CN111217609B - Preparation method of 3D printing integral silicon carbide heat shield - Google Patents
Preparation method of 3D printing integral silicon carbide heat shield Download PDFInfo
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- 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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Abstract
The invention discloses a preparation method of a 3D printing integral silicon carbide heat shield, which comprises the steps of adding prepared ceramic slurry into a charging barrel of a 3D printer, extruding the ceramic slurry into a silk-shaped unit body, stacking layer by layer, and forming to obtain an integral heat shield ceramic green body; the first layer is an inner layer, the inner layer is an integral structural layer, the thickness of the inner layer is 5-15 mm, and the inner wall of the inner layer is a main reflecting surface; the second layer begins with a secondary reflective layer having convective slits that create turbulent flow. The 3D printing integral silicon carbide heat shield prepared by the method; the printable heat shield has a regular integral structure, a polished inner surface forms a reflecting surface, and high-temperature desiliconization treatment is carried out to remove high-temperature sintering pollution such as silicon vapor and the like; the high-temperature chemical stability is good, and the atmosphere in the furnace has a three-dimensional network outer layer with lower thermal conductivity and the stability of a printing structure, so that the heat shield has an accurate process installation position and better controllability.
Description
Technical Field
The invention relates to the technical field of high-temperature resistance furnaces, in particular to a preparation method of a 3D printing integral silicon carbide heat shield.
Background
The high-temperature resistance furnace is equipment for performing sintering, heating, melting, heat treatment and other processes on an article by using resistance heating in vacuum or inert gas atmosphere, and is widely applied to sintering and research tests of high-temperature materials such as inorganic materials, ceramic materials, functional materials, hard alloys, high-melting-point oxides, high-temperature metals and the like.
The heat shield of the high-temperature resistance furnace has the main functions of heat insulation and heat preservation, reduces heat loss in the furnace and enables a heating zone in the furnace body and workpieces in the furnace to reach and maintain a certain required temperature. The heat shield has the effect of preventing heat loss, and the heat insulation effect of the heat shield directly influences the heat preservation performance in the furnace, so that the overall performance of the high-temperature furnace is greatly influenced. Therefore, the method has important significance in reducing the energy consumption of the high-temperature resistance furnace, improving the heat efficiency and protecting the environment.
The common heat shields of the vacuum resistance furnace are metal heat shields, sandwich type heat shields and nonmetal heat shields.
(1) Metal heat shield
The metal screen is heated and cooled quickly, the advantage of high vacuum of 10-8Pa is easily achieved, and the metal screen is widely applied.
The metal heat shield has the disadvantage that metal vapor at high temperature may affect the sintering or testing of the material. The maximum service temperature of tungsten is 2650 ℃, the maximum service temperature of molybdenum is 1900 ℃, the maximum service temperature of tantalum is 2400 ℃, and the maximum service temperature of stainless steel is 950 ℃.
(2) Sandwich type heat shield
The inner layer is a molybdenum sheet, the middle layer is a carbon felt, a graphite felt or an aluminum silicate fiber felt, the outer layer is stainless steel, and the influence on the vacuum degree is caused by moisture absorption, binder volatilization and the like of the fiber.
(3) Graphite felt and carbon felt heat shield
The graphite felt heat shield is generally wrapped with a steel plate or steel frame as a support to maintain its shape. The thermal insulation performance is reduced by the reaction of the carbon felt graphite felt with oxygen, water vapor and oil vapor. The silicon carbide ceramic has the thermal conductivity of 90-110 w/(m.k), is relatively close to that of graphite of 129 w/(m.k), and has excellent thermal shock resistance. The pore structure in the ceramic greatly reduces heat conduction, and the heat conductivity of the ceramic is greatly reduced, so that the ceramic is an ideal heat insulation material.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a 3D printing integral silicon carbide heat shield, which has a regular integral structure, a polished inner surface forming a reflecting surface, a three-dimensional network outer layer with lower heat conductivity and printing structure stability, enables the heat shield to have an accurate process installation position, and is subjected to high-temperature desiliconization treatment, silicon vapor and other high-temperature sintering pollution removal and high-temperature chemical stability of silicon carbide, so that the atmosphere in a furnace has better controllability.
The technical scheme of the invention is to provide a preparation method of a 3D printing integral silicon carbide heat shield, which comprises the following steps: the method comprises the following steps: (1) slicing and layering the designed model of the heat shield, determining a printing program according to the structure, and importing the program into a 3D printing equipment program; (2) uniformly mixing silicon carbide powder, a dispersing agent, a binder and deionized water, ball-milling for 1-24 h, and then carrying out vacuum defoaming on the ball-milled slurry in a vacuum defoaming machine for 10-60 min to obtain ceramic slurry; (3) adding the prepared ceramic slurry into a charging barrel of a 3D printer, extruding the ceramic slurry into a filamentous unit body under the control of the printing program in the step (1), stacking layer by layer, and forming to obtain an integral ceramic heat shield ceramic green body; the ceramic green body of the ceramic heat shield is a cylinder or a square cylinder in shape, the first layer is an inner layer, the inner layer is an integral structure layer, the thickness is 5-15 mm, and the inner wall of the ceramic green body is a main reflecting surface; the second layer is an auxiliary reflecting layer, the auxiliary reflecting layer is provided with convection gaps and micro-pores for forming turbulent flow, the thickness of the auxiliary reflecting layer is 3-10 mm, and the number of layers is 3-15; the layers are connected by a connecting column, and the inner wall of the auxiliary reflecting layer is an auxiliary reflecting surface; (4) placing the printed ceramic green body of the ceramic heat shield in an oven at 25-150 ℃ for 0.5-24 h; (5) dewaxing the dried ceramic green body of the ceramic heat shield; (6) performing infiltration sintering on the dewaxed ceramic green body of the ceramic heat shield at 1450-1600 ℃ by adopting liquid silicon to obtain a silicon carbide ceramic heat shield; (7) desiliconizing the sintered silicon carbide ceramic heat shield at 1650-2300 ℃; (8) and polishing the inner surface of the silicon carbide ceramic heat shield after desiliconization to form a reflecting surface.
Specifically, the connecting cylinder is a cylinder, and the geometric dimension of the heat shield can be controlled at will according to design requirements.
Specifically, the silicon carbide ceramic powder accounts for 10-98 wt%, the dispersing agent accounts for 0.1-10 wt%, the binder accounts for 0.1-20 wt%, the deionized water accounts for 20-50 wt%, and the defoaming agent accounts for 0.01-8 wt%.
Specifically, the dispersant is one or more of ammonia water, tetramethylammonium hydroxide, ammonium polyacrylate, polyethyleneimine, sodium hexametaphosphate, sodium tripolyphosphate and polyethylene glycol.
Specifically, the binder is one or more of sodium carboxymethylcellulose, gum arabic, xanthan gum, phenolic resin, gelatin, silica sol, sodium alginate, agarose, polyvinyl alcohol, acrylic acid, and dextrin.
Specifically, the diameter of the connecting cylinder is 5-20 mm.
After the method is adopted, the invention has the following advantages: (1) have regular overall structure, because it is 3D whole printing, and the inlayer is as the structural layer of whole heat screen, and thickness is 5 ~ 15mm, can have regular wholeness and can guarantee again to have sufficient intensity. (2) The polished inner surface forms a reflecting surface; the heat is specularly reflected, more heat is reflected, and the absorbed heat is reduced, so that the heat is reduced to be transferred to the outer surface of the heat shield. And because the auxiliary reflecting layer is provided with a convection gap for forming turbulent flow, a better cooling effect can be achieved. (3) The outer layer of the three-dimensional network has lower thermal conductivity, the layers are connected by cylinders, and the maximum supporting force is obtained by the minimum sectional area; the connection columns of adjacent layers are at different positions, and the conduction distance is increased, so that the conduction loss is reduced. (4) The stability of the printing structure can ensure the uniformity of the size, and the design requirement is met, so that the heat shield has an accurate process installation position; (5) high-temperature desiliconization treatment is carried out to remove high-temperature sintering pollution such as silicon vapor and the like; (6) the high-temperature chemical stability of the silicon carbide ensures that the atmosphere in the furnace has better controllability. The high temperature resistant temperature is 2100 ℃ to 2300 ℃, and the highest heat shield can resist 2400 ℃ according to the different sizes of the heat shields.
Drawings
Fig. 1 is a schematic perspective view of a first embodiment of the present invention.
Fig. 2 is a schematic cross-sectional view of a first embodiment of the present invention.
Fig. 3 is an enlarged view of a portion a of fig. 2.
Fig. 4 is a schematic perspective view of a second embodiment of the present invention.
Fig. 5 is a schematic cross-sectional view of a second embodiment of the present invention.
Fig. 6 is an enlarged schematic view of a portion B of fig. 5.
Fig. 7 is a perspective view of a third embodiment of the present invention.
Fig. 8 is a schematic cross-sectional view of a third embodiment of the present invention.
Fig. 9 is an enlarged schematic view of the portion C of fig. 8.
Shown in the figure: 1. inner layer, 2, auxiliary reflection layer, 3, the spliced pole.
Detailed Description
The invention is further illustrated by the following figures and examples.
According to the preparation method of the 3D printing integral silicon carbide heat shield, all raw materials are commercially available products, and equipment is also conventional equipment in the industry. The deionized water added in the preparation process is only used as an auxiliary reagent and completely volatilized in a final product, so that the deionized water is not used as a main raw material.
Example one
As shown in fig. 1 to 3, a method for preparing a 3D printed integrated silicon carbide heat shield comprises the following steps:
(1) slicing and layering the designed model of the heat shield, determining a printing program according to the structure, and importing the program into a 3D printing equipment program; (2) uniformly mixing silicon carbide powder, a dispersing agent, a binder and deionized water, ball-milling for 2 hours, and then carrying out vacuum defoaming on the ball-milled slurry in a vacuum defoaming machine for 10min to obtain ceramic slurry;
the proportion of the silicon carbide ceramic powder is 50wt%, the proportion of the dispersing agent is 0.1 wt%, the proportion of the binding agent is 0.1 wt%, the proportion of the deionized water is 49.79 wt%, and the proportion of the defoaming agent is 0.01%. The dispersing agent adopts ammonia water, and the binder adopts sodium carboxymethylcellulose; (3) adding the prepared ceramic slurry into a charging barrel of a 3D printer, extruding the ceramic slurry into a filamentous unit body under the control of the printing program in the step (1), stacking layer by layer, and forming to obtain an integral ceramic heat shield green body; furthermore, the ceramic heat shield green body is cylindrical in shape, the first layer is an inner layer 1, the inner layer is an integral structure layer, the thickness is 16mm, and the inner wall of the ceramic heat shield green body is a main reflecting surface; the second layer is an auxiliary reflecting layer 2, the auxiliary reflecting layer is provided with convection gaps for forming turbulent flow, the thickness of the auxiliary reflecting layer is 7mm, and the number of layers is 10; the layers are connected by the connecting cylinders 3, and the connecting cylinders 3 on the front side and the back side of each auxiliary reflecting layer are distributed in a staggered manner and are not on the same axis, so that the direct transfer of heat is reduced. The inner wall of the auxiliary reflecting layer is an auxiliary reflecting surface. The inner diameter of the cylinder is 600mm, and the high temperature resistant temperature can reach 2100 ℃. (4) Placing the printed ceramic heat shield green body in an oven at 25 ℃ for 1 h; (5) dewaxing the dried ceramic heat shield green body; (6) the dewaxed ceramic heat shield green body is sintered at 1450 ℃ by adopting liquid silicon infiltration to obtain an integral silicon carbide ceramic heat shield; (7) desiliconizing the sintered silicon carbide ceramic heat shield at 1700 ℃; (8) and polishing the inner surface of the silicon carbide ceramic heat shield after desiliconization to form a reflecting surface.
Example two
As shown in fig. 4-6, a method for preparing a 3D printed integrated silicon carbide heat shield comprises the following steps:
(1) slicing and layering the designed model of the heat shield, determining a printing program according to the structure, and importing the program into a 3D printing equipment program; (2) uniformly mixing silicon carbide powder, a dispersing agent, a binder and deionized water, carrying out ball milling for 12 hours, and then carrying out vacuum defoaming on the ball-milled slurry in a vacuum defoaming machine for 35min to obtain ceramic slurry; the silicon carbide ceramic powder accounts for 60 wt%, the dispersing agent accounts for 5 wt%, the binder accounts for 5 wt%, the deionized water accounts for 26 wt%, and the defoaming agent accounts for 4 wt%. The dispersant is polyethyleneimine, and the binder is gelatin. (3) Adding the prepared ceramic slurry into a charging barrel of a 3D printer, extruding the ceramic slurry into a filamentous unit body under the control of the printing program in the step (1), stacking layer by layer, and forming to obtain an integral ceramic heat shield green body; the ceramic heat shield green body is cylindrical in shape, a bottom plate is arranged on the bottom surface of the ceramic heat shield green body, a through hole is formed in the center of the bottom plate, the side wall of the ceramic heat shield green body and the first layer of the bottom plate are both inner layers 1, each inner layer is an integral structure layer, the thickness of each inner layer is 8mm, and the inner wall of each inner layer is a main reflecting surface; the second layer is an auxiliary reflecting layer 2, the auxiliary reflecting layer is provided with convection gaps for forming turbulent flow, the thickness of the auxiliary reflecting layer is 3mm, and the number of layers is 6; the layers are connected by a connecting column 3, the diameter of the connecting column is 10mm, and the inner wall of the auxiliary reflecting layer is an auxiliary reflecting surface. The outer diameter of the cylinder is 600mm, and the high temperature resistant temperature can reach 2100 ℃. (4) Placing the printed ceramic heat shield green body in an oven at 100 ℃, and drying for 12 h; (5) dewaxing the dried ceramic heat shield green body; (6) the dewaxed ceramic heat shield green body is sintered at 1500 ℃ by adopting liquid silicon infiltration to obtain an integral silicon carbide ceramic heat shield; (7) desiliconizing the sintered silicon carbide ceramic heat shield at 1900 ℃; (8) and polishing the inner surface of the silicon carbide ceramic heat shield after desiliconization to form a reflecting surface.
EXAMPLE III
As shown in fig. 7-9, a method for preparing a 3D printed integrated silicon carbide heat shield comprises the following steps:
(1) slicing and layering the designed model of the heat shield, determining a printing program according to the structure, and importing the program into a 3D printing equipment program; (2) uniformly mixing silicon carbide powder, a dispersing agent, a binder and deionized water, ball-milling for 1-24 h, and then carrying out vacuum defoaming on the ball-milled slurry in a vacuum defoaming machine for 60min to obtain ceramic slurry; the proportion of the silicon carbide ceramic powder is 12 wt%, the proportion of the dispersing agent is 10wt%, the proportion of the binding agent is 20wt%, the proportion of the deionized water is 50wt%, and the proportion of the defoaming agent is 8%. The dispersant is sodium tripolyphosphate and the binder is dextrin. (3) Adding the prepared ceramic slurry into a charging barrel of a 3D printer, extruding the ceramic slurry into a filamentous unit body under the control of the printing program in the step (1), stacking layer by layer, and forming to obtain an integral ceramic heat shield green body; furthermore, the ceramic heat shield green body is of a cylindrical structure with a hexagonal cross section, the first layer is an inner layer 1, the inner layer is an integral structure layer, the thickness is 15mm, and the inner wall of the ceramic heat shield green body is a main reflecting surface; the second layer is an auxiliary reflecting layer 2, the auxiliary reflecting layer is provided with convection gaps for forming turbulent flow, the thickness of the auxiliary reflecting layer is 10mm, and the number of layers is 10; the layers are connected by a connecting cylinder 2, and the connecting cylinder in the silicon carbide ceramic heat shield is cylindrical. The diameter of the connecting cylinder is 20 mm. The inner wall of the auxiliary reflecting layer is an auxiliary reflecting surface. The outer diameter of a hexagonal concentric circle is 1000mm, and the highest high-temperature resistant temperature can reach 2300 ℃. (4) Placing the printed ceramic heat shield green body in an oven at 150 ℃ for 24 hours; (5) dewaxing the dried ceramic heat shield green body; (6) the dewaxed ceramic heat shield green body is sintered at 1600 ℃ by adopting liquid silicon infiltration to obtain an integral silicon carbide ceramic heat shield; (7) desiliconizing the sintered silicon carbide ceramic heat shield at 2300 ℃; (8) and polishing the inner surface of the silicon carbide ceramic heat shield after desiliconization to form a reflecting surface.
Claims (5)
1. A preparation method of a 3D printing integral silicon carbide heat shield is characterized by comprising the following steps: the method comprises the following steps:
(1) slicing and layering the designed model of the heat shield, determining a printing program according to the structure, and importing the program into a 3D printing equipment program;
(2) uniformly mixing silicon carbide powder, a dispersing agent, a binder and deionized water, ball-milling for 1-24 h, and then carrying out vacuum defoaming on the ball-milled slurry in a vacuum defoaming machine for 10-60 min to obtain ceramic slurry;
(3) adding the prepared ceramic slurry into a charging barrel of a 3D printer, extruding the ceramic slurry into a filamentous unit body under the control of the printing program in the step (1), stacking layer by layer, and forming to obtain an integral ceramic heat shield ceramic green body;
the ceramic green body of the ceramic heat shield is a cylinder or a square cylinder in shape, the first layer is an inner layer, the inner layer is an integral structure layer, the thickness is 5-15 mm, and the inner wall of the ceramic green body is a main reflecting surface; the second layer is an auxiliary reflecting layer, the auxiliary reflecting layer is provided with convection gaps and micro-pores for forming turbulent flow, the thickness of the auxiliary reflecting layer is 3-10 mm, and the number of layers is 3-15; the layers are connected by connecting cylinders, the connecting cylinders are cylinders, and the connecting cylinders of adjacent layers are in different positions; the inner wall of the auxiliary reflecting layer is an auxiliary reflecting surface;
(4) placing the printed ceramic green body of the ceramic heat shield in an oven at 25-150 ℃ for 0.5-24 h;
(5) dewaxing the dried ceramic green body of the ceramic heat shield;
(6) performing infiltration sintering on the dewaxed ceramic green body of the ceramic heat shield at 1450-1600 ℃ by adopting liquid silicon to obtain a silicon carbide ceramic heat shield;
(7) desiliconizing the sintered silicon carbide ceramic heat shield at 1650-2300 ℃;
(8) and polishing the inner surface of the silicon carbide ceramic heat shield after desiliconization to form a reflecting surface.
2. The method for preparing a 3D printing integrated silicon carbide heat shield according to claim 1, wherein the method comprises the following steps: the silicon carbide ceramic powder comprises 10-98 wt% of silicon carbide ceramic powder, 0.1-10 wt% of dispersing agent, 0.1-20 wt% of binder, 20-50 wt% of deionized water and 0.01-8 wt% of defoaming agent.
3. The method for preparing a 3D printing integrated silicon carbide heat shield according to claim 1, wherein the method comprises the following steps: the dispersant is one or more of ammonia water, tetramethyl ammonium hydroxide, ammonium polyacrylate, polyethyleneimine, sodium hexametaphosphate, sodium tripolyphosphate and polyethylene glycol.
4. The method for preparing a 3D printing integrated silicon carbide heat shield according to claim 1, wherein the method comprises the following steps: the binder is one or more of sodium carboxymethylcellulose, gum arabic, xanthan gum, phenolic resin, gelatin, silica sol, sodium alginate, agarose, polyvinyl alcohol, acrylic acid and dextrin.
5. The method for preparing a 3D printing integrated silicon carbide heat shield according to claim 1, wherein the method comprises the following steps: the diameter of the connecting cylinder is 5-20 mm.
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| CN116675539A (en) * | 2023-06-16 | 2023-09-01 | 山田新材料集团有限公司 | Preparation method of extrusion molding 3D printing high-solid-content high-heat-conductivity silicon carbide ceramic |
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| US9803296B2 (en) * | 2014-02-18 | 2017-10-31 | Advanced Ceramic Fibers, Llc | Metal carbide fibers and methods for their manufacture |
| CN202310130U (en) * | 2011-07-19 | 2012-07-04 | 北京智创联合科技有限公司 | Heat shield possessing multilayer structure |
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2019
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