Silicon carbide whisker toughened alumina ceramic arm and method of making same

Abstract

The application discloses a silicon carbide whisker toughened alumina ceramic arm and a preparation method thereof. The preparation method comprises the following steps: mixing alumina powder, silicon carbide whiskers, a dispersing agent and water to obtain a slurry, performing spray granulation and drying to obtain a composite powder, stirring the composite powder, water and a binder to obtain a mud, performing secondary mixing on the mud to obtain a printing mud, performing DIW-3D printing on the printing mud to obtain a ceramic arm wet blank, printing a core with an air channel shape on the wet blank, continuously printing the other half of the ceramic arm to obtain a ceramic arm wet blank, and performing baking, sintering and fine processing to obtain the ceramic arm. The ceramic arm prepared by the application has excellent mechanical properties, anti-static properties, heat conduction properties and corrosion resistance, can be applied to various environments and has a long service life, and the preparation method is simple and low in cost.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of ceramic materials, in particular to a silicon carbide whisker toughened alumina ceramic arm and a preparation method thereof. BACKGROUND

[0002] At present, the trade scale of electronic information industry in the world has reached tens of billions of dollars, becoming the world's first industry, and the semiconductor integrated circuit is the core product of the industry. The alumina ceramic arm is the "laborer" of the wafer in the integrated circuit manufacturing process, and almost participates in the whole process of chip manufacturing. Precise ceramic arms are indispensable in equipment such as lithography machines, CVD, PVD, uniform glue development, cleaning, detection, etc.

[0003] On the one hand, the preparation method of traditional ceramic arms mainly uses numerical control machine tools to finish machining ceramic plates, and then relies on the combination of ceramic plates to form ceramic arms with air channels. Adhesives are usually used to fix the ceramic plates, but the corrosion resistance and high temperature resistance of the adhesives are poor, which leads to a shorter service life of the ceramic arm in harsh environments. In order to improve the service life of the ceramic arm, Chinese patent documents CN115710119B and CN115849880B respectively disclose a method for preparing a ceramic arm using water-based injection molding and hot-pressing molding, which avoids the use of adhesives, so that the ceramic arm can serve in a more harsh environment for a longer time. However, although injection molding can achieve near-net-size forming, ceramic arms are custom-made, and injection molding requires the manufacture of metal molds according to different shapes of ceramic arms, which is relatively high in cost. The hot-pressing molding blank contains low-melting-point organic matter, and the heat generated during the blank processing by CNC numerical control machine tools and wire cutting machines may cause the blank to deform, so a certain amount of allowance is often left. The above two processes still have room for improvement.

[0004] On the other hand, alumina ceramic is an insulator, and in the process of transporting silicon wafers, repeated contact between the ceramic arm and the silicon wafers and the equipment often leads to the generation of static electricity. The electromagnetic field effect caused by static electricity can cause trouble in semiconductor manufacturing and application. The incorporation of a second conductive phase into the alumina matrix can effectively reduce the resistivity of the alumina ceramic, making it an anti-static ceramic material. For example, Chinese patent document CN115448742A discloses an alumina anti-static ceramic doped with CuO, V2O5, Fe2O3, etc. nano-conductive oxides, but the amount of such nano-metal oxides is relatively large, and may to some extent reduce the corrosion resistance of the alumina ceramic. SUMMARY

[0005] The technical problem solved by the present application is to overcome the shortcomings of the prior art and provide a silicon carbide whisker toughened alumina ceramic arm with simple preparation process, low cost, excellent mechanical properties, anti-static properties, corrosion resistance, adaptability to various environments and long service life and a preparation method thereof.

[0006] To solve the above technical problems, the present application adopts the following technical solutions.

[0007] A preparation method of a silicon carbide whisker toughened alumina ceramic arm, comprising the following steps:

[0008] (1) Alumina powder, silicon carbide whiskers, dispersants and water are weighed and mixed and ball milled to obtain a slurry; wherein the sum of the mass of the alumina powder and the silicon carbide whiskers is 100%, the mass fraction of the alumina powder is 85%-97%, and the mass fraction of the silicon carbide whiskers is 3%-15%;

[0009] (2) The slurry obtained in step (1) is spray granulated and dried to obtain an alumina / silicon carbide whisker composite powder;

[0010] (3) The alumina / silicon carbide whisker composite powder obtained in step (2), water and a binder are weighed and kneaded and stirred to obtain a body; wherein the sum of the mass of the alumina / silicon carbide whisker composite powder, water and the binder is 100%, the mass fraction of the alumina / silicon carbide whisker composite powder is 58%-80%, the mass fraction of the water is 18%-40%, and the mass fraction of the binder is 2%-5%;

[0011] (4) The body obtained in step (3) is subjected to secondary mixing to remove internal bubbles, and after aging, a printing body is obtained;

[0012] (5) The printing body obtained in step (4) is used for DIW-3D printing, the printing model is a half arm model, and a half ceramic arm wet blank is obtained;

[0013] (6) Polyethylene glycol is used for DIW-3D printing, the printing model is an airway model, and a polyethylene glycol core with an airway shape is printed on the above-mentioned half ceramic arm wet blank;

[0014] (7) The printing body is continued to be used for DIW-3D printing, the printing model is another half arm model, the printing of the other half ceramic arm wet blank is completed, and a ceramic arm wet blank is obtained;

[0015] (8) The obtained ceramic arm wet blank is baked to obtain a ceramic arm dry blank;

[0016] (9) sintering the obtained ceramic arm dry body at a temperature of 1600-1800 ℃ in a nitrogen atmosphere to obtain a ceramic blank, and after fine processing, a silicon carbide whisker toughened alumina ceramic arm is obtained.

[0017] Preferably, in step (5), the process conditions of the DIW-3D printing are: nozzle diameter of 0.8-2 mm, printing speed of 10-30 mm / s, layer thickness of 0.2-1 mm, and the printing paths of layers are perpendicular to each other.

[0018] Preferably, in step (6), the polyethylene glycol is polyethylene glycol 600 and / or polyethylene glycol 800, and the process conditions of the DIW-3D printing are: nozzle diameter of 0.2-0.5 mm, printing speed of 10-30 mm / s, layer thickness of 0.1-0.2 mm, and the printing paths of layers are perpendicular to each other.

[0019] Preferably, in step (5), the printing paste is first loaded into a first barrel, connected to a 3D printer, the power is started, the arm half model is introduced, and then DIW-3D printing is performed; in step (6), the polyethylene glycol is first melted and loaded into a second barrel, the melting temperature is 30-70 ℃, after cooling and solidification, it is connected to the 3D printer, the power is started, the airway model is introduced, and then DIW-3D printing is performed.

[0020] Preferably, in step (1), the ball milling medium is zirconium oxide ball, the mass ratio of alumina powder and silicon carbide whisker: water: zirconium oxide ball is 1:0.6-1:2-4, the ball milling time is 12-48 h, the diameter of the silicon carbide whisker is 30-100 nm, and the length is 10-30 μm; the dispersant is one of ammonium polyacrylate, ammonium citrate and tetramethylammonium hydroxide, and the mass of the dispersant is 0.3-1% of the sum of the mass of the alumina powder and the silicon carbide whisker.

[0021] Preferably, in step (2), when the spray granulation is performed, the inlet temperature of the spray tower is 150-300 ℃, and the outlet temperature is 90-150 ℃.

[0022] Preferably, in step (3), the binder is one or more of hydroxyethyl cellulose, methyl cellulose, ethyl cellulose and polyvinyl alcohol.

[0023] Preferably, in step (8), the baking system is: baking at 20 DEG C for 12-48 hours, baking at 40 DEG C for 6-24 hours, baking at 80 DEG C for 6-24 hours, and baking at 120 DEG C for 4-12 hours.

[0024] Preferably, in step (9), the sintering mode is normal pressure sintering or gas pressure sintering, and the gas pressure of the gas pressure sintering is 2-4 MPa.

[0025] As a general technical concept, the present application also provides a ceramic arm toughened by silicon carbide whiskers prepared by the above preparation method.

[0026] In the present application, the air channel is in the shape of Y, U or I, but is not limited thereto, and is generally flat and has a uniform thickness, usually 0.5-2.5 mm.

[0027] Compared with the prior art, the present application has the following advantages:

[0028] In the present application, silicon carbide whiskers are introduced into the alumina ceramic matrix, sintering is performed in a nitrogen atmosphere, nitrogen atoms are doped into the silicon carbide whiskers to improve the electrical conductivity of the silicon carbide whiskers, and the extrusion process of DIW-3D printing is used to promote the directional arrangement of the silicon carbide whiskers (the degree of directional arrangement is related to the size of the nozzle, and the smaller the nozzle, the more obvious the directional arrangement), and the layers are interlaced with each other (for example, the first layer is printed in the horizontal direction, and the second layer is printed in the vertical direction, forming an interlaced structure), which significantly enhances the bending strength and fracture toughness in the horizontal direction, and the directional arrangement of the silicon carbide whiskers also helps to reduce the resistivity and improve the thermal conductivity, and the anti-static effect can be achieved at a low addition amount.

[0029] In the present application, the ceramic arm is prepared by using the DIW (ink direct writing printing)-3D printing process, which has the advantages of simple process, high production efficiency, small machining allowance, low processing cost, and can realize the rapid preparation of an integrally formed arm, and has high air tightness and long service life.

[0030] In the present application, polyethylene glycol (PEG600, PEG800) is used as the second printing material, which has excellent printing performance, and can print the air channel core in the wet blank, which can avoid the stripe defects on the upper edge of the air channel of the ceramic arm wet blank prepared by using clay DIW-3D printing alone, promote the flatness of the inner upper surface of the air channel, and avoid air leakage; in addition, PEG can absorb water and gradually dissolve in the wet blank, and will not generate tension on the air channel during the drying and shrinkage of the wet blank, so as to avoid cracking of the air channel and ensure the integrity of the air channel. DETAILED DESCRIPTION

[0031] The application will be further described in conjunction with specific preferred embodiments, but the protection scope of the application is not limited thereby. The materials and instruments used in the following examples are commercially available. In the present example, the 3D printer can use the Syno-Source-2638 ceramic 3D printer of Hunan Yuanchuang Gaokeli Industrial Technology Co., Ltd., but is not limited thereto. The diameter of the silicon carbide whisker is 50 nm, and the length is 20 μm, but is not limited thereto.

[0032] Example 1

[0033] A method for preparing a silicon carbide whisker toughened alumina ceramic arm of the application comprises the following steps:

[0034] (1) 2800 g of alumina powder, 200 g of silicon carbide whisker, 10 g of ammonium polyacrylate, 5 g of tetramethylammonium hydroxide, 2400 g of deionized water, and 9000 g of zirconia balls are weighed into a ball mill jar for ball milling, and the ball milling time is 12 h to obtain a slurry.

[0035] (2) The slurry obtained in step (1) is spray granulated and dried to obtain a uniformly mixed alumina / silicon carbide whisker composite powder, wherein the inlet temperature of the spray tower is 230°C, and the outlet temperature is 110°C.

[0036] (3) 2500 g of alumina / silicon carbide whisker composite powder, 750 g of deionized water, 50 g of methyl cellulose, and 28 g of hydroxyethyl cellulose are weighed into a kneader for kneading and stirring to obtain a paste, and the stirring time is 2 h.

[0037] (4) The paste obtained in step (3) is subjected to secondary mixing using a vacuum paste mill to remove internal bubbles, and then aged for 12 h to obtain a printing paste.

[0038] (5) The printing paste obtained in step (4) is loaded into a first barrel and connected to the printer, the power is turned on, half of the arm model is introduced, the printing parameters are set for DIW-3D printing, and the printing is stopped when the airway layer is printed, to obtain a half ceramic arm wet blank; wherein the nozzle diameter is 1.5 mm, the printing speed is 20 mm / s, the layer thickness is 0.6 mm, the airway thickness is 0.6 mm, and the printing paths between layers are perpendicular to each other.

[0039] (6) Polyethylene glycol 800 is melted and loaded into a second barrel, the melting temperature is 60°C, and after cooling and solidification, it is connected to the 3D printer, the airway model is introduced, and DIW-3D printing is performed to print the polyethylene glycol with airway shape on the half ceramic arm wet blank, wherein the nozzle diameter is 0.4 mm, the printing speed is 10 mm / s, and the layer thickness is 0.2 mm.

[0040] (7) After the polyethylene glycol is printed, the first barrel containing the clay is connected to the 3D printer again, and the other half of the arm model is introduced for continuous printing, the printing of the ceramic arm is completed, and a ceramic arm wet blank is obtained.

[0041] (8) The ceramic arm wet blank is transferred to an oven for baking, and the baking system is: 20℃ x 24h + 40℃ x 12h + 80℃ x 8h + 120℃ x 4h, and a ceramic arm dry blank is obtained.

[0042] (9) The ceramic arm dry blank is placed in a sintering furnace for sintering, and a ceramic blank is obtained, the sintering mode is normal pressure sintering, the sintering atmosphere is nitrogen atmosphere, and the sintering temperature is 1650℃.

[0043] (10) The ceramic blank is finely processed using a precision machining center, and a silicon carbide whisker toughened alumina ceramic arm is obtained. The length, width and thickness of the ceramic arm are 400mm x 200mm x 2mm.

[0044] Example 2

[0045] A preparation method of a silicon carbide whisker toughened alumina ceramic arm according to the present application, comprising the following steps:

[0046] (1) 2700g of alumina powder, 300g of silicon carbide whisker, 8g of ammonium polyacrylate, 7g of tetramethylammonium hydroxide, 2400g of deionized water and 9000g of zirconia ball are weighed and placed in a ball mill pot for ball milling, and the ball milling time is 12h, to obtain a slurry.

[0047] (2) The slurry obtained in step (1) is spray granulated and dried to obtain a uniformly mixed alumina / silicon carbide whisker composite powder, wherein the inlet temperature of the spray tower is 230℃, and the outlet temperature is 110℃.

[0048] (3) 2500g of alumina / silicon carbide whisker composite powder, 800g of deionized water, 50g of methyl cellulose, 20g of hydroxyethyl cellulose and 10g of polyvinyl alcohol (PVA) are weighed and placed in a kneader for stirring, to obtain a clay, and the stirring time is 2h.

[0049] (4) The clay obtained in step (3) is subjected to secondary mixing using a vacuum clay mill to remove internal bubbles, and then aged for 12h, to obtain a printing clay.

[0050] (5) Put the printing mud obtained in step (4) into the first barrel and connect it to the 3D printer, start the power supply, import half of the arm model, set the printing parameters for DIW-3D printing, stop printing when the airway layer is printed, and obtain a half ceramic arm wet blank; wherein the nozzle diameter is 1.2 mm, the printing speed is 20 mm / s, the layer thickness is 0.4 mm, the airway thickness is 1.2 mm, and the printing paths between layers are perpendicular to each other.

[0051] (6) Put the melted polyethylene glycol 800 into the second barrel, the melting temperature is 60℃, and after cooling and solidification, connect it to the printer, import the airway model, and perform DIW-3D printing to print the polyethylene glycol with airway shape on the half ceramic arm wet blank, wherein the nozzle diameter is 0.4 mm, the printing speed is 10 mm / s, and the layer thickness is 0.2 mm.

[0052] (7) After the polyethylene glycol is printed, the first barrel containing the mud is connected to the printer again, the other half of the arm model is imported for continuous printing, the printing of the ceramic arm is completed, and a ceramic arm wet blank is obtained.

[0053] (8) Transfer the ceramic arm wet blank to the oven for baking, the baking schedule is 20℃×24h+40℃×16h+80℃×12h+120℃×6h, and a ceramic arm dry blank is obtained.

[0054] (9) Place the ceramic arm dry blank in a sintering furnace for sintering to obtain a ceramic blank, the sintering method is normal pressure sintering, the sintering atmosphere is nitrogen atmosphere, and the sintering temperature is 1680℃.

[0055] (10) Use a precision machining center to finely process the ceramic blank to obtain a silicon carbide whisker toughened alumina ceramic arm. The length, width and thickness of the ceramic arm are 400mm×200mm×3mm.

[0056] Example 3

[0057] A method for preparing a silicon carbide whisker toughened alumina ceramic arm according to the present application, comprising the following steps:

[0058] (1) Put 2800g of alumina powder, 200g of silicon carbide whisker, 10g of ammonium polyacrylate, 5g of tetramethylammonium hydroxide, 2400g of deionized water, and 9000g of zirconia balls into a ball mill jar for ball milling, the ball milling time is 12h, and a slurry is obtained.

[0059] (2) After the slurry obtained in step (1) is spray granulated and dried, a uniformly mixed alumina / silicon carbide whisker composite powder is obtained, wherein the inlet temperature of the spray tower is 230℃ and the outlet temperature is 110℃.

[0060] (3) Take 2500g of alumina / silicon carbide whisker composite powder, 750 deionized water, 50g of methyl cellulose, 28g of hydroxyethyl cellulose into a kneader for stirring to obtain a paste, and the stirring time is 2h.

[0061] (4) The paste obtained in step (3) is subjected to secondary mixing using a vacuum paste mill to remove internal bubbles, and then aged for 12h to obtain a printing paste.

[0062] (5) The printing paste obtained in step (4) is loaded into a first cartridge and connected to a 3D printer, the power is started, half of the arm model is introduced, the printing parameters are set, and printing is stopped when the airway layer is printed, and a half ceramic arm wet blank is obtained; wherein the nozzle diameter is 1.5mm, the printing speed is 20mm / s, the layer thickness is 0.6mm, the airway thickness is 1.2mm, and the printing paths between layers are perpendicular to each other.

[0063] (6) Polyethylene glycol 600 and polyethylene glycol 800 are mixed at a mass ratio of 1:1 and melted into a second cartridge, the melting temperature is 60℃, and after cooling and solidification, it is connected to the 3D printer, the airway model is introduced, and DIW-3D printing is performed, and the polyethylene glycol with the airway shape is printed on the half ceramic arm wet blank, wherein the nozzle diameter is 0.4mm, the printing speed is 10mm / s, and the layer thickness is 0.2mm.

[0064] (7) After the polyethylene glycol is printed, the cartridge containing the paste is connected to the 3D printer again, the other half of the arm model is introduced for continuous printing, and the printing of the ceramic arm is completed to obtain a ceramic arm wet blank.

[0065] (8) The ceramic arm wet blank is transferred to an oven for baking, and the baking schedule is 20℃×24h+40℃×16h+80℃×12h+120℃×6h to obtain a ceramic arm dry blank.

[0066] (9) The ceramic arm dry blank is placed in a sintering furnace for sintering to obtain a ceramic blank, and the sintering mode is gas pressure sintering, the sintering atmosphere is nitrogen atmosphere, the sintering temperature is 1600℃, and the pressure is 2MPa.

[0067] (10) A precision machining center is used to finely process the ceramic blank to obtain a silicon carbide whisker toughened alumina ceramic arm.

[0068] Example 4

[0069] A method for preparing a silicon carbide whisker toughened alumina ceramic arm according to the present application, comprising the following steps:

[0070] (1) Put 2700 g of alumina powder, 300 g of silicon carbide whisker, 8 g of ammonium polyacrylate, 7 g of tetramethylammonium hydroxide, 2400 g of deionized water, and 9000 g of zirconia balls into a ball mill tank for ball milling, and the ball milling time is 12 h to obtain a slurry.

[0071] (2) The slurry obtained in step (1) is spray granulated and dried to obtain a uniformly mixed alumina / silicon carbide whisker composite powder, wherein the inlet temperature of the spray tower is 230°C, and the outlet temperature is 110°C.

[0072] (3) Put 2500 g of alumina / silicon carbide whisker composite powder, 800 deionized water, 50 g of methyl cellulose, 20 g of hydroxyethyl cellulose, and 10 g of PVA into a kneader for stirring to obtain a paste, and the stirring time is 2 h.

[0073] (4) The paste obtained in step (3) is subjected to secondary mixing using a vacuum paste mill to remove internal bubbles, and then aged for 12 h to obtain a printing paste.

[0074] (5) The printing paste obtained in step (4) is loaded into a first barrel and connected to a 3D printer, the power is turned on, half of the arm model is introduced, the printing parameters are set for DIW-3D printing, and the printing is stopped when the airway layer is printed, to obtain a half ceramic arm wet blank; wherein the nozzle diameter is 1.2 mm, the printing speed is 20 mm / s, the layer thickness is 0.4 mm, the airway thickness is 0.8 mm, and the printing paths between layers are perpendicular to each other.

[0075] (6) Polyethylene glycol 600 is melted and loaded into a second barrel, the melting temperature is 60°C, and after cooling and solidification, it is connected to the 3D printer, the airway model is introduced, and DIW-3D printing is performed to print polyethylene glycol with an airway shape on the half ceramic arm wet blank, wherein the nozzle diameter is 0.4 mm, the printing speed is 15 mm / s, and the layer thickness is 0.2 mm.

[0076] (7) After the polyethylene glycol printing is completed, the barrel containing the paste is connected to the 3D printer again, the other half of the arm model is introduced for continuous printing, and the printing of the ceramic arm is completed to obtain a ceramic arm wet blank.

[0077] (8) The ceramic arm wet blank is transferred to an oven for baking, and the baking schedule is 20°C x 24 h + 40°C x 14 h + 80°C x 10 h + 120°C x 5 h to obtain a ceramic arm dry blank.

[0078] (9) The ceramic arm dry blank is placed in a sintering furnace for sintering to obtain a ceramic blank, and the sintering method is gas pressure sintering, the sintering atmosphere is nitrogen atmosphere, the gas pressure is 2 MPa, and the sintering temperature is 1600°C.

[0079] (10) using a precision machining center to finely process the ceramic blank, to obtain a silicon carbide whisker toughened alumina ceramic arm.

[0080] Comparative Example 1

[0081] A preparation method of an alumina ceramic arm, comprising the following steps:

[0082] (1) 3000 g of alumina powder, 6 g of magnesium oxide, 800 g of deionized water, 50 g of methyl cellulose, 20 g of hydroxyethyl cellulose, and 10 g of PVA were placed in a kneader for stirring to obtain a paste, and the stirring time was 2 h.

[0083] (2) The paste obtained in step (1) was subjected to secondary mixing using a vacuum paste mill to remove internal bubbles, and then was aged for 12 h to obtain a printing paste.

[0084] (3) The printing paste obtained in step (2) was loaded into a first cartridge and connected to a printer, the power was started, half of the arm model was introduced, and the printing parameters were set for printing, and the printing was stopped when the airway layer was printed, wherein the nozzle diameter was 1.2 mm, the printing speed was 20 mm / s, the layer thickness was 0.4 mm, the airway thickness was 0.8 mm, and the printing paths between layers were perpendicular to each other.

[0085] (4) Polyethylene glycol 600 was melted and loaded into a second cartridge, the melting temperature was 60℃, and after cooling and solidification, it was connected to the printer, the airway model was introduced, and DIW printing was performed to print the polyethylene glycol with an airway shape on the half ceramic arm wet blank, wherein the nozzle diameter was 0.4 mm, the printing speed was 10 mm / s, and the layer thickness was 0.2 mm.

[0086] (5) After the polyethylene glycol was printed, the first cartridge loaded with the paste was connected to the 3D printer again, the other half of the arm model was introduced for continuous printing, and the printing of the ceramic arm was completed to obtain a ceramic arm wet blank.

[0087] (6) The ceramic arm wet blank was transferred to an oven for baking, the baking schedule was 20℃×24h+40℃×14h+80℃×10h+120℃×5h, and a ceramic arm dry blank was obtained.

[0088] (7) The ceramic arm dry blank was placed in a sintering furnace for sintering to obtain a ceramic blank, the sintering method was normal pressure sintering, the sintering atmosphere was air atmosphere, and the sintering temperature was 1580℃.

[0089] (8) using a precision machining center to finely process the ceramic blank, to obtain a silicon carbide whisker toughened alumina ceramic arm.

[0090] Comparative Example 2

[0091] A preparation method of an alumina ceramic arm, comprising the following steps:

[0092] (1) Put 2800 g of alumina powder, 200 g of silicon carbide whisker, 10 g of ammonium polyacrylate, 5 g of tetramethylammonium hydroxide, 2400 g of deionized water, and 9000 g of zirconia ball into a ball mill tank for ball milling, and the ball milling time is 12 h.

[0093] (2) After the slurry obtained in step (1) is spray granulated and dried, a uniformly mixed alumina / silicon carbide whisker composite powder is obtained, wherein the inlet temperature of the spray tower is 230°C, and the outlet temperature is 110°C.

[0094] (3) Put 2500 g of alumina / silicon carbide whisker composite powder, 750 g of deionized water, 50 g of methyl cellulose, and 28 g of hydroxyethyl cellulose into a kneader for stirring to obtain a paste, and the stirring time is 2 h.

[0095] (4) The paste obtained in step (3) is subjected to secondary mixing using a vacuum paste mill to remove internal bubbles, and then aged for 12 h to obtain a printing paste.

[0096] (5) The printing paste obtained in step (4) is loaded into a first cartridge and connected to a printer, the power is turned on, half of the arm model is introduced, and the printing parameters are set for printing, and the printing is stopped when the airway layer is printed, wherein the nozzle diameter is 1.5 mm, the printing speed is 20 mm / s, the layer thickness is 0.6 mm, the airway thickness is 0.6 mm, and all layer printing paths are in the X-axis direction.

[0097] (6) Polyethylene glycol 800 is melted and loaded into a second cartridge, the melting temperature is 60°C, and after cooling and solidification, it is connected to the printer, the airway model is introduced, and DIW printing is performed to print polyethylene glycol with an airway shape on the half ceramic arm wet blank, wherein the nozzle diameter is 0.4 mm, the printing speed is 10 mm / s, and the layer thickness is 0.2 mm.

[0098] (7) After the polyethylene glycol printing is completed, the cartridge loaded with the paste is connected to the printer again, the other half of the arm model is introduced for continuous printing, and the printing of the ceramic arm is completed to obtain a ceramic arm wet blank.

[0099] (8) The ceramic arm wet blank is transferred to an oven for baking, and the baking schedule is 20°C x 24 h + 40°C x 12 h + 80°C x 8 h + 120°C x 4 h to obtain a ceramic arm dry blank.

[0100] (9) The ceramic arm dry blank is placed in a sintering furnace for sintering to obtain a ceramic roughcast, and the sintering method is normal pressure sintering, the sintering atmosphere is nitrogen atmosphere, and the sintering temperature is 1650°C.

[0101] (10) The ceramic roughcast is finely processed using a precision machining center to obtain a ceramic arm.

[0102] Comparative Example 3

[0103] A method for preparing an alumina ceramic arm, comprising the following steps:

[0104] (1) 2800 g of alumina powder, 200 g of silicon carbide whisker, 10 g of ammonium polyacrylate, 5 g of tetramethylammonium hydroxide, 2400 g of deionized water, 15 g of PVA and 9000 g of zirconia balls were weighed into a ball mill jar for ball milling, and the ball milling time was 12 h.

[0105] (2) The slurry obtained in step (1) was spray granulated and dried to obtain uniformly mixed alumina / silicon carbide.

[0106] (3) The ceramic green body obtained in step (2) was placed in a sintering furnace for sintering to obtain a ceramic plate, the sintering method was normal pressure sintering, the sintering atmosphere was nitrogen atmosphere, and the sintering temperature was 1650°C.

[0107] Table 1 Properties of silicon carbide whisker toughened alumina ceramic arm of Examples 1-5 and Comparative Examples 1-3

[0108]

[0109] Table 1 is a performance comparison table of the silicon carbide whisker toughened alumina ceramic arm of Examples 1-4 and Comparative Examples 1-3. As can be seen from the comparison of Examples 1-4 and Comparative Examples 1-3, the bending strength and fracture toughness gradually increase and the surface resistivity decreases with the increase of the content of silicon carbide whiskers, indicating that the introduction of silicon carbide whiskers has the expected effect. Comparing Examples 1-2 and Examples 3-4 shows that gas pressure sintering is relatively more conducive to promoting the sintering densification of the ceramic, thereby promoting the improvement of various properties. Comparing Examples 1-4 and Comparative Example 2 shows that making the printing paths of the layers perpendicular to each other can effectively avoid the anisotropy of the mechanical properties in the horizontal plane and promote further improvement of the mechanical properties. Comparing Example 1 and Comparative Example 3 shows that, at the same content of silicon carbide whiskers, the material prepared by the method of the present application has higher bending strength and fracture toughness and lower surface resistivity than the material prepared by isostatic pressing. Since the whiskers of the present application can be oriented, while the dry pressing and isostatic pressing can be randomly distributed, the ceramic arm of the present application has better performance in the horizontal direction. This is also the demand of the prior art for ceramic arms, and the performance in the Z direction is not required. The DIW-3D printing process is a layer-by-layer manufacturing process, which can promote the directional arrangement of silicon carbide whiskers in the horizontal direction, and the layers are interlaced, making it difficult for cracks to propagate perpendicular to the horizontal direction, thereby increasing the fracture toughness. Similarly, the directional arrangement of silicon carbide whiskers in each layer increases the probability of contact between them in the horizontal direction, thereby reducing the resistivity. In summary, the silicon carbide whisker toughened alumina ceramic arm provided by the present application has higher bending strength, fracture toughness and lower resistivity, and has a wide application prospect in the semiconductor industry.

[0110] The above is only a preferred embodiment of the present application, and does not limit the present application in any form. Although the present application has been disclosed as above with reference to the preferred embodiment, it is not intended to limit the present application. Any person skilled in the art can make many possible changes and modifications to the technical solutions of the present application, or modify equivalent embodiments, without departing from the spirit and technical solutions of the present application, using the disclosed methods and technical contents. Therefore, any simple modification, equivalent replacement, equivalent change and modification of the above embodiments made in accordance with the technical essence of the present application, without departing from the technical solutions of the present application, are still within the scope of protection of the present application.

Claims

1. A method for preparing a silicon carbide whisker-toughened alumina ceramic arm, characterized in that, Includes the following steps: (1) Weigh alumina powder, silicon carbide whiskers, dispersant and water, mix and ball mill to obtain a slurry; wherein the sum of the mass of the alumina powder and the silicon carbide whiskers is 100%, the mass fraction of the alumina powder is 85% to 97%, and the mass fraction of the silicon carbide whiskers is 3% to 15%; (2) Spray granulation and drying of the slurry obtained in step (1) to obtain alumina / silicon carbide whisker composite powder; (3) Weigh the alumina / silicon carbide whisker composite powder, water and binder obtained in step (2), knead and stir to obtain mud; wherein, the sum of the mass of alumina / silicon carbide whisker composite powder, water and binder is 100%, the mass fraction of the alumina / silicon carbide whisker composite powder is 58% to 80%, the mass fraction of the water is 18% to 40%, and the mass fraction of the binder is 2% to 5%; (4) The clay obtained in step (3) is kneaded a second time to remove internal air bubbles, and then aged to obtain printing clay. (5) Use the printing clay obtained in step (4) for DIW-3D printing. The printing paths between layers are perpendicular to each other. The printing model is a half-arm model, and a half-ceramic arm wet blank is obtained. (6) Polyethylene glycol is used for DIW-3D printing. The printing model is a gas channel model. A polyethylene glycol core with a gas channel shape is printed on the above half of the ceramic arm wet blank. (7) Continue to use the printing clay to perform DIW-3D printing. The printing model is the other half of the arm model. Complete the printing of the other half of the ceramic arm wet blank to obtain the ceramic arm wet blank. (8) The obtained wet ceramic arm blank is baked to obtain a dry ceramic arm blank; (9) The obtained ceramic arm blank is sintered at a temperature of 1600℃~1800℃ in a nitrogen atmosphere to obtain a ceramic blank. After fine processing, a silicon carbide whisker toughened alumina ceramic arm is obtained.

2. The method for preparing the silicon carbide whisker-toughened alumina ceramic arm according to claim 1, characterized in that, In step (5), the process conditions for DIW-3D printing are: nozzle diameter of 0.8mm to 2mm, printing speed of 10mm / s to 30mm / s, and layer thickness of 0.2mm to 1mm.

3. The method for preparing a silicon carbide whisker-toughened alumina ceramic arm according to claim 1, characterized in that, In step (6), the polyethylene glycol is polyethylene glycol 600 and / or polyethylene glycol 800, and the process conditions for DIW-3D printing are: nozzle diameter of 0.2mm to 0.5mm, printing speed of 10mm / s to 30mm / s, layer thickness of 0.1mm to 0.2mm, and printing paths between layers are perpendicular to each other.

4. The method for preparing the silicon carbide whisker-toughened alumina ceramic arm according to any one of claims 1 to 3, characterized in that, In step (5), the printing clay is first loaded into the first material cylinder, connected to the 3D printer, the power is turned on, the arm half model is imported, and then DIW 3D printing is performed; in step (6), the polyethylene glycol is first melted and loaded into the second material cylinder at a melting temperature of 30℃~70℃, cooled and solidified, then connected to the 3D printer, the power is turned on, the air channel model is imported, and then DIW-3D printing is performed.

5. The method for preparing the silicon carbide whisker-toughened alumina ceramic arm according to any one of claims 1 to 3, characterized in that, In step (1), the milling medium is zirconia balls, and the mass ratio of alumina powder to silicon carbide whiskers to water to zirconia balls is 1:0.6 to 1:2 to 4. The milling time is 12 to 48 hours. The diameter of the silicon carbide whiskers is 30 nm to 100 nm, and the length is 10 μm to 30 μm. The dispersant is one of ammonium polyacrylate, ammonium citrate, and tetramethylammonium hydroxide, and the mass of the dispersant is 0.3% to 1% of the sum of the masses of the alumina powder and the silicon carbide whiskers.

6. The method for preparing the silicon carbide whisker-toughened alumina ceramic arm according to any one of claims 1 to 3, characterized in that, In step (2), during the spray granulation, the inlet temperature of the spray tower is 150℃~300℃ and the outlet temperature is 90℃~150℃.

7. The method for preparing the silicon carbide whisker-toughened alumina ceramic arm according to any one of claims 1 to 3, characterized in that, In step (3), the adhesive is one or more of hydroxyethyl cellulose, methyl cellulose, ethyl cellulose and polyvinyl alcohol.

8. The method for preparing the silicon carbide whisker-toughened alumina ceramic arm according to any one of claims 1 to 3, characterized in that, In step (8), the baking regime is as follows: baking at 20℃ for 12h to 48h, baking at 40℃ for 6h to 24h, baking at 80℃ for 6h to 24h, and baking at 120℃ for 4h to 12h.

9. The method for preparing the silicon carbide whisker-toughened alumina ceramic arm according to any one of claims 1 to 3, characterized in that, In step (9), the sintering method is atmospheric pressure sintering or gas pressure sintering, and the gas pressure of gas pressure sintering is 2MPa to 4MPa.

10. A silicon carbide whisker-toughened alumina ceramic arm prepared by any one of claims 1 to 9.

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