A porous plate with a matrix hole structure based on 3D printing technology and a preparation process method

Abstract

The present invention provides a porous plate with a matrix hole structure based on 3D printing technology. The porous plate is a silicon carbide plate, which is a porous plate prepared by 3D printing technology first, and then a pneumatic hammer is used to feed compressed gas to clean the hole structure; the pores are arranged in a matrix distribution. In addition, the present invention also provides a preparation method of the porous plate. By designing the process and processing method, the improvement of the ceramic preparation efficiency by more than 50% and the finished product rate by more than 70% are effectively realized, thereby improving the product quality and production efficiency.

Description

Technical Field

[0001] The present invention belongs to the technical field of ceramic materials and preparation processes, and particularly relates to a porous plate with a matrix hole structure based on 3D printing technology and a preparation process method. Background Art

[0002] Traditional ceramic porous plates are components mainly used in the wafer processing process. Generally, the manufacturing method is sintering first and then machining. However, due to the characteristics of high hardness, brittleness, and difficult machining of ceramics, it has always been impossible to solve the problems of low processing efficiency, easy chipping, and low yield when obtaining a porous structure on a ceramic plate. Now, some researchers, such as those disclosed in CN202311276320.5, have provided a preparation method for cutting array through-holes on a ceramic sheet using laser cutting technology. Although array through-holes can be obtained, the requirements for the welding process are high, and the possibility of mass production is relatively low. In addition, for current traditional ceramic porous plates, due to process limitations during processing, the main products on the market have simple structures, and it is difficult to process complex structures, especially the processing and forming of ultra-thin ceramic plates with matrix holes that require high flatness. Therefore, there is an urgent need for a process in the field of preparing ceramic porous plates to solve the above problems. Summary of the Invention

[0003] Technical Solution: To solve the above technical problems, the present invention provides a porous plate with a matrix hole structure based on 3D printing technology. The porous plate is a silicon carbide plate, which is a porous plate prepared by 3D printing technology first, and then a pneumatic hammer is used to feed compressed gas to clean the hole structure; the pores are arranged in a matrix distribution.

[0004] As an improvement, the plate thickness is 3 - 4 mm, the length and width of the plate are both 250 - 350 mm, and the pore density is 270 - 300 per decimeter 2 .

[0005] As an improvement, the pressure of the compressed gas is 0.6 - 1 mpa, and the distance from the surface of the porous plate is 2 - 3 mm.

[0006] At the same time, a preparation process for the above-mentioned porous plate with a matrix hole structure based on 3D printing technology is provided. The specific steps are as follows: The specific steps are as follows:

[0007] (1) Preparation work:

[0008] (1.1) Preparation of raw material powder: Add silicon carbide powder to a mixer, add water and a dispersant, then perform centrifugal ball milling, and after drying, dispersing, and grading and screening, obtain the raw material powder for the required 3D printing powder, and the powder diameter is 20 - 200 μm;

[0009] (1.2) Preparation of printing powder:

[0010] Mix the above raw material powder with a curing agent to obtain printing powder;

[0011] (2) 3D printing process

[0012] (2.1) Import the part design drawing into a 3D printer and perform slicing. The number of slices is:

[0013]

[0014] N is the number of slices, k is a constant,, Z is the height of the part in the printing direction, d is the layer height, for example, it is a multiple of the diameter of the printing material silicon carbide powder;

[0015] (2.2) Preparation of green body printing:

[0016] Add the printing powder into the storage tank of the 3D printer, and perform binder jet printing to the number of sliced layers by using the cyclic steps of "powder spreading - compaction - binder spraying", thus completing the preparation of the green body; the powder spreading thickness of the binder jet printing is 20 - 600 μm / layer;

[0017] (2.3) Removal of floating sand:

[0018] Take out the printed green body from the 3D printer and perform floating sand removal by using compressed air blowing; the blowing pressure is 0.1 - 0.5 MPa, and the blowing distance is 20 - 50 cm;

[0019] (3) Hole cleaning:

[0020] Use a pulse air hammer to move on the surface of the porous plate green body in step (2) at 1 - 10 mm, and perform sand blowing for each hole through the process of "pressurization - pulse blowing"; the pulse air hammer has a piston of a pneumatic hammer device, and realizes the pressurization and blowing processes by using reciprocating motion to achieve the purpose of hole cleaning; the working pressure of the pulse air hammer is 0.6 - 2 MPa, and the distance from the surface of the porous plate is 1 - 10 mm;

[0021] (4) High-temperature degreasing:

[0022] Perform high-temperature degreasing on the green body after removing floating sand in step (3), the degreasing temperature is 800 - 1300 °C, and the degreasing time is 1 - 8 h;

[0023] (5) Carburizing treatment:

[0024] (5.1) Mix carbon black, dispersant, solvent, emulsifier, and additive to prepare a carbon black solution;

[0025] (5.2) Place the degreased green body in step (4) in a vacuum impregnation tank and evacuate to a vacuum degree of 0.5 - 1.5 MPa;

[0026] (5.3) Introduce the carbon black solution into the impregnation tank in step (5.2), and keep the vacuum degree for impregnation for 0.5 - 5 h;

[0027] (5.4) Take out the impregnated green body in step (5.3), and dry it at 80 - 200 °C for 1 - 5 h to remove the solvent;

[0028] (5.5) Repeat steps (5.2) - (5.4) to obtain a carbon-containing green body;

[0029] (6) Reaction silicon infiltration:

[0030] Place the carbon-containing green body in step (5) in a sintering furnace, and carry out sintering silicon infiltration at 1500 - 1800 °C and a vacuum degree of 100 - 1000 Pa. The sintering time is 2 - 10 h to obtain silicon carbide ceramics.

[0031] As an improvement, the rotational speed of the centrifugal ball milling in step (1.1) is 500 - 2000 rpm, and the ball milling time is 1 - 24 h; the drying temperature is 80 - 150 °C, and the drying time is 1 - 10 h; the weight percentage of the dispersant in the total material amount is 0.01 - 0.5%; the weight percentage of water in the total material amount is 0.5 - 8%.

[0032] As an improvement, the mass percentages of each component in the carbon black solution in step (5.1) are: carbon black 20 - 60%, dispersant 1 - 5%, emulsifier 1 - 5%, additive 0.1 - 3%, and the balance is solvent; the emulsifier is alkylphenol polyoxyethylene ether, polyoxyethylene alkylamine, polyoxyethylene alkylolamide, glycerol caprylate, glycerol cocoate, stearic acid acyl ether or glycerol caprate; the additive is polycarbosilane or polycarbosiloxane.

[0033] As an improvement, in step (6) of sintering silicon infiltration, the ratio of the silicon material is 1 - 5% of the binder by mass percentage, 0.1 - 2% of boron nitride, 0.5 - 5% of water, and the balance is polysilicon particles.

[0034] Beneficial effects: The porous plate proposed by the present invention has the following advantages compared with the conventional ones:

[0035] (1) In the present invention, the 3D printing (SLS) technology is adopted as a whole. After printing, the internal holes will be blocked due to the resin flow and need to be sandblasted. Traditional sandblasting requires manual cleaning of each hole one by one, resulting in too high labor costs.

[0036] (2) In the present invention, an air hammer is used for cleaning and dredging, and compressed air is used to feed and control the air hammer. The pressure of the compressed air is 0.6 - 1 mpa. The air hammer moves reciprocally through the piston, pressurizes at a distance of 2 - 3 mm from the product surface, and achieves the effect of cleaning the holes through the back-and-forth pulsed gas impact.

[0037] (3) By designing the process and processing method, the present invention effectively improves the ceramic preparation efficiency (more than 50%) and the finished product rate (more than 70%), thereby improving the product quality and production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] Figure 1 It is a schematic structural diagram of the porous plate of the present invention.

[0039] Figure 2 It is a schematic flow diagram of the preparation method of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0040] The technical solutions in the embodiments of the present invention will be clearly and completely described below, so that those skilled in the art can better understand the advantages and features of the present invention, and thus make a clearer definition of the protection scope of the present invention. The embodiments described in the present invention are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative work belong to the protection scope of the present invention.

[0041] A porous plate with a matrix hole structure based on 3D printing technology. The porous plate is a silicon carbide plate, which is a porous plate prepared by 3D printing technology first, and then a pneumatic hammer is used to feed compressed gas to clean the hole structure; the pores are arranged in a matrix distribution.

[0042] In the present invention, the plate thickness is 3 - 4 mm, the length and width of the plate are 250 - 350 mm, and the pore density is 270 - 300 per decimeter 2 . The pressure of the compressed gas is 0.6 - 1 mpa, and the distance from the surface of the porous plate is 2 - 3 mm. Compared with the conventional method in the present invention, it can solve the problem of powder adhesion in the holes caused by resin flow during the 3D printing process, and use an air hammer to clean the adhered substances in the holes, so that the hole structure of the ceramic green body is uniform.

[0043] The preparation process method of the porous plate with a matrix hole structure based on 3D printing technology of the present invention will be described in detail and introduced below through specific embodiments.

[0044] See Figure 1 As shown, it is a porous plate with a matrix hole structure based on 3D printing technology of the present invention. The plate size is 250 - 350 mm, the internal pore diameter is 1 - 10 mm, the plate thickness is 1 - 5 mm, preferably 3 - 4 mm, and the pore density is 270 - 300 per square decimeter.

[0045] See Figure 2As shown, it is the process flow chart for preparing the porous plate of the present invention. The present invention proposes a preparation process method for a porous plate with a matrix hole structure based on 3D printing technology. The specific steps include:

[0046] Step 1: Preparation work

[0047] Raw material powder preparation: Add silicon carbide powder into a mixer, add water and a dispersant, then carry out centrifugal ball milling, followed by drying, dispersing, and grading and screening to obtain the raw material powder for the required 3D printing powder. The powder diameter is 20 - 200 μm.

[0048] Printing powder preparation: Mix the above raw material powder with a curing agent to obtain the printing powder.

[0049] Preferably, in the present invention, the centrifugal ball milling speed is 500 - 2000 rpm, and the ball milling time is 1 - 24 h; the drying temperature is 80 - 150 °C, and the drying time is 1 - 10 h.

[0050] The dispersant is one or several of hydroxyethyl acrylate, trimethylolpropane triacrylate, dipentaerythritol hexaacrylate, pentaerythritol acrylate, BYK410, KOS110, or KOS2000, so that the silicon carbide powder is fully dispersed and suspended in water.

[0051] Preferably, in the present invention, the weight percentage of the dispersant in the total material is 0.01 - 0.5%; the weight percentage of the water in the total material is 0.5 - 8%.

[0052] Step 2: 3D printing process

[0053] First, import the part design drawing into a 3D printer and perform slicing. The number of slices is:

[0054]

[0055] N is the number of slices, k is a constant,, Z is the height of the part in the printing direction, d is the layer height, for example, a multiple of the diameter of the printing material silicon carbide powder;

[0056] Then, green body preparation: Add the printing powder into the storage tank of the 3D printer, and perform binder jet printing by using the cyclic steps of "powder spreading - compaction - binder spraying" until the number of slices is reached, that is, the green body preparation is completed; the powder spreading thickness for the binder jet printing is 20 - 600 μm / layer;

[0057] Finally, floating sand cleaning: Take out the printed green body from the 3D printer, and perform floating sand cleaning by using compressed air blowing; the blowing pressure is 0.1 - 0.5 MPa, and the blowing distance is 20 - 50 cm.

[0058] When setting the injection pressure in the present invention, if the pressure is too high, the green body will be damaged and scrapped; if the pressure is too low, it is difficult to clean the floating sand completely, and it needs to be cleaned again, reducing the production efficiency. The disadvantages brought by inappropriate injection distance highlight the advantages.

[0059] Step Three: Clean the holes

[0060] Use a pulsed air hammer to move on the surface of the porous plate green body in Step Two at a distance of 1-10 mm, and through the process of "pressurization - pulsed injection", blow and remove sand from each hole one by one; the pulsed air hammer has a piston of a pneumatic hammer device, and uses reciprocating motion to achieve the pressurization and injection processes to achieve the purpose of cleaning the holes; the working pressure of the pulsed air hammer is 0.6-2 MPa, and the distance from the surface of the porous plate is 1-10 mm.

[0061] Step Four: High-temperature degreasing

[0062] Subject the green body with floating sand removed in Step Three to high-temperature degreasing, with the degreasing temperature being 800-1300 °C and the degreasing time being 1-8 h.

[0063] In the present invention, the function of high-temperature degreasing is to remove organic substances such as the glue used in 3D printing, cause the organic substances to coke and decompose, and avoid generating pores during the sintering process, which affects the densification degree of the ceramic.

[0064] Step Five: Carburizing treatment

[0065] 5.1 Mix carbon black, dispersant, solvent, emulsifier, and additive to prepare a carbon black solution;

[0066] 5.2 Place the degreased green body in Step Four in a vacuum impregnation tank and evacuate to a vacuum degree of 0.5-1.5 MPa;

[0067] 5.3 Introduce the carbon black solution into the impregnation tank in Step 5.2 and keep the vacuum degree for impregnation for 0.5-5 h;

[0068] 5.4 Take out the impregnated green body in Step 5.3 and dry it at 80-200 °C for 1-5 h to remove the solvent;

[0069] 5.5 Repeat Steps 5.2-5.4 to obtain a carbon-containing green body.

[0070] Preferably, in 5.1 of the present invention, the mass percentages of each component in the carbon black solution include: 20-60% of carbon black, 1-5% of dispersant, 1-5% of emulsifier, 0.1-3% of additive, and the balance is solvent; the emulsifier is one or more of alkylphenol polyoxyethylene ether, polyoxyethylene alkylamine, polyoxyethylene alkylolamide, glycerol caprylate, glycerol cocoate, stearic acid acyl ether, or glycerol caprate; the additive is polycarbosilane or polycarbosiloxane.

[0071] Step 6: Reaction silicon infiltration

[0072] Place the carbon-containing green body obtained in Step 5 in a sintering furnace, and perform sintering silicon infiltration at 1500 - 1800 °C and a vacuum degree of 100 - 1000 Pa. The sintering time is 2 - 10 h to obtain silicon carbide ceramics.

[0073] Preferably, in the sintering silicon infiltration of the present invention, the ratio of silicon materials is 1 - 5% by mass of binder, 0.1 - 2% of boron nitride, 0.5 - 5% of water, and the balance is polysilicon particles.

[0074] In the present invention, the porosity of the 3D printed green body after direct sintering is extremely high, and the degree of ceramic densification is too low. It is necessary to introduce silicon carbide through carburization and silicon infiltration reactions to fill the voids and improve the densification degree.

[0075] Example 1

[0076] The present invention is produced and processed according to the above-provided preparation process method to obtain a porous plate, and multiple groups of parallel experimental tests are carried out on it. The performance characterization parameters during the test include density, hardness, porosity, flatness, roundness, and concentricity. The experimental data obtained are shown in Table 1.

[0077] Table 1 Performance parameters of the porous plate

[0078]

[0079] As can be seen from Table 1, the preparation process of the porous plate prepared by the present invention is excellent, and the performance is relatively stable. The plate density is 3.09 - 3.12 g / cm 3 , the hardness is 2190 - 2210 kg / mm 2 , the porosity is 0.12 ± 0.02%, the flatness is 0.01 mm / m, the roundness is 0.010 ± 0.006, and the concentricity is 0.03.

[0080] Example 2

[0081] When the present invention uses a pulse air hammer to move at a certain height on the surface of the porous plate green body in Step 2, the performance of the prepared porous plate is tested with different pressures, and the experimental data are as follows, shown in Table 2.

[0082] Table 2 Comparison of the performance of porous plates using different air hammer parameters

[0083]

[0084] As can be seen from Table 2, by using a relatively high air pressure, such as 0.8 MPa, and blowing and cleaning at an appropriate distance, the roundness and concentricity of the round holes in the perforated plate can be effectively improved, and the number of times of blowing and cleaning required is less. When using a relatively low air pressure, such as 0.5 MPa for cleaning, multiple times of blowing and cleaning are required to obtain an ideal effect, which will significantly reduce the production efficiency.

[0085] Example 3

[0086] In the present invention, a carburizing treatment for the degreased green body and a silicon infiltration treatment for the carburized green body are adopted. Different from the control group, specifically, the control group is a perforated plate prepared without carburizing and silicon infiltration treatment. The perforated plate prepared by the carburizing and silicon infiltration treatment process in the present invention is used as the experimental group. Then, multiple performance parameters of the experimental group and the control group are measured. The specific data are shown in Table 3.

[0087] Table 3 Comparison of the Performance of Perforated Plates with Different Parameters

[0088]

[0089] As can be obtained from Table 3, it can be concluded that after the carburizing and silicon infiltration process treatment in the present invention, compared with the perforated plate obtained by the control group without the carburizing and silicon infiltration process treatment, the density has increased a lot and remains at 3.1 ± 0.15 g / cm 3 or so; the hardness has increased to 2198 ± 100 kg / mm 2 ; the porosity has decreased, and the present invention can reach 0.13%; the flexural strength has increased, and the present invention can reach 300 MPa, and the flatness has decreased. The present invention can reach 0.01 mm / m.

[0090] The above embodiments only represent several implementation manners of the present invention. The description is relatively specific and detailed, but it should not be construed as a limitation on the scope of the invention patent. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can still be made, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the present invention patent should be subject to the appended claims.

Claims

1. A preparation process method of a porous plate with a matrix hole structure based on 3D printing technology, characterized in that: The specific steps are as follows: (1) Preparation work: (1.1) Preparation of raw material powder: Add silicon carbide powder into a mixer, add water and dispersant, then perform centrifugal ball milling, followed by drying, dispersing, and grading and screening to obtain the raw material powder for the required 3D printing powder. The powder diameter is 20 - 200 μm. (1.2) Preparation of printing powder: Mix the above raw material powder with a curing agent to obtain the printing powder. (2) 3D printing process: (2.1) Import the part design drawing into the 3D printer and perform slicing. The number of slices is: N is the number of slices, K is a constant, Z is the height of the part in the printing direction, and d is the layer height; (2.2) Preparation of green body: Add the printing powder into the storage tank of the 3D printer, and perform binder jet printing to the number of sliced layers by using the cyclic steps of "powder spreading - compaction - binder spraying", thus completing the preparation of the green body. The powder spreading thickness of the binder jet printing is 20 - 600 μm / layer. (2.3) Removal of loose sand: Take out the printed green body from the 3D printer and use compressed air blowing to remove the loose sand. The blowing pressure is 0.1 - 0.5 MPa, and the blowing distance is 20 - 50 cm. (3) Cleaning of holes: Use a pulse air hammer to move on the surface of the porous plate green body in step (2) at a distance of 1 - 10 mm, and perform blowing to remove sand for each hole through the process of "pressurization - pulse blowing". The pulse air hammer has a piston of a pneumatic hammer device, and realizes the pressurization and blowing processes by reciprocating motion to achieve the purpose of cleaning the holes. The working pressure of the pulse air hammer is 0.6 - 2 MPa, and the distance from the surface of the porous plate is 1 - 10 mm. (4) High-temperature debinding: Subject the green body after removing loose sand in step (3) to high-temperature debinding. The debinding temperature is 800 - 1300 °C, and the debinding time is 1 - 8 h. (5) Carburizing treatment: (5.1) Mix carbon black, dispersant, solvent, emulsifier, and additive to prepare a carbon black solution. The mass percentages of each component in the carbon black solution in step (5.1) are: carbon black 20 - 60%, dispersant 1 - 5%, emulsifier 1 - 5%, additive 0.1 - 3%, and the balance is solvent. The emulsifier is one or several of alkylphenol polyoxyethylene ether, polyoxyethylene alkylamine, polyoxyethylene alkylolamide, glycerol caprylate, glycerol cocoate, stearic acid acyl ether, or glycerol caprate; the additive is polycarbosilane or polycarbosiloxane. (5.2) Place the debound green body in step (4) in a vacuum impregnation tank and evacuate to a vacuum degree of 0.5 - 1.5 MPa. (5.3) Introduce the carbon black solution into the impregnation tank in step (5.2) and keep the vacuum degree for impregnation for 0.5 - 5 h. (5.4) Take out the impregnated green body in step (5.3) and dry it at 80 - 200 °C for 1 - 5 h to remove the solvent. (5.5) Repeat steps (5.2) - (5.4) to obtain a carbon-containing green body. (6) Reaction silicon infiltration: Place the carbon-containing green body in step (5) in a sintering furnace and perform sintering silicon infiltration at 1500 - 1800 °C and a vacuum degree of 100 - 1000 Pa. The sintering time is 2 - 10 h to obtain silicon carbide ceramics. The aperture diameter of the matrix holes is 1 - 10 mm.

2. The preparation process method of a porous plate with a matrix hole structure based on 3D printing technology according to claim 1, characterized in that: The porous plate prepared by the process method is a silicon carbide plate. First, a porous plate is prepared by 3D printing technology, and then a pneumatic hammer is used to feed compressed gas to clean the hole structure; the pores are arranged in a matrix distribution; the plate thickness is 1-100 mm, and the length and width of the plate are both 10-350 mm; the pressure of the compressed gas is 0.6-1 MPa, and the distance from the surface of the porous plate is 1-10 mm.

3. The preparation process of a porous plate with a matrix hole structure based on 3D printing technology according to claim 1, characterized in that: The rotational speed of the centrifugal ball milling in step (1.1) is 500-2000 rpm, and the ball milling time is 1-24 h; the drying temperature is 80-150 °C, and the drying time is 1-10 h; the weight percentage of the dispersant in the total material is 0.01-0.5%; the weight percentage of water in the total material is 0.5-8%.

4. The preparation process of a porous plate with a matrix hole structure based on 3D printing technology according to claim 1, characterized in that: In step (6), the ratio of the silicon material in the silicon infiltration during sintering is 1-5% of the binder by mass percentage, 0.1-2% of boron nitride, 0.5-5% of water, and the balance is polysilicon particles.

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