除。
The invention discloses a method for manufacturing a calcium oxide-based ceramic casting mold based on 3D printing technology. The method comprises the following steps of organically treating the calcium oxide ceramic powder after particle grading, and then adding an appropriate amount of sintering aid and reinforcing short fibers. Mix uniformly to make calcium oxide-based ceramic powder for 3D printing; then use light-curing adhesive and organically treated calcium oxide-based ceramic powder for 3D printing to realize the formation of calcium oxide-based ceramic casting blank; Degreasing, reactive infiltration and high-temperature enhanced sintering are performed on the calcium-based ceramic casting mold to finally obtain a high-strength calcium oxide-based ceramic casting mold, and the surface of the prepared ceramic casting mold is treated with water repellency. The method improves the hydration resistance of the calcium oxide-based ceramic casting mold; the calcium oxide-based ceramic casting mold prepared by the invention has excellent high-temperature comprehensive performance, and can meet the casting requirements of higher-temperature alloys and high-temperature chemically active metals. And the core is easy to remove.
Description
Technical Field
The invention belongs to the technical field of rapid precision casting, and particularly relates to a method for manufacturing a calcium oxide-based ceramic casting mold based on a 3D printing technology.
Background
At present, ceramic casting molds widely used at home and abroad for near-net-shape precision casting mainly comprise two types, namely silicon oxide-based and aluminum oxide-based. The silica-based ceramic has the use temperature of 1520-1560 ℃, the yield is higher under the casting condition of 1500-1550 ℃, but the high-temperature performance is extremely poor when the use temperature is higher than 1550 ℃, so the silica-based ceramic is not suitable for the casting condition of high-temperature alloy at higher temperature; the alumina-based ceramic has the advantages of high refractoriness, good chemical stability, good thermal stability, good creep resistance, no crystal transformation and the like, and the service temperature of the alumina-based ceramic is more than 1550 ℃ and can reach 1850 ℃ at most. Although alumina-based ceramic molds have some superior properties to silica-based ceramic molds, the core removal of alumina-based ceramic molds is very difficult, typically with a 40% scrap rate, which has been a major reason that has prevented their widespread use for a long time.
The melting point of calcium oxide is 2572 ℃, the boiling point is 2850 ℃, and the saturated vapor pressure at high temperature is lower than that of other alkaline oxides. Therefore, the calcium oxide can bear high use temperature; the chemical thermal stability is good, and the chemical thermal stability is not reacted with metals such as titanium and the like at high temperature, so that the surface quality of the blade can be improved; the thermal expansion coefficient of the calcium oxide ceramic is similar to that of the high-temperature alloy, the molten metal can contract synchronously with the metal when being solidified, thermal expansion cracking caused by stress can be avoided, the creep resistance of the high-temperature alloy blade is good, and the high-temperature alloy blade can meet the casting use requirement of a new generation of ultra-high temperature alloy blades; the calcium oxide-based ceramic core is easy to remove, so that the corrosion of the core removal to the blade is avoided, and the core removal difficulty and cost are reduced; the calcium oxide raw material is easy to obtain and low in price. Therefore, calcium oxide is an ideal material for manufacturing a ceramic mold for a hollow blade. However, the preparation of the calcium oxide-based ceramic casting mold is complicated in material design and manufacturing process, and the calcium oxide is easy to absorb moisture and hydrate, so that the manufacturing difficulty of the calcium oxide-based ceramic casting mold is increased. Therefore, it is of great significance to manufacture a calcium oxide-based ceramic mold having good overall performance, manufacturing accuracy, and hydration resistance.
Disclosure of Invention
The invention aims to overcome the defects and provide a method for manufacturing a calcium oxide-based ceramic casting mold based on a 3D printing technology, wherein the 3D printing technology based on a powder bed and a non-water-based adhesive can be used for manufacturing the calcium oxide ceramic casting mold with a core and a shell integrated in one step, and the calcium oxide-based ceramic casting mold has good comprehensive performance, manufacturing precision and hydration resistance.
In order to achieve the above object, the present invention comprises the steps of:
step one, mixing the calcium oxide ceramic powder with the particle sizes of 40 μm, 20 μm and 5 μm according to the weight ratio of 50:35:15, carrying out particle grading and surface organic treatment;
step two, uniformly mixing the calcium oxide ceramic powder subjected to organic treatment, mineralizer powder and reinforcing short fibers to obtain calcium oxide-based ceramic powder for 3D printing;
step three, establishing a three-dimensional CAD model of the calcium oxide-based ceramic casting mould and establishing data of layering and scanning paths;
step four, importing the manufacturing data of the calcium oxide-based ceramic casting mold into a 3D printer, and performing 3D printing forming by using the ceramic powder prepared in the step two to obtain a green body of the calcium oxide-based ceramic casting mold;
fifthly, carrying out vacuum degreasing treatment on the calcium oxide-based ceramic casting mould blank;
sixthly, carrying out vacuum reaction infiltration strengthening treatment on the degreased calcium oxide-based ceramic casting mould;
and seventhly, performing high-temperature reinforced sintering on the infiltration-reinforced calcium oxide-based casting blank in the atmosphere to obtain the high-strength calcium oxide-based ceramic casting.
And step eight, performing surface waterproofing treatment on the calcium oxide-based ceramic casting mould.
In the first step, the particle size of the calcium oxide ceramic powder is 2-40 μm.
In the first step, the surface organic treatment is to generate an organic film on the surface of the calcium oxide ceramic powder by using a Kh50 silane coupling agent as a raw material, and the specific method is as follows:
step one, uniformly mixing a silane coupling agent and absolute ethyl alcohol to prepare an organic solution, wherein the mass fraction of the silane coupling agent in the organic solution is 5%, and the mass fraction of the absolute ethyl alcohol is 95%;
secondly, fully and uniformly mixing the calcium oxide powder with finished particle grading with the organic solution according to the mass ratio of 3:1 to prepare mixed slurry;
and thirdly, standing the mixed slurry at room temperature for 3-5 hours, then placing the mixed slurry in a vacuum drying oven, and completely drying the powder to obtain the calcium oxide ceramic powder subjected to surface organic treatment.
In the second step, the mineralizer is nano ZrO2Nano MgO and nano Y2O3The adding amount of one or three of the calcium oxide powder is 2 to 5 percent of the mass of the calcium oxide powder;
in the second step, the reinforcing short fiber is ZrO2The length of the fiber is 0.5 mm-2 mm, and the adding amount of the fiber is 2% -5% of the weight of the calcium oxide powder;
in the fourth step, the 3D printing process is a powder bed-based resin-based adhesive 3D printing process, the adhesive is a photosensitive resin-based adhesive, and the photosensitive resin-based adhesive contains 80% of photosensitive resin, 10% of ethanol, 5% of photoinitiator and 5% of colorant.
And in the fifth step, vacuum degreasing is to place the calcium oxide ceramic casting mould in a vacuum degreasing furnace, heat the calcium oxide ceramic casting mould to 1200 ℃, preserve heat for 3 hours, and perform degreasing and presintering.
In the sixth step, the vacuum reaction infiltration is to place the degreased calcium oxide ceramic casting mould and the calcium metal particles or magnesium metal particles in a vacuum infiltration device, heat the mixture to the melting point temperature of the infiltration metal, and carry out heat preservation infiltration for 2 hours.
And seventhly, performing high-temperature reinforced sintering, namely placing the infiltrated calcium oxide ceramic casting mold in an atmosphere sintering furnace, heating to 1500-1600 ℃, and preserving heat for 3 hours to perform reinforced sintering.
In the eighth step, the method for performing waterproof treatment on the surface of the calcium oxide-based ceramic casting mold comprises the following steps: and (4) placing the calcium oxide-based ceramic casting mold prepared in the step seven into a carbon dioxide atmosphere box at the temperature of 200-300 ℃, and generating a compact calcium carbonate layer on the surface of the casting mold in situ.
Compared with the prior art, the invention has the following beneficial effects:
1. the 3DP process based on powder bed bonding molding can rapidly manufacture a casting mold with a complex structure, particularly, a core and a shell of the casting mold are formed at one time, so that the defects of core deviation, perforation and the like caused by mold assembly in the traditional investment casting process can be avoided, and the dimensional precision of a casting can be ensured;
2. the biggest difficulty in manufacturing the calcium oxide-based ceramic casting mold is the hydration problem of calcium oxide, the 3D printing process adopted in the invention adopts the resin-based adhesive, and the manufacturing process is carried out in a vacuum drying environment, so that the calcium oxide is not contacted with water, and the hydration of the calcium oxide can be effectively avoided; secondly, by adding a proper amount of mineralizers such as zirconia, yttria and the like, the sintering of the calcium oxide-based ceramic casting mold can be promoted, and the hydration resistance of the casting mold after sintering can be improved;
3. the calcium oxide-based ceramic casting mold prepared by the invention can effectively solve the technical problems of difficult core stripping and high rejection rate of the aluminum oxide-based ceramic casting mold, can greatly improve the manufacturing yield, has high use temperature and good high-temperature performance, and can meet the requirement of precision casting at higher temperature.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
Example 1:
1) selecting calcium oxide ceramic powder of 40 microns, 20 microns and 5 microns, carrying out particle grading according to the mass ratio of 50:35:15, and uniformly mixing;
2) carrying out surface organic treatment on the uniformly mixed powder, and specifically operating as follows:
(1) uniformly mixing a silane coupling agent and absolute ethyl alcohol to prepare an organic solution, wherein the mass fraction of the silane coupling agent in the organic solution is 5%, and the mass fraction of the absolute ethyl alcohol is 95%;
(2) fully and uniformly mixing the calcium oxide powder subjected to particle grading with the organic solution according to the mass ratio of 3:1 to prepare mixed slurry;
(3) standing the mixed slurry at room temperature for 3-5 h, then placing the mixed slurry in a vacuum drying oven, and completely drying the powder to obtain calcium oxide ceramic powder subjected to surface organic treatment;
3) adding 5 percent of nano ZrO by mass into the calcium oxide ceramic powder after organic treatment2Mineralizer powder and 5% of ZrO with mass fraction of 0.5 mm-2 mm2Short fibers and uniformly mixing the short fibers to obtain the 3D printingCalcium oxide-based ceramic powder;
3) establishing a three-dimensional CAD model of the calcium oxide-based ceramic casting mould and establishing data of layering and scanning paths;
4) importing the manufacturing data of the calcium oxide-based ceramic casting mold into a 3D printer, and performing 3D printing forming to obtain a calcium oxide-based ceramic casting mold biscuit blank;
5) heating the calcium oxide-based ceramic biscuit blank to 1200 ℃ in a vacuum degreasing furnace, preserving heat for 3 hours, and degreasing and presintering;
6) putting the degreased calcium oxide ceramic casting mold and metal magnesium particles into a vacuum infiltration device according to the mass ratio of 1:2, heating to 650 ℃, and carrying out heat preservation infiltration for 2 hours; (ii) a
7) Placing the calcium oxide-based casting mold blank subjected to infiltration strengthening in an atmosphere sintering furnace, heating to 1550 ℃, preserving heat for 3 hours, and performing high-temperature strengthening sintering to obtain a high-strength calcium oxide-based ceramic casting mold;
8) the calcium oxide-based ceramic casting mold prepared by the process is placed in a carbon dioxide atmosphere box at the temperature of 200 ℃, and a compact calcium carbonate layer is generated in situ on the surface of the casting mold.
Example 2:
step one, mixing the calcium oxide ceramic powder with the particle sizes of 40 μm, 20 μm and 5 μm according to the weight ratio of 50:35:15, carrying out particle grading and surface organic treatment, wherein the surface organic treatment is carried out by selecting a Kh50 silane coupling agent as a raw material;
step two, uniformly mixing a silane coupling agent and absolute ethyl alcohol to prepare an organic solution, wherein the mass fraction of the silane coupling agent in the organic solution is 5%, and the mass fraction of the absolute ethyl alcohol is 95%;
step three, fully and uniformly mixing the calcium oxide powder with finished particle grading with the organic solution according to the mass ratio of 3:1 to prepare mixed slurry;
standing the mixed slurry at room temperature for 3 hours, then placing the mixed slurry in a vacuum drying oven, and completely drying the powder to obtain calcium oxide ceramic powder subjected to surface organic treatment;
step five, evenly mixing the calcium oxide ceramic powder, mineralizer powder and reinforced short fibers after organic treatment to obtain the calcium oxide ceramic powderThe mineralizer is nano MgO, the addition amount of the mineralizer is 2 percent of the mass of the calcium oxide powder, and the reinforcing short fiber is ZrO2The length of the fiber is 0.5mm, and the adding amount of the fiber is 2 percent of the mass of the calcium oxide powder;
step six, establishing a three-dimensional CAD model of the calcium oxide-based ceramic casting mould and establishing data of layering and scanning paths;
step seven, importing the manufacturing data of the calcium oxide-based ceramic casting mold into a 3D printer, and performing 3D printing forming by using the ceramic powder prepared in the step two to obtain a calcium oxide-based ceramic casting mold blank, wherein the 3D printing process is a powder bed-based resin-based adhesive 3D printing process, the adhesive is a photosensitive resin-based adhesive, and the photosensitive resin-based adhesive contains 80% of photosensitive resin, 10% of ethanol, 5% of photoinitiator and 5% of colorant;
step eight, placing the calcium oxide ceramic casting mold in a vacuum degreasing furnace, heating to 1200 ℃, preserving heat for 3 hours, and performing degreasing and presintering;
putting the degreased calcium oxide ceramic casting mold and metal calcium particles into a vacuum infiltration device, heating to 850 ℃, preserving heat and infiltrating for 2 hours to finish vacuum reaction infiltration strengthening treatment on the degreased calcium oxide-based ceramic casting mold;
tenthly, performing high-temperature reinforced sintering, namely putting the infiltrated calcium oxide ceramic casting mold into an atmosphere sintering furnace, heating to 1500 ℃, preserving heat for 3 hours, and performing reinforced sintering to obtain a high-strength calcium oxide-based ceramic casting mold;
step eleven, placing the calcium oxide-based ceramic casting mold prepared in the step above in a carbon dioxide atmosphere box at 300 ℃, and generating a compact calcium carbonate layer on the surface of the casting mold in situ.
Example 3:
step one, mixing the calcium oxide ceramic powder with the particle sizes of 40 μm, 20 μm and 5 μm according to the weight ratio of 50:35:15, carrying out particle grading and surface organic treatment, wherein the surface organic treatment is carried out by selecting a Kh50 silane coupling agent as a raw material;
step two, uniformly mixing a silane coupling agent and absolute ethyl alcohol to prepare an organic solution, wherein the mass fraction of the silane coupling agent in the organic solution is 5%, and the mass fraction of the absolute ethyl alcohol is 95%;
step three, fully and uniformly mixing the calcium oxide powder with finished particle grading with the organic solution according to the mass ratio of 3:1 to prepare mixed slurry;
standing the mixed slurry at room temperature for 5 hours, then placing the mixed slurry in a vacuum drying oven, and completely drying the powder to obtain calcium oxide ceramic powder subjected to surface organic treatment;
step five, uniformly mixing the organized calcium oxide ceramic powder, mineralizer powder and reinforcing short fibers to obtain the calcium oxide-based ceramic powder for 3D printing, wherein the mineralizer is nano Y2O3The addition amount of the short reinforcing fiber is 5 percent of the mass of the calcium oxide powder, and the short reinforcing fiber is ZrO2The length of the fiber is 2mm, and the adding amount of the fiber is 5 percent of the mass of the calcium oxide powder;
step six, establishing a three-dimensional CAD model of the calcium oxide-based ceramic casting mould and establishing data of layering and scanning paths;
step seven, importing the manufacturing data of the calcium oxide-based ceramic casting mold into a 3D printer, and performing 3D printing forming by using the ceramic powder prepared in the step two to obtain a calcium oxide-based ceramic casting mold blank, wherein the 3D printing process is a powder bed-based resin-based adhesive 3D printing process, the adhesive is a photosensitive resin-based adhesive, and the photosensitive resin-based adhesive contains 80% of photosensitive resin, 10% of ethanol, 5% of photoinitiator and 5% of colorant;
step eight, placing the calcium oxide ceramic casting mold in a vacuum degreasing furnace, heating to 1200 ℃, preserving heat for 3 hours, and performing degreasing and presintering;
putting the degreased calcium oxide ceramic casting mold and metal calcium particles into a vacuum infiltration device, heating to 850 ℃, preserving heat and infiltrating for 2 hours to finish vacuum reaction infiltration strengthening treatment on the degreased calcium oxide-based ceramic casting mold;
tenthly, performing high-temperature reinforced sintering, namely putting the infiltrated calcium oxide ceramic casting mold into an atmosphere sintering furnace, heating to 1600 ℃, preserving heat for 3 hours, and performing reinforced sintering to obtain a high-strength calcium oxide-based ceramic casting mold;
step eleven, placing the calcium oxide-based ceramic casting mold prepared in the step above in a carbon dioxide atmosphere box at 150 ℃, and generating a compact calcium carbonate layer in situ on the surface of the casting mold.
Example 4:
step one, mixing the calcium oxide ceramic powder with the particle sizes of 40 μm, 20 μm and 5 μm according to the weight ratio of 50:35:15, carrying out particle grading and surface organic treatment, wherein the surface organic treatment is carried out by selecting a Kh50 silane coupling agent as a raw material;
step two, uniformly mixing a silane coupling agent and absolute ethyl alcohol to prepare an organic solution, wherein the mass fraction of the silane coupling agent in the organic solution is 5%, and the mass fraction of the absolute ethyl alcohol is 95%;
step three, fully and uniformly mixing the calcium oxide powder with finished particle grading with the organic solution according to the mass ratio of 3:1 to prepare mixed slurry;
standing the mixed slurry at room temperature for 4 hours, then placing the mixed slurry in a vacuum drying oven, and completely drying the powder to obtain calcium oxide ceramic powder subjected to surface organic treatment;
step five, uniformly mixing the organized calcium oxide ceramic powder, mineralizer powder and reinforcing short fibers to obtain the calcium oxide-based ceramic powder for 3D printing, wherein the mineralizer is nano ZrO2Nano MgO and nano Y2O3The mixing proportion of the three mixtures is 1:1:1, the addition amount of the three mixtures is 3 percent of the mass of the calcium oxide powder, and the reinforcing short fiber is ZrO2The length of the fiber is 1.2mm, and the adding amount of the fiber is 4 percent of the mass of the calcium oxide powder;
step six, establishing a three-dimensional CAD model of the calcium oxide-based ceramic casting mould and establishing data of layering and scanning paths;
step seven, importing the manufacturing data of the calcium oxide-based ceramic casting mold into a 3D printer, and performing 3D printing forming by using the ceramic powder prepared in the step two to obtain a calcium oxide-based ceramic casting mold blank, wherein the 3D printing process is a powder bed-based resin-based adhesive 3D printing process, the adhesive is a photosensitive resin-based adhesive, and the photosensitive resin-based adhesive contains 80% of photosensitive resin, 10% of ethanol, 5% of photoinitiator and 5% of colorant;
step eight, placing the calcium oxide ceramic casting mold in a vacuum degreasing furnace, heating to 1200 ℃, preserving heat for 3 hours, and performing degreasing and presintering;
putting the degreased calcium oxide ceramic casting mold and metal magnesium particles into a vacuum infiltration device, heating to 650 ℃, preserving heat, infiltrating for 2 hours, and completing vacuum reaction infiltration strengthening treatment on the degreased calcium oxide-based ceramic casting mold;
step ten, high-temperature reinforced sintering, namely placing the infiltrated calcium oxide ceramic casting mold in an atmosphere sintering furnace, heating to 1550 ℃, preserving heat for 3 hours, and carrying out reinforced sintering to obtain a high-strength calcium oxide-based ceramic casting mold;
step eleven, placing the calcium oxide-based ceramic casting mold prepared in the step above in a carbon dioxide atmosphere box at 180 ℃, and generating a compact calcium carbonate layer in situ on the surface of the casting mold.
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| CN115673241B (en) * | 2022-10-26 | 2024-07-26 | 华中科技大学 | Soluble ceramic shell or ceramic core material and preparation method and application thereof |
| CN115583831B (en) * | 2022-10-26 | 2023-05-26 | 中国地质大学（武汉） | Calcium oxide-based ceramic core rapidly formed based on micro-extrusion 3D printing technology and preparation method thereof |
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