CN114478000B - Liquid injection sintering equipment based on high-purity strontium titanate powder material and use method - Google Patents
Liquid injection sintering equipment based on high-purity strontium titanate powder material and use method Download PDFInfo
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- CN114478000B CN114478000B CN202210065580.7A CN202210065580A CN114478000B CN 114478000 B CN114478000 B CN 114478000B CN 202210065580 A CN202210065580 A CN 202210065580A CN 114478000 B CN114478000 B CN 114478000B
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- C04B35/475—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on bismuth titanates
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- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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Abstract
The invention discloses liquid injection sintering equipment based on a high-purity strontium titanate powder material and a using method thereof, wherein the liquid injection sintering equipment comprises a separation cavity, a first feeding hole and a second feeding hole, wherein the side wall of the separation cavity is provided with the first feeding hole and the second feeding hole in a vertically staggered manner; the screening and separating assembly is arranged in the position of the plane of the first feeding hole in the separating cavity; the mixing cavity is fixed below the separation cavity, and the center above the mixing cavity is connected with a central pipe which is communicated with the upper part of the center of the separation cavity; and the liquid injection pipe is distributed with a plurality of liquid injection pipes along the peripheral circumference of the central pipe, and the liquid injection pipes penetrate through the separation cavity and the mixing cavity. Compared with the prior art, the invention can change the fineness of the material particles entering the central tube, the energy consumption for sintering is less, the time is short, and the purity of the strontium titanate main material in the sintered finished product is high.
Description
Technical Field
The invention relates to the technical field of high-temperature material sintering equipment, in particular to liquid injection sintering equipment based on a high-purity strontium titanate powder material and a using method thereof.
Background
Sintering is the process of heating a powder or powder compact to a temperature below the melting point of the essential components therein, and then cooling to room temperature. As a result of sintering, bonding between the powder particles occurs, the strength of the sintered body increases, and the agglomerates of the powder particles become agglomerates of grains, thereby obtaining the desired physical and mechanical properties of the article or material. Strontium titanate, useful as electronic ceramic material and artificial gem, of formula SrTiO 3 A melting point of 2060 ℃ is a high-refractive-index materialAnd a high temperature superconducting substrate material. Due to SrTiO 3 High melting point, sintering SrTiO by the existing sintering furnace 3 The powder needs higher temperature and longer time, and the energy consumption is high. The sintering temperature can be reduced by adding a sintering aid during sintering, and when the sintering aid can form a solid solution with a sintered object, the sintering aid can distort crystal lattices and activate the crystal lattices, but the introduction of the sintering aid can reduce SrTiO 3 The purity of the material.
Therefore, it is necessary to provide a liquid injection sintering apparatus based on high-purity strontium titanate powder material and a method for using the same, so as to solve the problems in the background art.
Disclosure of Invention
In order to achieve the purpose, the invention provides the following technical scheme: an injection sintering device based on a high-purity strontium titanate powder material comprises,
the side wall of the separation cavity is provided with a first feeding hole and a second feeding hole in a vertically staggered manner;
the screening and separating assembly is arranged in the position of the plane of the corresponding feed inlet in the separating cavity;
the mixing cavity is fixed below the separation cavity, and the center above the mixing cavity is connected with a central pipe which is communicated with the upper part of the center of the separation cavity;
and the liquid injection pipe is distributed with a plurality of liquid injection pipes along the peripheral circumference of the central pipe, and the liquid injection pipes penetrate through the separation cavity and the mixing cavity.
Further, preferably, the screening separation module includes,
the guide vanes are circumferentially distributed at the position of the plane of the feeding hole I, and an annular inner ring defined by each guide vane corresponds to the opened upper end face of the central pipe;
the spokes of the spoke support extend to the inner wall of the separation cavity along the radial direction of the spoke with the side wall of the upper end face of the central tube as a starting point, the spokes and the separation cavity are fixedly connected together, and the upper end face and the lower end face of the flow guide page are respectively connected with the upper end face of the separation cavity and the spoke support;
the lower part of the spoke support corresponds to the position of the plane of the second feeding port, and the space between the inner wall of the separation cavity below the second feeding port and the outer wall of the central tube is communicated with each liquid injection tube.
Further, as a preferred mode, the center of each guide vane is rotatably connected with the upper end face of the separation cavity and the spoke support through a rotating shaft.
Preferably, the upper end surface of the rotating shaft penetrates through the upper end surface of the separation cavity to the outer wall of the separation cavity, a connecting rod is fixed on each rotating shaft outside the separation cavity, a sliding groove is formed in the other end of each connecting rod, a sliding pin is connected in the sliding groove in a sliding manner, each sliding pin is fixed in an adjusting turntable together, and the adjusting turntable is rotatably connected with the upper end surface of the separation cavity.
Further, preferably, the top of the mixing cavity is provided with an air duct.
Further, as preferred, it has the notes liquid heating pipe to inlay in the notes liquid pipe inner wall, it runs through to mix the intracavity and is equipped with the notes liquid valve to annotate liquid socle portion.
Further, preferably, the bottom in the central tube is provided with a feeding door.
Further, preferably, a temperature adjusting heating pipe is embedded in the inner wall of the mixing cavity.
Further, preferably, the liquid injection pipe and the mixing chamber are made of refractory materials, and the outer wall of the liquid injection pipe and the outer wall of the mixing chamber are coated with heat insulation materials.
Furthermore, preferably, the use method of the injection sintering equipment based on the high-purity strontium titanate powder material,
the main material is blown into the separation cavity from the first feeding hole with certain kinetic energy through the fan, wherein the fineness of material particles entering the central tube can be controlled by adjusting the size of a gap between every two guide vanes through rotating the adjusting turntable, the main material particles with corresponding fineness enter the central tube, and other main materials enter the liquid injection tube, wherein the main material is SrTiO 3 ；
Blowing the auxiliary material into the separation cavity from the second feeding hole with certain kinetic energy through a fan, and enabling the auxiliary material to enter the liquid injection pipe, wherein the auxiliary material comprises a sintering aid;
heating and sintering the main material and the auxiliary material in the liquid injection pipe together into a liquid-phase material through a liquid injection heating pipe;
opening a feed door to enable the screened solid-phase particles to fall into a mixing cavity, wherein the fineness of the screened solid-phase particle main material is higher;
opening the liquid injection valve to inject the liquid phase material into the mixing cavity, wherein after the liquid phase material is mixed with the solid phase particles, the solid phase particles with high fineness are beneficial to improving the sintering densification speed, so that high final sintering density can be obtained in the particle rearrangement stage, the solid phase particles can move in the liquid phase, and the material migration between the solid phase particles and between the solid phase/liquid phase is strengthened;
and the temperature of the mixed sintering of the liquid-phase material and the solid-phase particles is controlled in the mixing cavity through the temperature-adjusting heating pipe.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the size of the gap between the guide vanes can be changed by rotating the adjusting turntable so as to change the rotation angle of the material particles which need to rotate when passing through the gap between the guide vanes, and the larger the material particles are, the larger the inertia of the material particles is, the more difficult the material particles pass through the gap between the guide vanes, so that the fineness of the material particles entering the central tube is changed.
In the invention, the existence of the auxiliary materials can reduce the sintering temperature, the materials enter the plurality of liquid injection pipes respectively, the inner diameters of the liquid injection pipes are smaller, the contact area between the materials and the liquid injection heating pipe is large, and the energy consumption and the time required by sintering the materials into a liquid phase are less and short.
According to the invention, after the liquid phase material and the solid phase particles are mixed, the solid phase particles with high fineness are beneficial to improving the sintering densification speed, the high final sintering density can be conveniently obtained in the particle rearrangement stage, the solid phase particles can conveniently move in the liquid phase, the migration of substances among the solid phase particles and between the solid phase and the liquid phase is strengthened, the sintering speed is accelerated, the sintering energy consumption is reduced, and the purity of the main material in the liquid phase material is improved.
Drawings
FIG. 1 is a schematic structural diagram of a liquid injection sintering device based on a high-purity strontium titanate powder material;
FIG. 2 is a schematic sectional structure diagram of a liquid injection sintering apparatus based on a high-purity strontium titanate powder material;
FIG. 3 is a schematic view of the structure of the sieving separator assembly;
in the figure: 1. a separation chamber; 2. a mixing chamber; 21. a temperature-adjusting heating pipe; 3. a first feeding hole; 4. a second feeding hole; 5. a central tube; 51. a feed gate; 6. a liquid injection pipe; 61. injecting liquid into the heating pipe; 62. a liquid injection valve; 7. an air duct; 8. a screening separation assembly; 81. a flow guide page; 82. a spoke support; 83. a rotating shaft; 84. adjusting the turntable; 85. a connecting rod; 86. a chute; 87. and (4) a sliding pin.
Detailed Description
Referring to fig. 1 and 2, in an embodiment of the present invention, an apparatus for liquid injection sintering based on a high-purity strontium titanate powder material includes,
the side wall of the separation cavity 1 is provided with a first feeding hole 3 and a second feeding hole 4 in a vertically staggered manner;
the screening and separating assembly 8 is arranged in the separation cavity 1 at a position corresponding to the plane where the first feeding hole 3 is located;
the mixing chamber 2 is fixed below the separation chamber 1, the center above the mixing chamber 2 is connected with a central pipe 5 which is communicated with the upper part of the center of the separation chamber 1, and a discharge door is also arranged in the mixing chamber 2;
and the liquid injection pipes 6 are distributed along the peripheral circumference of the central pipe 5, and penetrate through the separation cavity 1 and the mixing cavity 2.
Referring to fig. 3, in the present embodiment, the screening separation assembly 8 includes,
the guide vanes 81 are circumferentially distributed on the plane where the first feeding hole 3 is located, and an annular inner ring formed by surrounding of each guide vane 81 corresponds to the open upper end face of the central tube 5;
the spokes of the spoke support 82 extend to the inner wall of the separation cavity 1 along the radial direction of the spoke support with the side wall of the upper end surface of the central tube 5 as a starting point, and the spokes and the separation cavity are fixedly connected together, and the upper end surface and the lower end surface of the guide vane 81 are respectively connected with the upper end surface of the separation cavity 1 and the spoke support 82;
the lower part of the spoke support 82 corresponds to the position of the plane of the second feeding hole 4, and the space between the inner wall of the separation cavity 1 below the second feeding hole 4 and the outer wall of the central tube 5 is communicated with each liquid injection tube 6;
that is to say, the material with certain kinetic energy enters the separating cavity 1 from the first feeding hole 3, passes through the gap between the guide vanes 81, enters the ring formed by the guide vanes, enters the central tube 5, and the material which cannot pass through the guide vanes 81 loses kinetic energy and then enters the separating cavity 1 together with the material entering the liquid injection tube 6 through the second feeding hole 4, so that the separating effect is achieved.
In this embodiment, the center of each guide vane 81 is rotatably connected to the upper end surface of the separation chamber 1 and the spoke support 82 through a rotating shaft 83.
In this embodiment, the upper end surface of the rotating shaft 83 penetrates through the upper end surface of the separation chamber 1 to the outer wall thereof, a connecting rod 85 is fixed to each rotating shaft 83 outside the separation chamber 1, a sliding groove 86 is formed at the other end of the connecting rod 85, a sliding pin 87 is slidably connected in the sliding groove 86, each sliding pin 87 is jointly fixed in an adjusting turntable 84, and the adjusting turntable 84 is rotatably connected with the upper end surface of the separation chamber 1;
that is to say, through rotating the adjustment carousel 84, can drive every connecting rod 85 around the rotation of axis of rotation 83 in step, and then make every water conservancy diversion page or leaf 81 rotate in step to change the clearance size between every water conservancy diversion page or leaf 81, pass the corner that the clearance between water conservancy diversion page or leaf 81 needs rotated in order to change the material granule, because the bigger its inertia of material granule is bigger, also difficult passing the clearance between water conservancy diversion page or leaf 81, thereby change the fineness of the material granule that gets into in the center tube 5.
In this embodiment, the top of mixing chamber 2 has seted up air duct 7, air duct 7 is used for discharging the air current in the mixing chamber 2, preferably the round platform type body of upwards closing up, can prevent that the material from being taken out by the air current.
In the embodiment, a liquid injection heating pipe 61 is embedded in the inner wall of the liquid injection pipe 6, and the bottom of the liquid injection pipe 6 penetrates into the mixing chamber 2 and is provided with a liquid injection valve 62;
the materials entering the liquid injection pipe 6 from the part of the first feed port 3 and the second feed port 4 can be heated and sintered into a liquid phase by the liquid injection heating pipe 61, and the materials enter the liquid injection pipes 6 respectively, the inner diameter of each liquid injection pipe 6 is smaller, the contact area between the materials and the liquid injection heating pipe 61 is large, the sintering efficiency is high, and the sintered liquid phase materials can be injected into the mixing chamber 2 from the liquid injection valve 62.
In this embodiment, the bottom of the central tube 5 is provided with a feed gate 51 for controlling the amount of powder falling into the mixing chamber 2.
In this embodiment, a temperature adjusting heating pipe 21 is embedded in the inner wall of the mixing chamber 2.
In this embodiment, the liquid inlet pipe 6 and the mixing chamber 2 are made of refractory material, the outer wall of the liquid inlet pipe is coated with heat insulating material, and the refractory material is preferably magnesia-chrome material which can bear high temperature of more than two thousand degrees.
Also discloses a use method of liquid injection sintering equipment based on the high-purity strontium titanate powder material,
the main materials are blown into the separation cavity 1 from the first feeding hole 3 through the fan with certain kinetic energy, wherein the fineness of material particles entering the central tube 5 can be controlled by adjusting the size of a gap between each guide vane 81 through rotating the adjusting turntable 84, the main material particles with corresponding fineness enter the central tube 5, and the rest main materials enter the liquid injection tube 6, wherein the main material is SrTiO 3 ；
Blowing auxiliary materials into the separation cavity 1 from the second feeding port 4 with certain kinetic energy through a fan, and feeding the auxiliary materials into the liquid injection pipe 6, wherein the auxiliary materials comprise sintering aids for adjusting the temperature coefficient and the dielectric constant of the dielectric material and reducing the sintering temperature, and the sintering aids preferably comprise MgO, znO and SiO 2 ；
The main material and the auxiliary material in the liquid injection pipe 6 are heated and sintered together into a liquid-phase material through the liquid injection heating pipe 61, the sintering temperature can be reduced due to the existence of the auxiliary material, the sintering temperature is preferably 1000-1300 ℃, and the contact area between the material and the liquid injection heating pipe 61 is large due to the small space in the liquid injection pipe 6, so that the energy consumption for reaching the temperature is low, and the time is short;
the feeding door 51 is opened to enable the screened solid-phase particles to fall into the mixing cavity 2, and the fineness of the screened solid-phase particle main materials is high;
the liquid injection valve 62 is opened to inject the liquid-phase material into the mixing chamber 2, and after the liquid-phase material is mixed with the solid-phase particles, the solid-phase particles with high fineness are beneficial to improving the sintering densification speed, so that the high final sintering density can be obtained in the particle rearrangement stage, the solid-phase particles can move in the liquid phase, the material migration between the solid-phase particles and between the solid phase and the liquid phase is strengthened, the sintering speed is accelerated, the sintering energy consumption is reduced, and the use of sintering aids is reduced, so that the purity of the main materials in the liquid-phase material is improved;
meanwhile, the temperature of the mixed sintering of the liquid-phase material and the solid-phase particles is controlled in the mixing cavity 2 through a temperature-adjusting heating pipe 21, and the temperature is preferably 700-1000 ℃;
and taking out the material after sintering and cooling from a discharge door in the mixing cavity 2.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (7)
1. The liquid injection sintering equipment based on the high-purity strontium titanate powder material is characterized by comprising,
the side wall of the separation cavity (1) is provided with a first feeding hole (3) and a second feeding hole (4) in a vertically staggered manner;
the screening and separating assembly (8) is arranged in the separating cavity (1) and corresponds to the plane where the first feeding hole (3) is located;
the mixing cavity (2) is fixed below the separation cavity (1), and the center above the mixing cavity (2) is connected with a central pipe (5) which is communicated with the upper part of the center of the separation cavity (1);
the liquid injection pipes (6) are distributed along the periphery of the central pipe (5) and penetrate through the separation cavity (1) and the mixing cavity (2);
the screening separation assembly (8) comprises,
the guide vanes (81) are circumferentially distributed on the plane where the first feed inlet (3) is located, and an annular inner ring surrounded by each guide vane (81) corresponds to the open upper end face of the central pipe (5);
the spokes of the spoke support (82) extend to the inner wall of the separation cavity (1) along the radial direction of the spoke support with the side wall of the upper end surface of the central tube (5) as a starting point, the spokes and the separation cavity are fixedly connected together, and the upper end surface and the lower end surface of the flow guide vane (81) are respectively connected with the upper end surface of the separation cavity (1) and the spoke support (82);
the lower part of the spoke support (82) corresponds to the position of the plane of the second feeding hole (4), and the space between the inner wall of the separation cavity (1) below the second feeding hole (4) and the outer wall of the central tube (5) is communicated with each liquid injection tube (6);
a liquid injection heating pipe (61) is embedded in the inner wall of the liquid injection pipe (6), and the bottom of the liquid injection pipe (6) penetrates into the mixing cavity (2) and is provided with a liquid injection valve (62);
a temperature adjusting heating pipe (21) is embedded in the inner wall of the mixing cavity (2).
2. The injection sintering equipment based on the high-purity strontium titanate powder material is characterized in that the center of each guide vane (81) is rotatably connected with the upper end face of the separation cavity (1) and the spoke support (82) through a rotating shaft (83).
3. The liquid injection sintering equipment based on the high-purity strontium titanate powder material is characterized in that the upper end face of the rotating shaft (83) penetrates through the upper end face of the separation cavity (1) to the outer wall of the separation cavity, a connecting rod (85) is fixed on each rotating shaft (83) outside the separation cavity (1), a sliding groove (86) is formed in the other end of each connecting rod (85), a sliding pin (87) is connected in each sliding groove (86) in a sliding mode, each sliding pin (87) is fixed in an adjusting rotary disc (84) together, and the adjusting rotary discs (84) are rotatably connected with the upper end face of the separation cavity (1).
4. The liquid injection sintering equipment based on the high-purity strontium titanate powder material according to claim 1, wherein the top of the mixing chamber (2) is provided with a gas guide pipe (7).
5. The liquid injection sintering equipment based on the high-purity strontium titanate powder material is characterized in that a feeding gate (51) is arranged at the bottom in the central pipe (5).
6. The liquid injection sintering equipment based on the high-purity strontium titanate powder material as claimed in claim 1, wherein the liquid injection pipe (6) and the mixing chamber (2) are made of refractory materials, and the outer wall of the liquid injection pipe is coated with heat insulation materials.
7. The use method of the injection sintering equipment based on the high-purity strontium titanate powder material according to any one of claims 1 to 6 is characterized in that,
the main material is blown into the separation cavity (1) from the feed inlet I (3) with certain kinetic energy through the fan, wherein the fineness of the material particles entering the central tube (5) can be controlled by adjusting the size of a gap between each guide vane (81) through rotating the adjusting turntable (84), the main material particles corresponding to the fineness enter the central tube (5), the rest main material enters the liquid injection tube (6), wherein the main material is SrTiO 3 ；
Blowing auxiliary materials into the separation cavity (1) from the second feeding hole (4) with certain kinetic energy through a fan, and feeding the auxiliary materials into the liquid injection pipe (6), wherein the auxiliary materials comprise sintering aids;
the main material and the auxiliary material in the liquid injection pipe (6) are heated and sintered together into liquid-phase material through a liquid injection heating pipe (61);
opening a feeding door (51) to enable the screened solid-phase particles to fall into the mixing cavity (2), wherein the fineness of the main materials of the screened solid-phase particles is higher;
opening a liquid injection valve (62) to inject a liquid-phase material into the mixing chamber (2), wherein after the liquid-phase material is mixed with solid-phase particles, the solid-phase particles with high fineness are beneficial to improving the sintering densification speed, high final sintering density is obtained at a particle rearrangement stage, and the solid-phase particles move in a liquid phase to strengthen the material migration between the solid-phase particles and between the solid-phase and liquid-phase;
meanwhile, the temperature of the mixed sintering of the liquid-phase material and the solid-phase particles is controlled in the mixing cavity (2) through a temperature-adjusting heating pipe (21).
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| CN202210065580.7A CN114478000B (en) | 2022-01-20 | 2022-01-20 | Liquid injection sintering equipment based on high-purity strontium titanate powder material and use method |
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| CN202210065580.7A CN114478000B (en) | 2022-01-20 | 2022-01-20 | Liquid injection sintering equipment based on high-purity strontium titanate powder material and use method |
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| DE4415723A1 (en) * | 1994-05-05 | 1995-11-09 | Huels Chemische Werke Ag | Round burner for burning coal dust |
| CN205300246U (en) * | 2015-12-22 | 2016-06-08 | 郑州德森环境科技有限公司 | Vertical gradient sintering machine |
| CN205505731U (en) * | 2016-02-01 | 2016-08-24 | 罗松文 | High -efficient water conservancy diversion structure of catalytic debinding stove |
| CN109974355A (en) * | 2019-04-16 | 2019-07-05 | 西北工业大学 | A kind of gas-liquid separator |
| CN111928647A (en) * | 2020-08-24 | 2020-11-13 | 张家港宏昌钢板有限公司 | Sintering flue gas circulating device and technological method thereof |
| CN214095505U (en) * | 2021-01-15 | 2021-08-31 | 河南三特炉业科技有限公司 | Novel industrial hot air circulating furnace |
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