CN107353008B - Preparation method of layered metal-ceramic composite material part - Google Patents
Preparation method of layered metal-ceramic composite material part Download PDFInfo
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
- B22D23/04—Casting by dipping
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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
- 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
- C04B35/10—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 aluminium oxide
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- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5093—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with elements other than metals or carbon
- C04B41/5096—Silicon
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- C—CHEMISTRY; METALLURGY
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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
- C04B2235/6023—Gel casting
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a preparation method of a layered metal-ceramic composite part, and belongs to the technical field of near-net forming of complex parts made of metal-ceramic composite materials. The technical scheme is as follows: preparing a resin mould for ceramic slurry gel injection moulding with a laminated structure inside by a photocuring rapid forming technology, preparing a part ceramic blank by gel injection moulding, freeze drying and degreasing sintering, controlling the interface combination condition or improving the wettability between an impregnated metal melt and ceramic by vapor deposition of an interface layer material, and finally realizing the compounding of metal and ceramic by non-pressure metal impregnation. The method can expand the designability of parts and obtain good layered metal oriented toughening effect on metal-ceramic composite material parts.
Description
Technical Field
The invention belongs to the technical field of near-net forming of complex parts made of metal-ceramic composite materials, and relates to a preparation method of layered metal-ceramic composite material parts.
Background
The ceramic material has excellent performances of low density, high temperature resistance, corrosion resistance, high strength, high hardness, high wear resistance and the like, and has a good application prospect in the fields of aerospace and the like, but the inherent low toughness of the ceramic material limits the wide application of the ceramic material. The metal-ceramic composite material formed by compounding the metal and the ceramic can integrate the characteristics of the metal and the ceramic through material design, so that the material has the excellent performance of the ceramic and the good toughness of the metal.
At present, the laminated metal-ceramic composite material mainly adopts a synthesis method of hot-pressing sintering after alternately laminating prefabricated ceramic layer sheets and metal layer sheets. In the preparation process of the method, certain pressure is required to be applied to the material to complete the preparation, so that the method is suitable for preparing the bulk material. For parts, only parts with simple shapes and consistent orientation directions of the laminae can be prepared, and corresponding dies are required to be prepared in the preparation process, so that the time and the preparation cost are increased. However, this approach presents difficulties for near-net shape forming of complex structural parts, and difficulty in achieving homogeneous material layer-to-layer communication, and orientation variation or varying layer thickness design of the layer structure.
Disclosure of Invention
The invention aims to provide a preparation method of a layered metal-ceramic composite part, which is based on a photocuring rapid prototyping technology, prepares the layered metal-ceramic composite part through gel injection molding and pressureless infiltration, is beneficial to directionally improving the toughness of a ceramic composite material, and solves the manufacturing problem of the metal-ceramic composite part with a complex structure.
The invention is realized by the following technical scheme:
a method for preparing a layered metal-ceramic composite part, comprising the steps of:
1) preparing a part resin mold with a layered structure inside by a photocuring rapid prototyping technology;
2) preparing ceramic slurry by adopting a gel injection molding method, and obtaining a ceramic biscuit of the part through a vacuum injection molding process;
3) freeze-drying the ceramic biscuit of the part, and removing the resin mold shell;
4) carrying out vacuum degreasing treatment on the ceramic biscuit of the part processed in the step 3) at 600-900 ℃, and burning out organic matters remained in the biscuit to obtain a laminated ceramic blank body with a resin sheet layer inside;
5) and (3) carrying out metal infiltration on the ceramic blank treated in the step (4) by adopting a metal infiltration process, and carrying out surface processing to obtain the layered metal-ceramic composite part with the internal dimension ranging from micron to millimeter.
Step 1) preparing a part resin mold with a layered structure inside by a photocuring rapid prototyping technology, which specifically comprises the following steps:
(1) designing the thickness, the shape and the spacing of a resin sheet layer structure in the part model by using three-dimensional modeling software according to the appearance, the wall thickness and the working load of the part to obtain a three-dimensional model of the resin mold;
the method comprises the following steps that a connecting structure and through holes between resin sheet layers are designed, the connecting structure is used for keeping the distance between the resin layers, and a metal infiltration channel is formed after the resin sheets are burned out and used for connecting metal layers; the through hole is used for ceramic slurry to flow and is connected with the ceramic layer;
(2) and converting the three-dimensional model of the resin mold into an STL format, slicing the three-dimensional model in layers, carrying out support treatment, introducing the three-dimensional model into SL (static pressure) molding equipment for preparation, cleaning the liquid residual resin on the surface, removing the support, and curing to obtain the part resin mold with the internal laminated structure.
Preferably, the resin sheet layer thickness is designed to be a minimum of 100 μm.
Preferably, the gel injection molding method in the step 2) adopts an acrylamide water-based gel system, the ceramic solid phase content is 40-60%, and the slurry viscosity is less than 1 Pa.s.
Preferably, the ceramic powder contained in the ceramic slurry in step 2) is alumina, zirconia, silicon carbide, titanium carbide, tungsten carbide, boron carbide, titanium boride, zirconium boride or silicon nitride.
Preferably, the following operations are further included between the step 4) and the step 5):
and depositing an interface layer material on the surface of the layered ceramic blank by adopting a chemical vapor deposition method.
Still further preferably, the vapor deposition interface layer material is carbon, silicon carbide, silicon nitride, boron nitride or metallic nickel.
The metal infiltration process in the step 5) is pressureless infiltration, specifically argon is used as protective gas, and two or more alloys of aluminum, magnesium, copper, iron, titanium, nickel and zirconium are used as infiltration metals.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention discloses a preparation method of a layered metal-ceramic composite part, which is based on the principle that layered toughening has good effect, and comprises the steps of firstly preparing a resin mold for ceramic slurry gel injection molding with a layered structure inside by a photocuring rapid prototyping technology, then preparing a part ceramic blank by adopting gel injection molding, freeze drying and degreasing sintering, controlling the interface combination condition or improving the wettability between an impregnated metal melt and ceramic by using a gas-phase deposition interface layer material, and finally realizing the compounding of metal and ceramic by non-pressure metal impregnation to obtain the layered metal toughened metal-ceramic composite part with the micron to millimeter scale inside. The method of the invention introduces a high-flexibility and high-precision photocuring rapid molding technology to design the metal toughening layer in and between layers, realizes the control of the compounding mode of metal and ceramic in the composite material, and the single layer of the same material can be designed into a closed or non-closed curved surface according to the requirements, and the layers of the same material can be connected with each other, realizes the cross-linking and intercommunication structure of the metal layer and the ceramic layer, and improves the mechanical property of the laminated structure. The method can expand the designability of parts and obtain good layered metal oriented toughening effect on metal-ceramic composite material parts.
Drawings
FIG. 1 is a schematic view of the internal layered structure of a resin mold;
FIG. 2 is a schematic view of a single resin sheet layer;
FIG. 3 is a schematic cross-sectional view of FIG. 2;
FIG. 4 is a schematic structural view of parts of embodiment 1; wherein, (a) is a perspective view; (b) is a cross section;
FIG. 5 is a schematic structural view of parts of embodiment 2; wherein, (a) is a perspective view; (b) is a cross section;
FIG. 6 is a schematic view of the structure of a resin sheet layer of example 2;
wherein 1 is a resin sheet layer; 2 is a resin mold shell; 3 is a through hole; and 4 is an interlayer connection structure.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
A method for preparing a layered metal-ceramic composite part, comprising the steps of:
1) resin mould for preparing part with internal laminated structure
The thickness, shape and spacing of the resin sheet layer structure in the part model are designed according to the form of figure 4 by UG three-dimensional modeling, the thickness of the resin sheet layer is 150 μm, the spacing of the sheet layers is 500 μm, and the resin sheet layer connecting structure and the through holes are designed according to figures 2 and 3; and then converting the designed three-dimensional model of the resin mold into an STL format, and carrying out layered slicing and supporting treatment on the model by using Magics software. And importing the data processed by the Magics into an RP manufacturing program of an SPS600 photocuring rapid prototyping machine to prepare a blade photocuring resin mold. Cleaning off the residual resin on the surface with alcohol, removing the support, placing the resin mold into an ultraviolet curing box, and further curing to obtain a resin mold with a layered structure inside, as shown in fig. 1, wherein 1 is a resin sheet layer; and 2 is a resin mold shell.
2) Gel casting
Acrylamide (AM) and N, N' -Methylene Bisacrylamide (MBAM) are dissolved into deionized water according to the mass ratio of 24:1 by adopting an acrylamide water-based gel system to prepare a premixed liquid with the mass fraction of 15%. Weighing the premixed liquid according to the using amount of the ceramic slurry, pouring the premixed liquid into a ball milling tank, slowly adding silicon carbide (SiC) ceramic powder (with the grain size of 1-50 mu m gradation), adding a tetramethylammonium hydroxide solution with 2 wt% of solid phase components as a dispersing agent, and performing ball milling for 30 minutes by using a planetary ball mill and a corundum milling ball with the mass ratio of the material balls of 1:2.5 and the rotating speed of 360r/min to prepare the ceramic slurry with the solid phase content of 60% and the slurry viscosity of less than 1 Pa.s. Adding a prepared catalyst TEMED (25 mass percent of tetramethylethylenediamine solution) and an initiator APS (30 mass percent of ammonium persulfate solution) into the prepared ceramic slurry, wherein the mass ratio of the catalyst to the initiator is 1: 6-7. And uniformly stirring in a vacuum casting machine, pouring into a resin mold, standing at normal temperature in an atmospheric environment for 40min after vacuum casting is finished, and performing monomer crosslinking and curing to obtain a part biscuit.
3) Freeze drying process
And (2) freezing the solidified ceramic biscuit of the part in a freezing cabinet at the temperature of-30 ℃ to ensure that the water in the ceramic biscuit of the part is completely frozen and crystallized, taking out the ceramic biscuit of the part, stripping the resin mold shell by using liquid nitrogen, putting the ceramic biscuit of the part into a freeze dryer, and freeze-drying for 72 hours in a vacuum environment of 1-10 Pa.
4) Degreasing
And (3) putting the dried ceramic biscuit of the part into a vacuum sintering furnace, carrying out vacuum degreasing treatment on the ceramic biscuit of the part at 900 ℃, and burning out organic matters remained in the biscuit to obtain a ceramic blank body with a laminated structure formed by resin sheet layers in the biscuit.
5) Chemical vapor deposition
And placing the degreased ceramic blank in chemical vapor deposition equipment, and performing chemical vapor deposition on a Si interface layer on the surface of the ceramic blank, wherein the thickness of the Si interface layer is 5-10 mu m.
6) Infiltration of metals
And (3) putting the ceramic blank subjected to chemical vapor deposition into a non-pressure infiltration furnace, taking argon as a protective gas, taking Al-Si-Mg alloy as a main component of the infiltration metal, and carrying out heat preservation for 2 hours at 950 ℃ for infiltration. And carrying out surface finish machining to obtain the layered-ceramic composite material part with the micrometer-millimeter scale inside.
Example 2
A method for preparing a layered metal-ceramic composite part, comprising the steps of:
1) resin mould for preparing part with internal laminated structure
The thickness, shape and spacing of the resin sheet layer structure in the part model are designed according to the form of figure 5 by UG three-dimensional modeling, the thickness of the resin sheet layer is 200 μm, the spacing of the sheet layers is 500 μm, the resin sheet layer connecting structure and the through holes are designed according to figure 6, in the figure, 3 is the through holes, and 4 is the interlayer connecting structure. And then converting the designed three-dimensional model of the resin mold into an STL format, and carrying out layered slicing and supporting treatment on the model by using Magics software. And importing the data processed by the Magics into an RP manufacturing program of an SPS600 photocuring rapid prototyping machine to prepare a blade photocuring resin mold. And cleaning the liquid residual resin on the surface by using alcohol, removing the support, and placing the resin mold into an ultraviolet curing box for further curing to obtain the resin mold with the internal laminated structure.
2) Gel casting
Acrylamide (AM) and N, N' -Methylene Bisacrylamide (MBAM) are dissolved into deionized water according to the mass ratio of 24:1 by adopting an acrylamide water-based gel system to prepare a premixed liquid with the mass fraction of 15%. Weighing the premixed liquid according to the using amount of the ceramic slurry, pouring the premixed liquid into a ball milling tank, slowly adding alumina (Al2O3) ceramic powder (with the grain size of 1-100 mu m gradation), adding a tetramethylammonium hydroxide solution with 2 wt% of solid phase components as a dispersing agent, and performing ball milling for 30 minutes by using a planetary ball mill and a corundum milling ball with the mass ratio of the material balls to the material balls of 1:2.5 and the rotating speed of 360r/min to prepare the ceramic slurry with the solid phase content of 60% and the slurry viscosity of less than 1 Pa.s. Adding a prepared catalyst TEMED (25 mass percent of tetramethylethylenediamine solution) and an initiator APS (30 mass percent of ammonium persulfate solution) into the prepared ceramic slurry, wherein the mass ratio of the catalyst to the initiator is 1: 6-7. And uniformly stirring in a vacuum casting machine, pouring into a resin mold, standing at normal temperature in an atmospheric environment for 40min after vacuum casting is finished, and performing monomer crosslinking and curing to obtain a part biscuit.
3) Freeze drying process
And (2) freezing the solidified ceramic biscuit of the part in a freezing cabinet at the temperature of-30 ℃ to ensure that the water in the ceramic biscuit of the part is completely frozen and crystallized, taking out the ceramic biscuit of the part, stripping the resin mold shell by using liquid nitrogen, putting the ceramic biscuit of the part into a freeze dryer, and freeze-drying for 72 hours in a vacuum environment of 1-10 Pa.
4) Degreasing
And (3) putting the dried ceramic biscuit of the part into a vacuum sintering furnace, carrying out vacuum degreasing treatment on the ceramic biscuit of the part at 900 ℃, and burning out organic matters remained in the biscuit to obtain a ceramic blank body with a laminated structure formed by resin sheet layers in the biscuit.
5) Infiltration of metals
Putting the ceramic body into a pressureless infiltration furnace, taking argon as shielding gas, taking Al-Si-Mg alloy as a main component of infiltration metal, and carrying out heat preservation for 2 hours at 950 ℃ for infiltration. And performing surface finishing to obtain the laminated metal toughened metal-ceramic composite material part with the micrometer-millimeter scale inside.
Claims (7)
1. A method for preparing a layered metal-ceramic composite part, comprising the steps of:
step 1) preparing a part resin mold with a layered structure inside by a photocuring rapid prototyping technology, which specifically comprises the following steps:
(1) designing the thickness, the shape and the spacing of a resin sheet layer structure in the part model by using three-dimensional modeling software according to the appearance, the wall thickness and the working load of the part to obtain a three-dimensional model of the resin mold;
the method comprises the following steps that a connecting structure and through holes between resin sheet layers are designed, the connecting structure is used for keeping the distance between the resin layers, and a metal infiltration channel is formed after the resin sheets are burned out and used for connecting metal layers; the through hole is used for ceramic slurry to flow and is connected with the ceramic layer;
(2) converting the three-dimensional model of the resin mold into an STL format, slicing in layers, carrying out support treatment, introducing into SL (static pressure) molding equipment for preparation, cleaning away liquid residual resin on the surface, removing the support, and curing to obtain a part resin mold with a layered structure inside;
step 2) preparing ceramic slurry by adopting a gel injection molding method, and obtaining a ceramic biscuit of the part through a vacuum injection molding process;
step 3) performing freeze drying treatment on the part ceramic biscuit, and removing the resin mold shell;
step 4) performing vacuum degreasing treatment on the ceramic biscuit of the part processed in the step 3) at 600-900 ℃, and burning out organic matters remained in the biscuit to obtain a ceramic blank body with a laminated structure and a resin sheet layer formed in the ceramic blank body;
step 5) carrying out metal infiltration on the ceramic blank treated in the step 4) by adopting a metal infiltration process, and then carrying out surface processing to obtain a metal-ceramic composite part toughened by layered metal with the internal dimension ranging from micron to millimeter;
the photocuring rapid prototyping technology in the step 1) can carry out in-layer and interlayer design on the metal toughening layer to realize control on the compounding mode of metal and ceramic in the composite material, and the single layer of the same material can be designed into a closed or non-closed curved surface according to requirements, and the layers of the same material can be connected with each other to realize a cross-linking and intercommunication structure of the metal layer and the ceramic layer.
2. The method of manufacturing a layered metal-ceramic composite part according to claim 1, wherein the resin sheet layer thickness is designed to be a minimum of 100 μm.
3. The method for preparing a layered metal-ceramic composite part according to claim 1, wherein the gel injection molding method of step 2) employs an acrylamide water-based gel system, the ceramic solid content is 40% to 60%, and the slurry viscosity is less than 1 Pa-s.
4. The method for preparing the layered metal-ceramic composite part according to claim 1, wherein the ceramic powder contained in the ceramic slurry of step 2) is alumina, zirconia, silicon carbide, titanium carbide, tungsten carbide, boron carbide, titanium boride, zirconium boride or silicon nitride.
5. The method for preparing a layered metal-ceramic composite part according to claim 1, further comprising the following operations between step 4) and step 5):
and depositing an interface layer material on the surface of the layered ceramic blank by adopting a chemical vapor deposition method.
6. The method of making a layered metal-ceramic composite part according to claim 5, wherein the vapor deposited interface layer material is carbon, silicon carbide, silicon nitride, boron nitride, or metallic nickel.
7. The method of claim 1, wherein the metal infiltration step of step 5) is pressureless infiltration, specifically argon is used as a shielding gas, and an alloy of two or more of aluminum, magnesium, copper, iron, titanium, nickel, and zirconium is used as the infiltration metal.
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