CN114953102B - Device and method for preparing seamless ceramic hollow floating ball by hollow pressurizing grouting - Google Patents
Device and method for preparing seamless ceramic hollow floating ball by hollow pressurizing grouting Download PDFInfo
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- CN114953102B CN114953102B CN202210691038.2A CN202210691038A CN114953102B CN 114953102 B CN114953102 B CN 114953102B CN 202210691038 A CN202210691038 A CN 202210691038A CN 114953102 B CN114953102 B CN 114953102B
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- 238000007667 floating Methods 0.000 title claims abstract description 48
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- 239000007788 liquid Substances 0.000 claims abstract description 52
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000005238 degreasing Methods 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 abstract description 9
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- 239000000463 material Substances 0.000 description 10
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/26—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
- B28B1/265—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor pressure being applied on the slip in the filled mould or on the moulded article in the mould, e.g. pneumatically, by compressing slip in a closed mould
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/26—Producing shaped prefabricated articles from the material by slip-casting, i.e. by casting a suspension or dispersion of the material in a liquid-absorbent or porous mould, the liquid being allowed to soak into or pass through the walls of the mould; Moulds therefor ; specially for manufacturing articles starting from a ceramic slip; Moulds therefor
- B28B1/261—Moulds therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
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- Ceramic Engineering (AREA)
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- Mechanical Engineering (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Producing Shaped Articles From Materials (AREA)
Abstract
The invention provides a device and a method for preparing a seamless ceramic hollow floating ball by hollow pressurized grouting. The device comprises an outer mold frame, a mold, an inner mold cavity, a slurry pipeline and a liquid discharge pipeline, wherein a slurry flowing hole is formed in the lowest part of the inner mold cavity, the slurry pipeline is U-shaped, the first end of the slurry pipeline is connected with the slurry flowing hole, the second end is connected with automatic grouting equipment, and the height of the second end is larger than that of the first end. Grouting is carried out through a slurry pipeline, and a U-shaped slurry pipeline is utilized to enable a slurry flowing hole to be plugged by slurry, so that the integrity of a blank body is ensured. When the hollow floating ball is prepared, a blank is formed in an inner die cavity by adopting a pressurizing grouting and single-side liquid discharging mode, then the blank is obtained by demoulding, and the ceramic hollow floating ball is obtained after drying, degreasing and sintering. The blank with uniform thickness and high density is prepared by adopting the method, and the seamless hollow floating ball obtained after sintering has few defects, high quality stability and controllable size.
Description
Technical Field
The invention relates to the technical field of inorganic ceramic hollow floating ball preparation, in particular to a device and a method for preparing a seamless ceramic hollow floating ball by hollow pressurized grouting.
Background
In the 21 st century, deep sea exploration and development has been increasingly emphasized by countries around the world, and the deep sea exploration and development has been continuously developed without the deep diving equipment. The requirements for developing deep diving equipment such as full sea deep (deepest 11000 m) deep diving equipment are urgent, wherein the research on high-performance ceramic hollow buoyancy balls which are one of the deep sea key materials of the equipment is not great in China.
At present, a domestic preparation method of a Si 3N4 ceramic hollow floating ball adopts a method of gel casting of a half spherical shell or 3D printing and then sealing and sintering, wherein gel casting monomers have certain toxicity and are not easy to realize mass production, and a 3D printing-molded Si 3N4 ceramic half spherical shell green body is unevenly contracted in a post-treatment process to form a wall thickness gradient.
It is also reported that thousands of Al 2O3 ceramic hollow floating balls carried on U.S. sea god type deep diving apparatus are seamless floating balls, but the technique of gypsum mold normal pressure hollow rolling grouting molding is used, belonging to primary gypsum mold single-sided grouting molding, which has the defects that: 1) Single-sided liquid discharge under normal pressure leads to insufficient green body density; 2) The rolling auxiliary molding of the die is easy to cause uneven thickness of the ball blank and has great operation difficulty; 3) The demolding is difficult, the blank is easy to damage during demolding, and higher yield is difficult to ensure.
Disclosure of Invention
In view of the above, the invention aims to provide a device and a method for preparing a seamless ceramic hollow floating ball by hollow pressurized grouting, which can obtain a blank body with uniform thickness and higher density, and the blank body is sintered to obtain the seamless hollow floating ball, which has few defects and good overall quality stability, and can greatly reduce material consumption and procedures.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
The utility model provides a device of hollow pressurization slip casting preparation seamless ceramic hollow floater, the device includes external mold frame, mould, interior die cavity, thick liquids pipeline and flowing back pipeline, the inside cavity of mould has formed interior die cavity, sets up the thick liquid hole in the lowest department of die cavity, thick liquids pipeline is the U-shaped, and the first end and the thick liquid hole of thick liquids pipeline are connected, and the second end of thick liquids pipeline passes mould, external mold frame and automatic slip casting equipment connection, and the height of second end is greater than the height of first end. Grouting is carried out through a slurry pipeline, and a U-shaped slurry pipeline is utilized to enable a slurry flowing hole to be plugged by slurry, so that the integrity of a blank body is ensured.
Further, the slurry pipeline is used for grouting the inner die cavity to form a blank body, and the vertical distance H between the second end and the inner wall of the blank body is 3-5 mm, so that the slurry in the inner die cavity is higher than the slurry flowing holes.
Further, the automatic grouting equipment is connected with an air compressor. The compressed air of the air compressor is utilized to push the slurry into the inner die cavity, so that the slurry is pressurized and injected.
Further, the inside of the die is provided with a plurality of communicated micropores, the micropores are used for enabling liquid in the slurry to pass through, but solid substances in the slurry cannot pass through, one end of the liquid discharge pipeline is communicated with the die, and the other end of the liquid discharge pipeline penetrates out of the outer die frame. In the process of injecting the slurry into the inner mold cavity through the slurry pipeline, redundant liquid is discharged through the liquid discharge pipeline through micropores of the mold. By adopting the liquid discharging mode, liquid can only be discharged from the die to the outer side direction of the outer die frame, and the formed hollow floating ball obtained by the single-side liquid discharging mode has uniform structure, does not have interlayer defects and can ensure the quality of the hollow floating ball.
Further, the device also comprises a vacuumizing pipeline, one end of the vacuumizing pipeline is connected with the internal mold cavity, and the other end of the vacuumizing pipeline is connected with the vacuumizing device. Before the slurry is injected, the inner mold cavity is vacuumized through a vacuumizing pipeline, so that the effects of exhausting and defoaming during slurry feeding are achieved, and the blank is prevented from being left to foam.
Further, the outer die frame comprises an upper outer die frame and a lower outer die frame, and the upper outer die frame and the lower outer die frame are buckled and connected together to form the outer die frame. The outer mold frame is formed by two parts, so that the outer mold frame can be opened or closed conveniently.
The invention also provides a method for preparing the seamless ceramic hollow floating ball by hollow pressurized grouting, which comprises the following steps:
s1, pressurizing and sealing an upper outer mold frame and a lower outer mold frame;
s2, opening a valve of a vacuumizing pipeline, closing a valve of a slurry pipeline and a valve of a liquid discharge pipeline, and vacuumizing by using the vacuumizing pipeline to ensure that the pressure of an inner die cavity is less than 100Pa;
S3, closing a valve of the vacuumizing pipeline, opening a valve of the slurry pipeline and a valve of the liquid discharging pipeline, and pressurizing and injecting the slurry into the inner mold cavity through the slurry pipeline;
s4, stopping pressurizing grouting, demoulding to obtain a blank, and drying, degreasing and sintering to obtain the ceramic hollow floating ball.
Further, the step S3 includes three stages: the first stage, pressurizing the slurry to 0.1-0.2 MPa and maintaining the pressure for 2-4 min; step two, pressurizing the slurry to 0.5-0.6 MPa and maintaining the pressure for 8-10 min; and thirdly, pressurizing the slurry to 1.0-1.5 MPa and maintaining the pressure for 1.5-2 h. Through setting up the pressurization slip casting of different stages to increase pressure gradually, prevent that solid particle in the thick liquids from plugging up the micropore and making liquid unable to discharge, also help solid particle in the thick liquids and liquid quick separation simultaneously. And the pressurizing grouting molding is used, and the maximum holding pressure is increased to 1.5MPa, so that a green body with higher density can be prepared.
In step S4, the outer mold frame is opened during demolding, so that the upper outer mold frame and the lower outer mold frame are separated, and the seamless blank is obtained by demolding through a compressed air back blowing mode. The upper outer mold frame and the lower outer mold frame can be separated to obtain a seamless blank body, so that the seamless ceramic hollow floating ball is convenient to prepare.
In the step S4, the blank is dried for 15-20 h at 100-120 ℃, degreased for 10-15 h at 600-700 ℃, and sintered for 10-15 h at 1610-1650 ℃ to obtain the seamless hollow floating ball.
Compared with the prior art, the device and the method for preparing the seamless ceramic hollow floating ball by hollow pressurized grouting have the following advantages:
(1) The method of pressurized grouting is adopted, the thickness of the formed blank body is relatively uniform, the processing amount is small, even the processing is not needed, the material consumption can be greatly reduced, the working procedures are reduced, and the cost is reduced; the relative density of the green body is high by means of pressurized grouting and single-side liquid discharge, and meanwhile, the uniformity degree of the tissue structure of the green body is increased, so that the sintering of the subsequent green body is facilitated;
(2) The wall thickness of the blank body can be conveniently controlled by controlling the time of pressurized grouting, and products with various specifications can be manufactured;
(3) The hollow floating ball is prepared by adopting a seamless direct solidification molding method, so that defects can be greatly reduced, and the overall quality stability of a hollow floating ball product is improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
FIG. 1 shows a device for preparing a seamless ceramic hollow floating ball by hollow pressurized grouting.
Reference numerals illustrate:
1. an outer mold frame; 2. a mold; 3. an inner mold cavity; 4. a die-closing surface; 5. a liquid discharge pipeline; 6. a liquid discharge pipeline valve; 7. a vacuumizing pipeline; 8. a vacuum pipeline valve; 9. a slurry pipeline; 10. a slurry pipeline valve; 11. a residual material recycling bin; 13. a pulp flow hole; 14. an upper outer mold frame; 15. and (5) a lower outer mold frame.
Detailed Description
The invention will be described in detail below with reference to the drawings in connection with embodiments. The described embodiments of the present invention are exemplary and intended to be illustrative of the present invention and should not be construed as limiting the invention.
It should be noted that, the positional or positional relationship indicated by the terms such as "upper", "lower", "left", "right", "front", "rear", etc. are based on the positional or positional relationship shown in the drawings, and are merely for convenience of describing the present invention and simplifying the description, and are not indicative or implying that the apparatus or element in question must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. Embodiments of the invention and features of the embodiments may be combined with each other without conflict.
The data in the examples set forth below were obtained by the inventors through numerous experiments, only a portion of which is shown in the specification for the sake of brevity, and one of ordinary skill in the art will understand and practice the application under the data. These examples are only for illustrating the present application and are not intended to limit the scope of the present application. It should be further understood that various changes and modifications to the present application may be made by those skilled in the art after reading the disclosure of the present application, and such changes and modifications are also within the scope of the present application.
As shown in fig. 1, the invention provides a device for preparing a seamless ceramic hollow floating ball by hollow pressurized grouting, which comprises an outer mold frame 1, a mold 2, an inner mold cavity 3, a slurry pipeline 9 and a liquid discharge pipeline 5, wherein the inner mold cavity 3 is formed in the hollow inside of the mold 2, and the device comprises the outer mold frame 1, the mold 2 and the inner mold cavity 3 from outside to inside. The lowest part of the inner die cavity 3 is provided with a slurry flowing hole 13, the slurry pipeline 9 is U-shaped, one end of the slurry pipeline 9 is a first end, and the other end is a second end. The first end of the slurry pipeline 9 is connected with the slurry flowing hole 13, the second end passes through the die 2, the outer die frame 1 and the automatic grouting equipment to be connected, and the height of the second end is larger than that of the first end. Grouting is carried out through the slurry pipeline 9, and the U-shaped slurry pipeline 9 is utilized, so that the slurry flowing holes 13 can be plugged by slurry, and the integrity of the blank body is ensured. The lowest position of the inner mold cavity 3 is at the lowest side in the height direction of the outer mold frame 1 (i.e., up and down in fig. 1). The second end has a height greater than the first end in the height direction of the outer mold frame 1. The automatic grouting device injects slurry into the inner die cavity 3 through the slurry pipeline 9 and the slurry flowing holes 13 so that the slurry forms a blank body in the inner die cavity 3. After the slurry is injected into the inner mold cavity 3, the liquid in the slurry is discharged, and solid particles in the slurry are left in the inner mold cavity 3 and are continuously accumulated into a blank body with a certain wall thickness. The blank is demoulded, dried and sintered to obtain the seamless ceramic hollow floating ball. The slurry includes, but is not limited to, any one of Al 2O3 slurry, si 3N4 slurry, zrO 2 slurry, siO 2 slurry, mgO slurry, and Y 2O3 slurry. Preferably, the diameter of the flow holes 13 is 5-8 mm. The vertical distance H between the second end and the inner wall of the blank body is 3-5 mm, so that the slurry in the inner die cavity 3 is higher than the slurry flowing holes 13. The inner wall of the blank refers to the side of the blank formed in the inner cavity 3 away from the mold 2 after grouting, the outer wall of the blank refers to the side of the blank formed in the inner cavity 3 close to the mold 2 after grouting, and the corresponding distance between the inner wall and the outer wall is the wall thickness of the blank.
A slurry pipeline valve 10 is arranged on the slurry pipeline 9 and is used for controlling the opening and closing of the slurry pipeline 9. Specifically, the slurry line valve 10 is a ball valve.
In the preparation process of the hollow floating ball, a pressurizing grouting mode is adopted. The automatic grouting equipment is connected with the air compressor. The slurry is pushed into the inner die cavity 3 by the compressed air of the air compressor, so that the slurry is pressurized and injected.
The inside of the mold 2 has a plurality of interconnected micro-holes for passing the liquid in the slurry but not the solid matter in the slurry. Specifically, the mold 2 is made of a high-strength resin material, and is convenient for reverse mold solidification molding to form the inner mold cavity 3. More specifically, the mold 2 may be an epoxy resin. One end of the liquid discharge pipeline 5 is communicated with the die 2, and the other end of the liquid discharge pipeline penetrates out of the outer die frame 1. Since the drain line 5 is in communication with the mold 2, and the plurality of micro-holes inside the mold 2 are in communication with each other. During the injection of the slurry into the inner mould cavity 3 via the slurry line 9, excess liquid is drained via the drain line 5 through the micro-holes of the mould 2. By adopting the liquid discharging mode, liquid can only be discharged from the die 2 to the outer side direction of the outer die frame 1, and the formed hollow floating ball obtained by the single-side liquid discharging mode has uniform structure, does not have interlayer defects, and can ensure the quality of the hollow floating ball. A drain pipeline valve 6 is arranged on the drain pipeline 5, and the opening and closing of the drain pipeline 5 is controlled through the drain pipeline valve 6. Specifically, the drain pipeline valve 6 is a ball valve.
For the inner mold cavity 3, the mold 2 is heated and softened, then a spherical mold body is put in, after the mold 2 is cooled and hardened, the mold body is taken out, and the inner mold cavity 3 is formed in the mold 2, and the inner mold cavity 3 and the mold body have the same size. In view of the fact that the molding technology of the inner cavity 3 is prior art, no further description is given here.
The device also comprises a vacuum-pumping pipeline 7 for evacuating the inner mould cavity 3. One end of the vacuumizing pipeline 7 is connected with the inner die cavity 3, and the other end of the vacuumizing pipeline is connected with the vacuumizing device. Before the slurry is injected, the inner mold cavity 3 is vacuumized through a vacuumizing pipeline 7, so that the effects of exhausting and defoaming during the slurry feeding are achieved, and the blank body is prevented from being left to foam. The vacuumizing pipeline 7 is provided with a vacuumizing pipeline valve 8 for controlling the opening and closing of the vacuumizing pipeline 7. Specifically, the vacuumizing pipeline valve 8 is a ball valve. In fig. 1, the evacuation line 7 and the slurry line 9 share a part of the lines.
After grouting is completed, the redundant slurry is required to be discharged, and the discharged slurry can be reserved for the next use. When grouting, the slurry pipeline 9 is used as a grouting pipeline to inject slurry into the inner die cavity 3, and when grouting is finished, the slurry pipeline 9 is used as a slurry discharging pipeline to discharge the redundant slurry in the inner die cavity 3 and collect the redundant slurry into the residual material recycling bin 11. Because the slurry pipeline 9 is of a U-shaped structure, according to the principle of the communicating vessel, slurry is ensured to be present at the second end of the slurry pipeline 9 in the slurry discharging process, then slurry is always present at the slurry flow hole 13, the slurry flow hole 13 is sealed by slurry, and after natural drying, the slurry at the slurry flow hole 13 is deposited and dried to seal the slurry flow hole 13, so that the formed blank body is complete.
The outer die frame 1 comprises an upper outer die frame 14 and a lower outer die frame 15, the upper outer die frame 14 and the lower outer die frame 15 are buckled and connected together to form the outer die frame 1, and the joint of the upper outer die frame 14 and the lower outer die frame 15 is a die clamping surface 4. The outer mold frame 1 is formed by two parts, so that the upper outer mold frame 14 and the lower outer mold frame 15 are separated after grouting is finished, and a blank formed by the inner mold cavity 3 is taken out. The outer mold frame 1 is made of marble or other hard stone materials, and can bear extrusion during pressurized sealing.
The device has long service life, does not need drying, and can be repeatedly used. Meanwhile, a plurality of groups of devices can be connected in series, so that the production efficiency is greatly improved.
The method for preparing the seamless ceramic hollow floating ball by hollow pressurization comprises the following steps:
s1, pressurizing and sealing an upper outer die frame 14 and a lower outer die frame 15;
Specifically, in order to prevent the slurry from overflowing from the joint of the upper outer mold frame 14 and the lower outer mold frame 15, the upper outer mold frame 14 and the lower outer mold frame 15 are subjected to a pressurizing treatment, so that the slurry is prevented from being lost. After the upper outer mold frame 14 and the lower outer mold frame 15 are closed, a pressure seal may be applied by a jack or other clamp.
S2, opening a vacuumizing pipeline valve 8, closing a slurry pipeline valve 10 and a liquid discharge pipeline valve 6, and vacuumizing by using the vacuumizing pipeline 7 to ensure that the pressure of the inner die cavity 3 is less than 100Pa;
s3, closing a vacuumizing pipeline valve 8, opening a slurry pipeline valve 10 and a liquid discharge pipeline valve 6, and pressurizing and injecting slurry into the inner mold cavity 3 through a slurry pipeline 9;
Specifically, the automatic grouting device pressurizes and injects slurry into the inner mold cavity 3 through the slurry pipeline 9 and the slurry flowing holes 13 in sequence. In total, the method comprises three stages in the compression slip casting: the first stage, pressurizing the slurry to 0.1-0.2 MPa and maintaining the pressure for 2-4 min; step two, pressurizing the slurry to 0.5-0.6 MPa and maintaining the pressure for 8-10 min; and thirdly, pressurizing the slurry to 1.0-1.5 MPa and maintaining the pressure for 1.5-2 h. Through setting up the pressurization slip casting of different stages to increase pressure gradually, prevent that the solid particle in the thick liquids from plugging up the micropore and making liquid unable discharge, also help solid particle in the thick liquids and liquid quick separation simultaneously, solid particle stays in interior die cavity 3, and liquid discharges flowing back pipeline 5 through the micropore. Because the pressurizing grouting molding is used, and the maximum holding pressure is increased to 1.5MPa, a green body with higher density can be prepared, and the relative density of the green body can reach 65-70%. When the micropores of the mould 2 are utilized for draining, the liquid in the slurry is naturally dried, and the obtained blank has fewer defects.
In the pressurized grouting process, the liquid near the inner side of the mold 2 is firstly discharged, and correspondingly, the solid particles near the mold 2 are firstly dried and deposited, so that the solid particles in the slurry are continuously accumulated along the contour of the inner side of the mold 2 from outside to inside, the inner mold cavity 3 is continuously filled, and a blank body with a certain wall thickness is gradually formed. Because of the pressurized grouting and the U-shaped pipe of the slurry pipeline 9, the slurry can only enter the inner mold cavity 3 from the slurry flowing hole 13, and cannot flow out of the slurry flowing hole 13 from the inner mold cavity 3.
S4, stopping pressurizing grouting, demoulding to obtain a blank, and drying, degreasing and sintering to obtain the ceramic hollow floating ball.
Specifically, the wall thickness of the green body is controlled according to the time of pressurized grouting, and the longer the time of pressurized grouting is, the thicker the wall thickness of the green body is. The wall thickness of the blank body can be conveniently controlled by controlling the pressurizing time, and products with various specifications can be manufactured. The wall thickness of the blank is typically 8-12mm.
And stopping grouting when the blank with the required wall thickness is reached, and immediately releasing pressure. At this time, the drain pipe valve 6 is closed, and the slurry pipe valve 10 is kept open, so that the slurry which is not solidified and formed is discharged from the slurry pipe 9 into the residual material recycling bin 11. Because the lowest part of the inner die cavity 3 is provided with the flow holes 13, the blank body has hole defects at the lowest part correspondingly, and the holes of the blank body can be naturally deposited, dried and solidified to form a complete blank body after the slurry is naturally dried for more than 30 hours.
In demolding, the outer mold frame 1 is opened, the upper outer mold frame 14 and the lower outer mold frame 15 are separated, and a seamless blank is obtained by demolding in a compressed air back blowing mode. Simple trimming is carried out on the holes of the blank, and the seamless hollow floating ball is prepared after drying for 15-20 h at 100-120 ℃, degreasing for 10-15 h at 600-700 ℃ and sintering for 10-15 h at 1610-1650 ℃. Wherein, the green body is always placed in a bowl-shaped corundum sagger with proper size in the drying, degreasing and sintering processes, so as to prevent cracking and deformation when the thermal stress is released or the thermal creep occurs.
The invention has the advantages of larger pressure assistance during grouting, more uniform thickness of the formed blank, small processing amount and even no need of processing, and can greatly reduce consumable materials and procedures, thereby reducing the cost and being suitable for mass production. Because the pressure grouting is adopted, the relative density of the green body is necessarily higher than the green body density formed by normal pressure slurry suction of a gypsum mold, and the uniformity of the green body tissue structure is increased, so that the sintering of the subsequent green body is facilitated. In addition, after grouting is completed, the upper outer die frame 14 and the lower outer die frame 15 are separated to obtain the blank of the hollow floating ball, and the blank of the two hollow floating ball semi-spherical shells does not need to be manufactured respectively and then subjected to sealing sintering, so that the hollow floating ball is prevented from being slotted, and the overall quality stability of the hollow floating ball can be improved.
Example 1
In this example, the present invention will be described in detail by taking a method for producing a seamless Al 2O3 ceramic hollow floating ball having an outer diameter of about 10cm as an example. The preparation method of the seamless Al 2O3 ceramic hollow floating ball comprises the following steps:
Mixing Al 2O3 powder, dispersant, binder and water in proportion, controlling the solid content to be 85% and the fineness to be 3 mu m, and then adding 0.8-1.5% (w/v) of nano TiO 2 powder to obtain 95% Al 2O3 slurry. The specific preparation method of the Al 2O3 slurry is the same as that of the prior art. TiO 2 powder is added to the Al 2O3 slurry as a sintering aid.
The specification of the inner die cavity 3 is designed and manufactured according to the specification of the die body, namely, the specification of the outer diameter is 14.5cm and the inner diameter is 12.5cm, namely, the wall thickness is 1 cm. The upper outer die frame 14 and the lower outer die frame 15 are assembled and closed, and pressurized and sealed by a jack. Only the vacuumizing pipeline valve 8 is opened, the vacuumizing pipeline 7 is utilized to vacuumize the interior of the inner die cavity 3 to 90Pa, then the vacuumizing pipeline valve 8 is closed, the slurry pipeline valve 10 and the liquid discharge pipeline valve 6 are opened, and the prepared Al 2O3 slurry is pressurized and injected into the inner die cavity 3 through the liquid discharge pipeline 5 and the slurry flowing hole 13. Pressurized grouting is divided into three stages: the first stage is pressurized to 0.2MPa and maintained for 2min, the second stage is pressurized to 0.6MPa and maintained for 8min, and the third stage is pressurized to 1.5MPa and maintained for 1.5h. In the pressurized grouting process, water in the Al 2O3 slurry is discharged from the outer mold frame 1 through the micropores of the mold 2.
And after the pressure maintaining is finished, immediately releasing pressure, closing the liquid discharge pipeline valve 6, and discharging the redundant slurry in the inner mold cavity 3 into the residual material recycling bin 11 along the slurry pipeline 9. And naturally drying for 35 hours, naturally depositing, drying and solidifying the slurry to well block the holes of the blank body, and forming the finished blank body of the Al 2O3 hollow floating ball.
The outer mold frame 1 is opened, the upper outer mold frame 14 and the lower outer mold frame 15 are separated, and the blank is obtained by demolding through a compressed air back blowing mode. Drying at 120 ℃ for 15h, degreasing at 700 ℃ for 10h, and sintering at 1650 ℃ for 10h to obtain the seamless 95% Al 2O3 ceramic hollow floating ball with the density reaching 3.90g/cm 3.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (7)
1. The method for preparing the seamless ceramic hollow floating ball by hollow pressurized grouting is characterized by comprising an outer mold frame (1), a mold (2), an inner mold cavity (3), a slurry pipeline (9) and a liquid discharge pipeline (5), wherein the inner mold cavity (3) is formed in the hollow inside of the mold (2), a slurry flowing hole (13) is formed in the lowest part of the inner mold cavity (3), the slurry pipeline (9) is U-shaped, a first end of the slurry pipeline (9) is connected with the slurry flowing hole (13), a second end of the slurry pipeline (9) penetrates through the mold (2), the outer mold frame (1) and automatic grouting equipment, the height of the second end is larger than that of the first end, a plurality of micropores which are communicated with each other are formed in the mold (2) and are used for enabling liquid in the slurry to pass through but solid matters in the slurry cannot pass through, one end of the liquid discharge pipeline (5) is communicated with the mold (2), and the other end of the slurry pipeline (9) penetrates out of the outer mold frame (1);
The method comprises the following steps:
s1, pressurizing and sealing an upper outer mold frame (14) and a lower outer mold frame (15);
S2, opening a vacuumizing pipeline valve (8), closing a slurry pipeline valve (10) and a liquid discharge pipeline valve (6), and vacuumizing by using a vacuumizing pipeline (7) to enable the pressure of the inner die cavity (3) to be less than 100Pa;
S3, closing a vacuumizing pipeline valve (8), opening a slurry pipeline valve (10) and a liquid discharge pipeline valve (6), and injecting slurry into the inner mold cavity (3) through pressurization of a slurry pipeline (9); pressurized grouting comprises three stages: the first stage, pressurizing the slurry to 0.1-0.2 MPa and maintaining the pressure for 2-4 min; the second step, pressurizing the slurry to 0.5-0.6 MPa and maintaining the pressure for 8-10 min; thirdly, pressurizing the slurry to 1.0-1.5 MPa and maintaining the pressure for 1.5-2 hours;
s4, stopping pressurizing grouting, demoulding to obtain a blank, and drying, degreasing and sintering to obtain the ceramic hollow floating ball.
2. The method for preparing the seamless ceramic hollow floating ball by the hollow pressurized grouting according to claim 1, wherein a blank body is formed by grouting the slurry pipeline (9) into an inner die cavity (3), and the vertical distance H between the second end and the inner wall of the blank body is 3-5 mm.
3. The method for preparing a seamless ceramic hollow floating ball by hollow pressurized grouting according to claim 1, wherein the automatic grouting equipment is connected with an air compressor.
4. The method for preparing the seamless ceramic hollow floating ball by hollow pressurized grouting according to claim 1, wherein the device further comprises a vacuumizing pipeline (7), one end of the vacuumizing pipeline (7) is connected with the inner die cavity (3), and the other end of the vacuumizing pipeline is connected with a vacuumizing device.
5. The method for preparing the seamless ceramic hollow floating ball by hollow pressurized grouting according to claim 1, wherein the outer mold frame (1) comprises an upper outer mold frame (14) and a lower outer mold frame (15), and the upper outer mold frame (14) and the lower outer mold frame (15) are buckled and connected together to form the outer mold frame (1).
6. The method for preparing the seamless ceramic hollow floating ball by the hollow pressurized grouting according to claim 1, wherein in the step S4, the outer mold frame (1) is opened during demolding, the upper outer mold frame (14) and the lower outer mold frame (15) are separated, and a seamless blank is obtained by demolding in a compressed air back blowing mode.
7. The method for preparing the seamless ceramic hollow floating ball by the hollow pressurized grouting according to claim 1, wherein in the step S4, the blank is dried at 100-120 ℃ for 15-20 h, degreased at 600-700 ℃ for 10-15 h, and sintered at 1610-1650 ℃ for 10-15 h to prepare the seamless hollow floating ball.
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