CN116332651A - Reactive sintering silicon carbide ceramic temperature equalizing plate and preparation method thereof - Google Patents
Reactive sintering silicon carbide ceramic temperature equalizing plate and preparation method thereof Download PDFInfo
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- CN116332651A CN116332651A CN202310213515.9A CN202310213515A CN116332651A CN 116332651 A CN116332651 A CN 116332651A CN 202310213515 A CN202310213515 A CN 202310213515A CN 116332651 A CN116332651 A CN 116332651A
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Abstract
The invention belongs to the technical field of ceramic temperature-equalizing plates, and particularly relates to a reaction sintering silicon carbide ceramic temperature-equalizing plate and a preparation method thereof. The preparation method comprises the steps of batching, mixing, granulating, press forming by using press forming equipment, drying, removing carbon, sintering and the like. The pressing forming equipment comprises an upper pressing die and a lower pressing die, a pressing die head is arranged between the upper pressing die and the lower pressing die, a pressing groove is formed in the top surface of the lower pressing die, a vibrating plate is movably arranged at the bottom of the pressing groove, a central stirring disc is horizontally arranged in the vibrating plate in a rotating mode, a plurality of stirring teeth are arranged on the top surface of the central stirring disc, a central follow-up disc is horizontally arranged on the top surface of the vibrating plate in a rotating mode, the uniformity of a compact prepared by the device is improved, and further the bending strength and hardness of the prepared silicon carbide ceramic temperature homogenizing plate are improved.
Description
Technical Field
The invention belongs to the technical field of ceramic temperature-equalizing plates, and particularly relates to a reaction sintering silicon carbide ceramic temperature-equalizing plate and a preparation method thereof.
Background
At present, common 3 materials of a temperature equalization plate are as follows: the three materials are copper material > silicon carbide ceramic material > tungsten steel material, wherein the silicon carbide ceramic material has the best oxidation resistance and hardness, and has the lowest thermal expansion coefficient, accurate size and difficult deformation. Therefore, the silicon carbide ceramic material is the best choice for manufacturing the temperature equalizing plate.
Silicon carbide ceramics not only have excellent normal temperature mechanical properties such as high flexural strength, excellent oxidation resistance, good corrosion resistance, high abrasion resistance and low friction coefficient, but also have excellent high temperature mechanical properties (strength, creep resistance and the like) which are the best of the known ceramic materials, so that the silicon carbide ceramics have wide application in the fields of mechanical sealing, semiconductors, petrochemical industry, military industry and the like. The silicon carbide ceramic temperature equalizing plate is a plate-shaped structure capable of providing a uniform temperature environment and is mainly used for manufacturing glass substrates of LCD liquid crystal panels. In the preparation process of the silicon carbide ceramic temperature-uniforming plate, the silicon carbide ceramic temperature-uniforming plate is required to have indexes such as high enough strength, hardness and wear resistance, so that the silicon carbide ceramic temperature-uniforming plate is usually subjected to powder preparation, briquette pressing, drying, sintering and other steps, and parameters involved in the steps are most, such as reasonable raw materials and powder with a reasonable proportion are required to be prepared in a powder preparation stage, reasonable pressure conditions and briquette size design are required in a briquette pressing stage, temperature setting and treatment time setting in a drying and sintering stage are required, and if the design is unreasonable, indexes such as hardness of a finished product can be influenced.
The briquette pressing process has a great influence on the hardness and strength of the product in each step of preparing the silicon carbide ceramic temperature homogenizing plate, and in this step, the formulated powder is pressed into a briquette by a hydraulic press, and the hardness and strength of the briquette after this step have been basically determined due to the large pressure, typically hundreds of MPa, during the pressing. The hydraulic presses currently used are mostly common devices, such as CN107127999A, CN211567043U and CN113601894a, and mainly consist of an upper pressing die and a lower pressing die, wherein the upper pressing die is driven by the hydraulic press to provide sufficient pressure. Because the powder added into the lower pressing die has a certain particle size when the briquettes are pressed, arch bridge effect can exist among the powder, under the action of the arch bridge effect, holes exist in the powder piled up in the lower pressing die, and the holes cannot be completely eliminated by strong pressure, so that the uniformity of the briquettes formed by pressing is poor, and the hardness of the final silicon carbide ceramic temperature-equalizing plate is directly influenced.
Disclosure of Invention
In order to solve the technical problems, the invention provides a reactive sintering silicon carbide ceramic temperature equalizing plate and a preparation method thereof.
The first object of the invention is to provide a method for preparing a reaction sintering silicon carbide ceramic temperature-uniforming plate, which comprises the following steps:
1) Weighing the raw materials according to the raw material proportion of the reaction sintering silicon carbide ceramic temperature-uniforming plate;
2) Ball milling and mixing;
3) Granulating by spraying;
4) And (5) press forming:
performing compression molding by using compression molding equipment;
5) Drying the biscuit;
6) Oxidizing in air to remove carbon;
7) Sintering at high temperature;
the press forming apparatus includes:
a pressing mold is arranged;
the lower compacting die is arranged below the upper compacting die, a compacting die head is arranged between the upper compacting die and the lower compacting die, a compacting groove is formed in the top surface of the lower compacting die, a vibrating plate is arranged at the bottom of the compacting groove in a vertically movable mode, a central stirring disc is arranged in the vibrating plate in a horizontally rotating mode, a plurality of stirring teeth are arranged on the top surface of the central stirring disc, a central follow-up disc is arranged on the top surface of the vibrating plate in a horizontally rotating mode, the stirring teeth penetrate through the top surface of the vibrating plate and are inserted into through holes in the central follow-up disc, a stirring motor and a vibrating mechanism are arranged in the lower compacting die, the stirring motor is connected with the central stirring disc to drive the central stirring disc to horizontally rotate, and the vibrating mechanism drives the vibrating plate to vibrate in the vertical direction.
Preferably, the vibration mechanism comprises a vibration motor and an eccentric wheel, wherein the eccentric wheel is arranged on a rotating shaft of the vibration motor, and the eccentric wheel is in contact with the bottom of the vibration plate.
Preferably, the inside horizontal rotation of vibrating plate is provided with the edge stirring dish, the edge stirring dish with the meshing of central stirring dish, just also be provided with a plurality of stirring teeth on the top surface of edge stirring dish, the last position horizontal rotation that corresponds with the edge stirring dish of vibrating plate is provided with the edge follower dish, stirring teeth on the edge stirring dish pass the top surface of vibrating plate and insert in the through-hole on the edge follower dish, just stirring teeth can be for the top surface activity of vibrating plate.
Preferably, a vertical driving rod is arranged in the center of the bottom surface of the central stirring disc, and a driving shaft at the top of the stirring motor is vertically inserted into the driving rod in a sliding manner.
Preferably, a pressing head is arranged on the bottom surface of the pressing die head, the position of the pressing head corresponds to the pressing groove, and the shape and the size of the pressing head are matched with the pressing groove.
Preferably, the reaction sintering silicon carbide ceramic temperature equalizing plate is composed of the following raw materials: a base material, a dispersant, a plasticizer and a lubricant;
the base material consists of submicron silicon carbide and a sintering aid, wherein the submicron silicon carbide accounts for 96% of the total weight of the base material, and the sintering aid accounts for 4% of the total weight of the base material;
the dispersant accounts for 0.8% of the total weight of the base material, the plasticizer accounts for 2.5% of the total weight of the base material, and the lubricant accounts for 3% of the total weight of the base material;
the sintering aid consists of aluminum nitride, aluminum oxide and yttrium oxide, and the aluminum nitride, the aluminum oxide and the yttrium oxide account for 1.4 percent, 1.6 percent and 1 percent of the total weight of the base material.
Preferably, the working pressure of the compression molding equipment is 160-200MPa.
Preferably, specific parameters of the oxidative carbon removal in the air are as follows:
and 5) loading the biscuit processed in the step 5) into an oxidation furnace, heating up in the atmospheric environment, heating up to 450 ℃ at a speed of 2 ℃/min, preserving heat for 2 hours, and oxidizing to remove free carbon in the biscuit.
Preferably, the processed biscuit is orderly put into a hot isostatic pressing sintering furnace, a furnace door is closed, a vacuum pump is started to vacuumize, the temperature is raised to 900 ℃ at 5 ℃/min, the vacuum is kept for 0.5h, the vacuum pump is closed, argon is started to be filled until the pressure gauge of the sintering furnace shows 0.01bar, the temperature is raised to 1200 ℃ at 4 ℃/min, and the temperature is kept for 1h; then argon is filled until the pressure gauge shows 5bar, the temperature is increased to 1900 ℃ at 3 ℃/min, and the temperature is kept for 1.5h; then argon is filled until the pressure gauge shows 95bar, the temperature is raised to 1950 ℃ at 1 ℃/min, the temperature is kept for 10min, a heating system is closed, the pressure in the furnace is kept unchanged, the pressure is relieved when the temperature is reduced to 1500 ℃, and then the furnace is cooled to room temperature along with the furnace and opened.
The second object of the invention is to provide a reactive sintering silicon carbide ceramic temperature equalizing plate prepared by the method.
Compared with the prior art, the invention has the following beneficial effects:
the vibrating plate is arranged in the lower pressing die, and the stirring disc inside the vibrating plate is positioned at a certain height position during vibration, so that stirring teeth repeatedly extend into powder in the process of up-down vibration of the vibrating plate to destroy cavities in the powder, the stirred powder is tightly vibrated by the vibrating plate during vibration, and finally the powder is tightly combined under the action of pressure, so that the uniformity of the briquettes is improved, and the strength and hardness of the silicon carbide ceramic temperature equalizing plate are improved.
After the biscuit is pressed by the pressing forming equipment, the prepared biscuit has good particle uniformity and high strength, the time consumed by the subsequent matched drying and calcining steps is shortened, and the bending strength and hardness of the prepared finished product of the temperature-uniforming plate are obviously improved compared with those of the prior art.
Drawings
Fig. 1 is a schematic perspective view of a press forming apparatus according to an embodiment of the present invention;
fig. 2 is a schematic front view of a press forming apparatus according to an embodiment of the present invention;
FIG. 3 is a schematic view showing an agitating state of a lower pressing mold according to an embodiment of the present invention when in operation;
FIG. 4 is a top view of a connection structure between the top surface of a vibrating plate and stirring teeth according to an embodiment of the present invention;
FIG. 5 is a schematic diagram of a vibration state of a lower pressing mold in operation according to an embodiment of the present invention;
fig. 6 is a schematic diagram of a state of the lower pressing mold according to the embodiment of the present invention when the lower pressing mold stops working;
FIG. 7 is a schematic view of the stirring tooth position and direction of rotation.
Detailed Description
In order that those skilled in the art will better understand the technical scheme of the present invention, the present invention will be further described with reference to specific embodiments and drawings.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
Example 1
A method for preparing a reaction sintering silicon carbide ceramic temperature-uniforming plate, which comprises the following steps:
the reaction sintering silicon carbide ceramic temperature equalizing plate is composed of the following raw materials: a base material, a dispersant, a plasticizer and a lubricant;
the base stock consists of submicron silicon carbide (d50=700 nm) and a sintering aid (d50=1.2 μm), the submicron silicon carbide accounting for 96% of the total weight of the base stock, and the sintering aid accounting for 4% of the total weight of the base stock;
the dispersant accounts for 0.8% of the total weight of the base material, the plasticizer accounts for 2.5% of the total weight of the base material, and the lubricant accounts for 3% of the total weight of the base material;
the sintering aid consists of aluminum nitride, aluminum oxide and yttrium oxide, wherein the aluminum nitride, the aluminum oxide and the yttrium oxide account for 1.4 percent, 1.6 percent and 1 percent of the total weight of the base material;
the dispersing agent is tetramethyl ammonium hydroxide;
the plasticizer is PVA water solution with the mass concentration of 10%;
the lubricant consists of polyethylene glycol and glycerin, wherein the polyethylene glycol accounts for 1.5% of the total weight of the base material, and the glycerin accounts for 1% of the total weight of the base material.
The innovation point of the invention is that the preparation method of the silicon carbide ceramic temperature-equalizing plate is changed, so the preparation raw material proportion of the silicon carbide ceramic temperature-equalizing plate is designed according to the prior art, and the corresponding preparation method is changed.
The preparation method of the reaction sintering silicon carbide ceramic temperature equalizing plate comprises the following steps:
1) Weighing the raw materials according to the proportion;
2) Ball milling and mixing:
3) And (3) spray granulation:
for a specific method of operation of ball milling mixing and spray granulation reference is made to the procedure of example 1 of CN108203300 a;
4) And (5) press forming:
the press forming equipment designed by the invention is utilized for press forming;
the press-forming apparatus of the present invention, as shown in fig. 1 to 6, includes:
an upper press mold 100;
the lower pressing die 300 is arranged below the upper pressing die 100, a pressing die head 200 is arranged between the upper pressing die 100 and the lower pressing die 300, a pressing groove 310 is formed in the top surface of the lower pressing die 300, a vibrating plate 311 is vertically and movably arranged at the bottom of the pressing groove 310, a cavity is formed in the vibrating plate 311, a central stirring disc 312 is horizontally arranged at the position of the cavity in the vibrating plate 311 in a rotating mode, a plurality of stirring teeth 314 are arranged on the top surface of the central stirring disc 312, a central follow-up disc 315 is horizontally arranged on the top surface of the vibrating plate 311 in a rotating mode, and the stirring teeth 314 penetrate through the top surface of the vibrating plate 311 and are inserted into through holes formed in the central follow-up disc 315. In this embodiment, the top surface of the vibration plate 311 is a movable plate, and the side wall of the movable plate is rotatably connected to an annular track disposed on the inner side wall of the cavity of the vibration plate 311, and when the stirring teeth 314 rotate, the movable plate is driven to rotate horizontally; or the top surface of the vibration plate 311 is fixed on the side wall of the cavity of the vibration plate 311, the through hole 318 on the top surface of the vibration plate 311 for the stirring teeth 314 to pass through is C-shaped, a plurality of stirring teeth 314 are distributed in a major arc shape, and the stirring motor 330 is a bidirectional rotating motor and reciprocally rotates, referring to fig. 4.
An agitation motor 330 and a vibration mechanism are arranged in the lower pressing mold 300 and below the vibration plate 311, the agitation motor 330 is connected with the central agitation disk 312 to drive the central agitation disk 312 to horizontally rotate, in particular, a through groove is arranged on the bottom surface of the central agitation disk 312, an output shaft of the agitation motor 330 penetrates through the through groove and can rotate in the through groove, an output shaft of the agitation motor 330 penetrates through the through groove and is connected with the bottom center of the central agitation disk 312, and a part of the agitation motor 330 which is not output shaft is embedded and installed in the lower pressing mold 300; the vibration mechanism drives the vibration plate 311 to vibrate in the vertical direction.
Illustratively, the upper and lower pressing molds 100 and 300 are connected by a positioning column 400, and the positioning column 400 may be disposed at a corner of a space between the upper and lower pressing molds 100 and 300, and the positioning column 400 may pass through the pressing mold head 200 to enable the pressing mold head 200 to move up and down between the upper and lower pressing molds 100 and 300. A detachable positioning bolt may be installed between the pressing die head 200 and the positioning column 400, and the positioning bolt penetrates through the pressing die head 200 and then abuts against the outer wall of the positioning column 400, so that the pressing die head 200 is positioned by friction force, and the positioning bolt is removed, so that the pressing die head 200 can move up and down.
In the embodiment of the present application, one end of the hydraulic rod 110 is disposed at the bottom of the upper pressing mold 100, the other end of the hydraulic rod 110 is connected with the top surface of the pressing mold head 200, the pressing head 210 is disposed on the bottom surface of the pressing mold head 200, the position of the pressing head 210 corresponds to the position of the pressing groove 310, and the shape and the area of the pressing head 210 are matched with the pressing groove 310. When the pressing die head 200 is pressed down by the driving of the hydraulic rod 110, the pressing head 210 is inserted into the pressing groove 310 so that the powder in the pressing groove 310 is pressed to form a compact.
During the pressing process, the pressing die head 200 moves downward, the stirring motor 330 and the vibration mechanism continuously work, and the stirring motor 330 drives the central stirring disk 312 to rotate, so that the stirring teeth 314 drive the central follow-up disk 315 to rotate. The through holes in the central follower disk 315 are shaped and sized to match the shape and size of each of the agitator teeth 314 and are positioned in a one-to-one correspondence. When the vibration mechanism drives the vibration plate 311 to vibrate up and down, the vibration plate 311 is always kept at a certain height position under a proper vibration frequency (such as the intermittent existence of driving force), and due to the gravity of the vibration plate 311 and the action of an elastic member (such as a spring connected between the inner bottom surface of the lower pressing mold 300 and the bottom surface of the vibration plate 311), the vibration plate 311 moves down rapidly within a short time after the driving force of the vibration mechanism disappears, the positions of the stirring teeth 314 remain unchanged, the stirring teeth 314 extend from the through holes of the central follower disk 315, and are inserted into the powder above the vibration plate 311, see fig. 3, and when the driving force of the vibration mechanism exists, the vibration plate 311 moves up rapidly, so that the tops of the stirring teeth 314 are flush with the tops of the central follower disk 315, see fig. 5. Because the stirring motor 330 drives the stirring teeth 314 to rotate through the central stirring disk 312, the stirring teeth 314 stir the powder in a large area through repeated insertion and rotation, so that cavities possibly existing in the powder are destroyed, the powder is tightly vibrated under the vibration action of the vibrating plate 311, the stirring teeth 314 can also transmit vibration waves, and the cavities in the powder disappear under the dual actions of vibration and stirring, so that the uniformity of briquettes formed after pressing is greatly improved.
When the compacting die head 200 moves down to a certain height, i.e., is about to come into contact with the powder in the compacting groove 310, the stirring motor 330 and the vibration mechanism stop operating to avoid damages to the compacted compact caused by stirring and vibration. At this time, the vibration plate 311 is on the inner bottom surface of the pressing groove 310, and the central stirring plate 312 also falls down to the inner bottom surface of the vibration plate 311 by gravity so that the stirring teeth 314 are flush with the top surface of the central follower plate 315. The top surface of the central follower disk 315 is now generally planar to provide adequate support for the powder above, see fig. 6.
The working pressure of the compression molding equipment is 200MPa, no pressure is applied during vibration, and the pressure is applied after the vibration mixing is finished.
5) And (5) biscuit baking:
placing the pressed biscuit into a baking oven at 120 ℃ for heat preservation for 4 hours, then heating to 700 ℃ in an inert gas environment at a speed of 2 ℃/min, and then preserving heat at 700 ℃ for 2 hours to remove wax substances in the biscuit; wherein argon is used as the inert gas.
6) Oxidizing and removing carbon in air:
placing the biscuit processed in the step 5) into an oxidation furnace, heating up in the atmospheric environment, heating up to 450 ℃ at a speed of 2 ℃/min, preserving heat for 2 hours, and oxidizing to remove free carbon in the biscuit;
7) High-temperature sintering:
orderly loading the treated biscuit into a hot isostatic pressing sintering furnace, closing a furnace door, opening a vacuum pump to vacuum, heating to 900 ℃ at 5 ℃/min, preserving heat for 0.5h, closing the vacuum pump, starting to charge argon until the pressure gauge of the sintering furnace shows 0.01bar, heating to 1200 ℃ at 4 ℃/min, and preserving heat for 1h; then argon is filled until the pressure gauge shows 5bar, the temperature is increased to 1900 ℃ at 3 ℃/min, and the temperature is kept for 1.5h; then argon is filled until the pressure gauge shows 95bar, the temperature is raised to 1950 ℃ at 1 ℃/min, the temperature is kept for 10min, a heating system is closed, the pressure in the furnace is kept unchanged, the pressure is relieved when the temperature is reduced to 1500 ℃, and then the furnace is cooled to room temperature along with the furnace and opened.
Compared with the embodiment 1 of CN108203300A, the preparation method of the embodiment adopts the special-structure compression molding equipment to perform compression molding to obtain the green body, after the green body is prepared, the subsequent drying time, the oxidation decarbonization time and the calcination time are shortened, the preparation efficiency of the silicon carbide ceramic temperature-equalizing plate is greatly improved, the bending strength of the prepared silicon carbide ceramic temperature-equalizing plate reaches 513MPa, the hardness can reach 2984HV, and the two indexes are obviously improved compared with CN 108203300A.
Example 2
A method of preparing a reaction-sintered silicon carbide ceramic isopipe substantially the same as that of example 1, except that:
in this embodiment, the vibration mechanism includes a vibration motor 320 and an eccentric 321, the eccentric 321 is disposed on a rotation shaft of the vibration motor 320, and the eccentric 321 is in contact with the bottom of the vibration plate 311.
Illustratively, the vibration motor 320 is horizontally disposed inside the lower pressing mold 300, and the eccentric wheel 321 is disposed on the rotation shaft of the vibration motor 320 to contact with the contact block 317 disposed at the bottom of the vibration plate 311, thereby converting the rotation of the eccentric wheel 321 into the up-and-down vibration of the vibration plate 311. The function of the contact block 317 is to drive between the vibration plate 311 and the eccentric wheel 321, which not only can transmit the vibration kinetic energy to the vibration plate 311 through the contact block 317, but also can avoid the eccentric wheel 321 from directly contacting with the vibration plate 311, thereby protecting the service life of the vibration plate 311. Preferably, the contact block 317 is detachably connected to the bottom of the vibration plate 311 by means of bolts, screws or screw connection, etc., so that replacement is facilitated.
In this embodiment, a movable space is provided in the lower pressing mold 300 at a position at the bottom of the pressing groove 310, the contact block 317 and the eccentric wheel 321 are both located in the movable space, and the vibration motor 320 is installed in the movable space.
Compared with the embodiment 1 of CN108203300A, the preparation method of the embodiment adopts the press forming equipment with a special structure, shortens the subsequent drying time, the oxidation decarbonization time and the calcination time after preparing the biscuit, greatly improves the preparation efficiency of the silicon carbide ceramic temperature-uniforming plate, and ensures that the bending strength of the prepared silicon carbide ceramic temperature-uniforming plate reaches 521MPa and the hardness reaches 2988HV.
Example 3
A method of preparing a reaction-sintered silicon carbide ceramic isopipe substantially the same as that of example 1, except that:
in this embodiment, an edge stirring disk 313 is further horizontally rotatably disposed inside the vibration plate 311, the edge stirring disk 313 is meshed with the central stirring disk 312, a plurality of stirring teeth 314 are also disposed on the top surface of the edge stirring disk 313, an edge following disk 316 is horizontally rotatably disposed on the top surface of the vibration plate 311 at a position corresponding to the edge stirring disk 313, and the stirring teeth 314 on the edge stirring disk 313 pass through the top surface of the vibration plate 311 and are inserted into through holes on the edge following disk 316.
Illustratively, the center agitation plate 312 is located at the inner center of the vibration plate 311, and the edge agitation plates 313 are located at the outer periphery of the center agitation plate 312 inside the vibration plate 311, so that the edge agitation plates 313 may be provided in plurality so that the agitation can cover a larger area.
It should be noted that, when the edge stirring plate 313 and the edge following plate 316 are disposed, the top surface of the edge following plate 316 and the top surface of the central following plate 315 are provided with the surrounding blocks, the number and the shape of the pressing heads 210 disposed on the bottom surface of the pressing die head 200 are matched with the number and the shape of the surrounding blocks, and the pressing heads 210 are in one-to-one correspondence with the surrounding block positions, so as to prevent powder leakage in the pressing process.
In this embodiment, the top surface of the vibration plate 311 is fixed on the side wall of the cavity of the vibration plate 311, the through hole 318 on the top surface of the vibration plate 311 for the stirring teeth 314 to pass through is C-shaped, the stirring teeth 314 are distributed in a major arc shape, the stirring motor 330 is a bi-directional rotating motor, and the stirring motor rotates reciprocally, and fig. 7 illustrates the positions and the rotation directions of the stirring teeth 314 corresponding to the top surfaces of the edge follower disk 316 and the central follower disk 315, wherein the direction pointed by the arrow is the rotation direction.
Compared with the embodiment 1 of CN108203300A, the preparation method of the embodiment adopts the press forming equipment with a special structure, shortens the subsequent drying time, the oxidation decarbonization time and the calcination time after preparing the biscuit, greatly improves the preparation efficiency of the silicon carbide ceramic temperature-equalizing plate, and ensures that the bending strength of the prepared silicon carbide ceramic temperature-equalizing plate reaches 523MPa and the hardness reaches 3001HV.
Example 4
A method of preparing a reaction-sintered silicon carbide ceramic isopipe substantially the same as that of example 1, except that:
in this embodiment, a vertical driving rod is provided at the center of the bottom surface of the central stirring plate 312, and a driving shaft at the top of the stirring motor 330 is vertically slidably inserted into the driving rod.
Illustratively, the cross-section of the receptacle inside the drive rod is non-circular, such as rectangular, triangular, oval, etc., and the drive shaft of the agitator motor 330 also needs to be shaped to match the receptacle inside the drive rod so that the agitator motor 330 is free to move up and down as the central agitator disk 312 is driven to rotate.
The bending strength of the silicon carbide ceramic temperature-uniforming plate prepared by the preparation method of the embodiment reaches 525MPa, and the hardness can reach 2998HV.
Comparative example 1
A method of preparing a reaction-sintered silicon carbide ceramic isopipe substantially the same as that of example 1, except that:
the press forming apparatus includes:
an upper press mold 100;
the lower pressing mold 300 is disposed below the upper pressing mold 100, the pressing mold head 200 is disposed between the upper pressing mold 100 and the lower pressing mold 300, and a pressing groove 310 is disposed on the top surface of the lower pressing mold 300. The upper and lower pressing molds 100 and 300 are connected through a positioning column 400, the positioning column 400 may be disposed at a corner of a space between the upper and lower pressing molds 100 and 300, and the positioning column 400 may pass through the pressing mold head 200 to enable the pressing mold head 200 to move up and down between the upper and lower pressing molds 100 and 300. One end of a hydraulic rod 110 is arranged at the bottom of the upper pressing die 100, the other end of the hydraulic rod 110 is connected with the top surface of the pressing die head 200, a pressing head 210 is arranged on the bottom surface of the pressing die head 200, the position of the pressing head 210 corresponds to the position of the pressing groove 310, and the shape and the area of the pressing head 210 are matched with those of the pressing groove 310. When the pressing die head 200 is pressed down by the driving of the hydraulic rod 110, the pressing head 210 is inserted into the pressing groove 310 so that the powder in the pressing groove 310 is pressed to form a compact.
The press molding apparatus of the present embodiment is different from the apparatus of embodiment 1 in that the vibration mechanism, the stirring motor 330, the vibration plate 311, the central stirring plate 312, the stirring teeth 314, and the central follower plate 315 are not provided.
Compared with the preparation method of the embodiment 1 of the invention, the preparation method of the comparative example does not adopt a component capable of improving the grain size uniformity of the biscuit, so that the bending strength of the prepared silicon carbide ceramic temperature-equalizing plate reaches 346MPa, and the hardness is 2031HV.
Example 5
A method for preparing a reaction sintering silicon carbide ceramic temperature-uniforming plate is basically the same as that of the embodiment 1, except that the working pressure of a compression molding device is 160MPa, and the bending strength of the prepared silicon carbide ceramic temperature-uniforming plate reaches 502MPa, and the hardness can reach 2941HV.
It should be noted that, in the present invention, the working pressure of the forming apparatus may be measured by providing a pressure sensor at the pressing head 210, or other structures of the prior art capable of measuring and implementing the working pressure may be adopted, which is not described in detail herein.
It should be noted that, the connection relationships of the components not specifically mentioned in the present invention are all default to the prior art, and the connection relationships of the structures are not described in detail because they do not relate to the invention points and are common applications of the prior art.
It should be noted that, when numerical ranges are referred to in the present invention, it should be understood that two endpoints of each numerical range and any numerical value between the two endpoints are optional, and because the adopted step method is the same as the embodiment, in order to prevent redundancy, the present invention describes a preferred embodiment. While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (10)
1. The preparation method of the reaction sintering silicon carbide ceramic temperature equalizing plate is characterized by comprising the following steps:
1) Weighing the raw materials according to the raw material proportion of the reaction sintering silicon carbide ceramic temperature-uniforming plate;
2) Ball milling and mixing;
3) Granulating by spraying;
4) And (5) press forming:
performing compression molding by using compression molding equipment;
5) Drying the biscuit;
6) Oxidizing in air to remove carbon;
7) Sintering at high temperature;
the press forming apparatus includes:
an upper press die (100);
lower compacting tool set (300) is in last compacting tool set (100) below, be provided with compacting tool set head (200) between last compacting tool set (100) and the lower compacting tool set (300), the top surface of lower compacting tool set (300) is provided with suppression groove (310), the vertical activity in suppression groove (310) bottom is provided with vibrating plate (311), the inside horizontal rotation of vibrating plate (311) is provided with central stirring dish (312), be provided with a plurality of stirring teeth (314) on the top surface of central stirring dish (312), horizontal rotation is provided with central follow-up dish (315) on the top surface of vibrating plate (311), stirring teeth (314) pass the top surface of vibrating plate (311) and insert in the perforation on central follow-up dish (315), the inside stirring motor (330) and the vibration mechanism of being provided with of lower compacting tool set (300), stirring motor (330) with central stirring dish (312) are connected, so as to drive central stirring dish (312) horizontal rotation, vibration mechanism drive vibration plate (311) are in the vibration direction.
2. The method for manufacturing the reactive sintered silicon carbide ceramic temperature uniformity plate according to claim 1, wherein the vibration mechanism comprises a vibration motor (320) and an eccentric wheel (321), the eccentric wheel (321) is arranged on a rotating shaft of the vibration motor (320), and the eccentric wheel (321) is in contact with the bottom of the vibration plate (311).
3. The method for preparing the reaction-sintered silicon carbide ceramic soaking plate according to claim 1, wherein an edge stirring disk (313) is further horizontally rotatably arranged inside the vibration plate (311), the edge stirring disk (313) is meshed with the central stirring disk (312), a plurality of stirring teeth (314) are also arranged on the top surface of the edge stirring disk (313), an edge following disk (316) is horizontally rotatably arranged on the top surface of the vibration plate (311) at a position corresponding to the edge stirring disk (313), and the stirring teeth (314) on the edge stirring disk (313) penetrate through the top surface of the vibration plate (311) and are inserted into through holes on the edge following disk (316), and the stirring teeth (314) can move relative to the top surface of the vibration plate (311).
4. The method for preparing a reactive sintered silicon carbide ceramic temperature uniformity plate according to claim 1, wherein a vertical driving rod is arranged in the center of the bottom surface of the central stirring disk (312), and a driving shaft at the top of the stirring motor (330) is vertically inserted into the driving rod in a sliding manner.
5. The method for preparing the reactive sintering silicon carbide ceramic soaking plate according to claim 1, wherein a pressing head (210) is arranged on the bottom surface of the pressing die head (200), the position of the pressing head (210) corresponds to the pressing groove (310), and the shape and the size of the pressing head (210) are matched with the pressing groove (310).
6. The method for preparing the reaction sintering silicon carbide ceramic temperature-uniforming plate by using the method for preparing the reaction sintering silicon carbide ceramic temperature-uniforming plate according to claim 1 is characterized in that the reaction sintering silicon carbide ceramic temperature-uniforming plate is composed of the following raw materials: base stock, dispersant, plasticizer and lubricant.
7. The method for preparing the reactive sintering silicon carbide ceramic temperature-uniforming plate according to claim 6, wherein the working pressure of the compression molding equipment is 160-200MPa.
8. The method for preparing the reactive sintering silicon carbide ceramic temperature-homogenizing plate by using the method is characterized in that the specific parameters of oxidizing and removing carbon in air are as follows:
and 5) loading the biscuit processed in the step 5) into an oxidation furnace, heating up in the atmospheric environment, heating up to 450 ℃ at a speed of 2 ℃/min, preserving heat for 2 hours, and oxidizing to remove free carbon in the biscuit.
9. The method for preparing the reactive sintering silicon carbide ceramic temperature-equalizing plate by using the method is characterized in that the treated biscuit is orderly filled into a hot isostatic pressing sintering furnace, a furnace door is closed, a vacuum pump is started to vacuumize, the temperature is raised to 900 ℃ at 5 ℃/min, the vacuum is kept for 0.5h, a vacuum pump is closed, argon is started to be filled until the pressure gauge of the sintering furnace shows 0.01bar, the temperature is raised to 1200 ℃ at 4 ℃/min, and the temperature is kept for 1h; then argon is filled until the pressure gauge shows 5bar, the temperature is increased to 1900 ℃ at 3 ℃/min, and the temperature is kept for 1.5h; then argon is filled until the pressure gauge shows 95bar, the temperature is raised to 1950 ℃ at 1 ℃/min, the temperature is kept for 10min, a heating system is closed, the pressure in the furnace is kept unchanged, the pressure is relieved when the temperature is reduced to 1500 ℃, and then the furnace is cooled to room temperature along with the furnace and opened.
10. The reactive-sintered silicon carbide ceramic temperature-equalizing plate prepared by the preparation method according to any one of claims 1 to 9.
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