CN111174578A - charging container for combustion, charging method thereof, and method for synthesizing high α phase silicon nitride - Google Patents
charging container for combustion, charging method thereof, and method for synthesizing high α phase silicon nitride Download PDFInfo
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- CN111174578A CN111174578A CN201811345840.6A CN201811345840A CN111174578A CN 111174578 A CN111174578 A CN 111174578A CN 201811345840 A CN201811345840 A CN 201811345840A CN 111174578 A CN111174578 A CN 111174578A
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- charging
- ignition
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- powder
- container
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D3/00—Charging; Discharging; Manipulation of charge
- F27D3/0025—Charging or loading melting furnaces with material in the solid state
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D3/00—Charging; Discharging; Manipulation of charge
- F27D3/0084—Charging; Manipulation of SC or SC wafers
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D5/00—Supports, screens, or the like for the charge within the furnace
- F27D5/0068—Containers
Abstract
the invention discloses a charging container for combustion and a charging method thereof, and a synthesis method of high α phase silicon nitride, wherein the charging container comprises a charging boat for charging, the charging boat is of a hollow structure with an opening at the top, the charging container for combustion also comprises a heat insulation material, the hollow structure of the charging boat is filled with a breathable heat insulation material, or the surface of the charging boat is provided with the breathable heat insulation material.
Description
Technical Field
the invention belongs to the technical field of combustion charging, and particularly relates to a charging container for combustion, a charging method thereof and a synthesis method of high α phase silicon nitride.
Background
the method for synthesizing the powder material by using the reaction between the reactants is characterized in that once ignited, the reactants automatically spread to an unreacted area until the reaction is complete, the whole process almost does not need to provide energy, and the reaction is rapid, the synthesis time is short, and the combustion synthesis method has the characteristics of simple combustion synthesis method, low energy consumption, low heat release period, low process cost and the like.
In the technical field of combustion synthesis of silicon nitride powder, a large number of patents and documents have been reported, and the disclosed results all achieve certain technical progress in some aspects, but have a plurality of defects. Patent CN200410029809.3 puts into porous graphite crucible with raw materials powder, burns synthetic reaction, and the aspect of choosing of output powder cost manual work and time more, produces unnecessary waste.
Disclosure of Invention
the technical problem to be solved by the invention is to provide a charging container for combustion and a charging method thereof, and a synthesis method of high α phase silicon nitride, aiming at the defects in the prior art, so that the success rate of ignition is ensured to be more than 99%, the combustion efficiency is high, and the smooth progress of combustion is ensured.
The technical scheme adopted for solving the technical problem of the invention is to provide a charging container for combustion, which comprises: a charge boat for feeding, charge boat are open-topped hollow out construction, and the container of feeding still includes for the burning: the hollow structure of the loading boat is filled with a breathable heat insulation material, or the surface of the loading boat is provided with the breathable heat insulation material.
Preferably, the hollow structure of the loading boat is a woven mesh-shaped hollow structure formed by connecting strip rods in a staggered manner, or hollow structures formed by connecting strip rods arranged in parallel through connecting rods.
Preferably, the gap between two adjacent parallel strip-shaped rods is 5-50 mm.
Preferably, the porosity of the heat insulation material is 30-60%.
Preferably, the heat insulation material is one or more of a polycrystalline fiber blanket, an alumina fiber blanket, a carbon fiber blanket and a ceramic fiber blanket.
Preferably, the loading boat comprises: the side wall rotationally connected with the bottom wall can rotate to enable one end, far away from the side wall, connected with the bottom wall to be not higher than the bottom wall.
Preferably, the loading boat is shaped as a rectangular parallelepiped, and includes: four lateral walls, every lateral wall all rotates with the diapire to be connected, can dismantle between four lateral walls and be connected.
Preferably, the material of the material boat is any one of 304, 304L, 316 and 316L stainless steel.
The present invention also provides a charging method using the above-described charging container for combustion, comprising the steps of:
1) filling a material to be combusted in a charging container;
2) selecting an ignition area in a charging container, digging out materials to be combusted in the ignition area, adding an ignition wire in the ignition area, adding ignition powder which is not filled in the ignition area, and filling the materials to be combusted or composite powder in the ignition area, wherein the composite powder is obtained by mixing the ignition powder dug out of the ignition area with silicon powder with the weight of 1/3-2/3.
The material shovel is used for charging materials into the charging container, and is preferably made of any one of 304 stainless steel, polytetrafluoroethylene, polyurethane and PVC.
Preferably, the ignition wire is any one of copper wire, silver-copper alloy wire, lead-antimony alloy wire and tungsten wire.
Preferably, when the bottom wall of the loading boat is rectangular, the ignition regions in the step 2) are two, wherein the first ignition region is located at 1/3-1/4 edge of the bottom wall in the length direction, and relative to the center of the bottom wall, the second ignition region is in central symmetry with the first ignition region.
Preferably, the thickness of the material to be combusted in the step 1) is 5-8 cm.
Preferably, the material to be combusted includes: 30-65 wt% of silicon powder, 70-20 wt% of diluent and 0-15 wt% of additive;
the ignition powder comprises: one of titanium powder, aluminum powder, magnesium powder, lithium powder and phosphorus powder.
Preferably, the diluent is silicon nitride and the additive is ammonium chloride or ammonium fluoride.
the invention also provides a synthesis method of the high α -phase silicon nitride, which comprises the following steps:
1) the material to be combusted and ignition powder are loaded into a loading container by the loading method, and the loading container is placed in a reaction kettle;
2) introducing nitrogen into the reaction kettle, igniting and burning to obtain the high α phase silicon nitride through synthetic reaction.
Preferably, the method further comprises the step m) of drying the material to be combusted before the step 1), wherein the drying temperature is 80-120 ℃, and the drying time is 2-4 hours.
The charging container for combustion and the charging method thereof ensure that the ignition success rate reaches more than 99 percent, the combustion efficiency is high, the smooth combustion is ensured, the phenomenon of burning interruption is avoided in the spreading process during combustion, the recycling powder quantity is small, and the workload of picking and sorting unburnt materials after combustion is reduced. Meanwhile, the combustion time and the rear-end furnace-discharging powder treatment period are greatly shortened, the dust pollution in the operation process in the prior art is avoided, and the production efficiency is improved.
Drawings
FIG. 1 is a schematic view of the construction of a combustion charging container not filled with a heat insulating material in example 2 of the present invention;
FIG. 2 is a schematic structural view of a combustion charge container filled with an insulating material in example 2 of the present invention;
fig. 3 is a schematic structural view of a combustion charge container with an open side wall in embodiment 2 of the present invention.
In the figure: 1-a loading boat; 2-heat insulation material; 3-a bar-shaped rod; 4-a bottom wall; 5-a side wall; 6-a first ignition region; 7-a second ignition region; 8-connecting rod.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Reference will now be made in detail to embodiments of the present patent, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are exemplary only for the purpose of explaining the present patent and are not to be construed as limiting the present patent.
Example 1
The present embodiment provides a charge container for combustion, including: a charge boat for feeding, charge boat are open-topped hollow out construction, and the container of feeding still includes for the burning: the hollow structure of the loading boat is filled with a breathable heat insulation material, or the surface of the loading boat is provided with the breathable heat insulation material.
The present embodiment provides a charging method using the above-described charging container for combustion, including the steps of:
1) filling the material to be combusted in the charging container;
2) selecting an ignition area in a charging container, digging out materials to be combusted in the ignition area, adding an ignition wire in the ignition area, adding ignition powder which is not filled in the ignition area, and filling the materials to be combusted or composite powder in the ignition area, wherein the composite powder is obtained by mixing the ignition powder dug out of the ignition area with silicon powder with the weight of 1/3-2/3.
the embodiment provides a method for synthesizing high α -phase silicon nitride, which comprises the following steps:
1) the material to be combusted and ignition powder are loaded into a loading container by the loading method, and the loading container is placed in a reaction kettle;
2) introducing nitrogen into the reaction kettle, igniting and burning to obtain the high α phase silicon nitride through synthetic reaction.
The charging container for combustion and the charging method thereof in the embodiment ensure that the ignition success rate reaches more than 99%, the combustion efficiency is high, the smooth combustion is ensured, the phenomenon of burning interruption is avoided in the spreading process during combustion, the recycled powder quantity is small, and the workload of picking and sorting unburnt materials after combustion is reduced. Meanwhile, the combustion time and the rear-end furnace-discharging powder treatment period are greatly shortened, the dust pollution in the operation process in the prior art is avoided, and the production efficiency is improved.
Example 2
As shown in fig. 1 to 3, the present embodiment provides a combustion charge container including: a charge boat 1 for feeding, charge boat 1 is open-topped hollow out construction, and the container of feeding still includes for the combustion: the hollow structure of the loading boat 1 is filled with the air-permeable heat-insulating material 2, or the surface of the loading boat 1 is provided with the air-permeable heat-insulating material 2.
As shown in fig. 1, it should be noted that the hollow structure of the loading boat 1 in this embodiment is formed by connecting bar-shaped rods 3 arranged in parallel with each other through a connecting rod 8.
It should be noted that the gap between two adjacent parallel bar rods 3 in this embodiment is 25 mm.
The porosity of the heat insulating material 2 in this example is 30 to 60%.
As shown in fig. 2, it should be noted that the thermal insulation material 2 in this embodiment is a polycrystalline fiber blanket.
The charge boat 1 in the present embodiment includes: the bottom wall 4, the lateral wall 5 that is connected with bottom wall 4, at least one of them lateral wall 5 is connected with bottom wall 4 rotation, and the lateral wall 5 that is connected with bottom wall 4 rotation makes this lateral wall 5 keep away from its one end that is connected with bottom wall 4 and is not higher than bottom wall 4.
As shown in fig. 3, the charging boat 1 in the present embodiment is a rectangular parallelepiped, and the charging boat 1 includes: four lateral walls 5, every lateral wall 5 all rotates with diapire 4 to be connected, can dismantle between four lateral walls 5 and be connected. In particular, each side wall 5 in this embodiment is coaxially connected to the bottom wall 4, being rotatable through 180 °.
In this embodiment, the material of the loading boat 1 is 304 stainless steel. Specifically, the material of the charge boat 1 in this embodiment is 304 stainless steel.
The present embodiment also provides a charging method using the above-described charging container for combustion, including the steps of:
1) filling a material to be combusted in a charging container;
2) selecting an ignition area in a charging container, digging out materials to be combusted in the ignition area, adding an ignition wire in the ignition area, adding ignition powder which is not filled in the ignition area, and filling the materials to be combusted or composite powder in the ignition area, wherein the composite powder is obtained by mixing the ignition powder dug out of the ignition area with silicon powder with the weight of 1/2 of the ignition powder. Specifically, the ignition wire in this embodiment is wound in a spring shape with a pitch of 5mm, and the ignition wire is connected to the ignition wire.
Specifically, in this embodiment, the material shovel is used to charge the material charging container, and in this embodiment, the material shovel is made of 304 stainless steel.
In this embodiment, the ignition wire is a copper wire.
Preferably, when the bottom wall 4 of the loading boat 1 is rectangular, the ignition regions in step 2) are two, wherein the first ignition region 6 is at 1/4 edge of the bottom wall 4 in the length direction, and the second ignition region 7 is symmetrical to the first ignition region 6 at the center of the bottom wall 4 relative to the center of the bottom wall 4. The first ignition region 6 is: a small pit with a bottom of 10cm by 10cm square and a depth of 5 cm.
Preferably, the thickness of the material to be combusted in the step 1) is 5-8 cm.
Preferably, the material to be combusted includes: 30 wt% of silicon powder and 70 wt% of diluent; the diluent is silicon nitride.
It should be noted that the ignition powder in this embodiment includes: titanium powder.
the embodiment also provides a method for synthesizing high α -phase silicon nitride, which comprises the following steps:
1) placing the material to be combusted in a drying room, wherein the temperature in the drying room is 80-120 ℃, and drying for 2-4 hours;
2) the material to be combusted and the ignition powder are loaded into the charging container by the charging method, and the charging container is placed in the reaction kettle, wherein the thickness of the material to be combusted in the charging container is 5-8 cm, so that on one hand, the phenomenon that the content of α -phase silicon nitride is too low due to overburning caused by over-thick material to be combusted can be avoided, and on the other hand, the phenomenon that the material to be combusted is too thin and is broken to burn and the combustion cannot normally spread can be avoided.
3) introducing nitrogen into the reaction kettle, igniting and burning to obtain the high α phase silicon nitride through synthetic reaction.
The charging method of the charging container for combustion in the embodiment ensures that the ignition success rate is over 99 percent, the combustion efficiency is high, the smooth combustion is ensured, the phenomenon of burning interruption is avoided in the spreading process during combustion, the recycled powder amount is small, and the workload of picking and sorting unburnt materials after combustion is reduced. Meanwhile, the combustion time and the rear-end furnace-discharging powder treatment period are greatly shortened, the dust pollution in the operation process in the prior art is avoided, and the production efficiency is improved.
Example 3
This embodiment provides a combustion charge container, which is different from embodiment 2 in that:
it should be noted that the gap between two adjacent parallel bar bars in this embodiment is 5 mm.
In the present embodiment, the porosity of the thermal insulation material is 30 to 60%.
In this embodiment, the heat insulating material is an alumina fiber mat.
In this embodiment, the material of the loading boat is 316 stainless steel.
The present embodiment also provides a charging method using the above-described charging container for combustion, which is different from the charging method in embodiment 2 in that:
the composite powder in the step 2) is obtained by mixing ignition powder dug out from an ignition area with silicon powder with the weight of 1/3 of that of the ignition powder.
It should be noted that the ignition powder in this embodiment includes: aluminum powder.
It should be noted that, the material shovel in this embodiment is made of PVC.
In the present embodiment, the ignition wire is a silver-copper alloy wire.
It should be noted that the first ignition region is located at 1/7 of the edge of the bottom wall in the length direction in the present embodiment.
It should be noted that, in this embodiment, the material to be combusted includes: 40 wt% of silicon powder, 50 wt% of diluent and 10 wt% of additive; the diluent is silicon nitride and the additive is ammonium chloride.
Example 4
This embodiment provides a combustion charge container, which is different from embodiment 2 in that:
it should be noted that the gap between two adjacent parallel bar bars in this embodiment is 50 mm.
In the present embodiment, the porosity of the thermal insulation material is 30 to 60%.
In this embodiment, the heat insulating material is a carbon fiber felt.
In this example, the material of the loading boat was 316L stainless steel.
The present embodiment also provides a charging method using the above-described charging container for combustion, which is different from the charging method in embodiment 2 in that:
the composite powder in the step 2) is obtained by mixing ignition powder dug out from an ignition area with silicon powder with the weight of 2/3 of that of the ignition powder.
It should be noted that the ignition powder in this embodiment includes: and (3) lithium powder.
In this embodiment, the material shovel is made of polyurethane.
In this embodiment, the material of the shovel is polytetrafluoroethylene.
In the present embodiment, the ignition wire is a lead-antimony alloy wire.
It should be noted that the first ignition region is located at 1/3 edge of the bottom wall in the length direction in the present embodiment.
The additive in this example was ammonium fluoride.
It should be noted that the ignition powder in this embodiment includes: and (4) magnesium powder.
It should be noted that, in this embodiment, the material to be combusted includes: 65 wt% of silicon powder, 20 wt% of diluent and 15 wt% of additive; the diluent is silicon nitride and the additive is ammonium chloride.
Example 5
This embodiment provides a combustion charge container, which is different from embodiment 2 in that:
the hollow structure of the material loading boat is a woven mesh-shaped hollow structure formed by connecting strip-shaped rods in a staggered manner.
In this embodiment, the heat insulating material is a ceramic fiber blanket.
Example 6
The present embodiment provides a charging method using the above-described charging container for combustion, including the steps of:
1) filling a material to be combusted in the charging container in the embodiment 3-5;
2) selecting an ignition area in a charging container, digging out materials to be combusted in the ignition area, adding an ignition wire in the ignition area, adding ignition powder which is not filled in the ignition area, and filling the materials to be combusted or composite powder in the ignition area, wherein the composite powder is obtained by mixing the ignition powder dug out of the ignition area with silicon powder with the weight of 1/3-2/3.
the embodiment provides a method for synthesizing high α -phase silicon nitride, which comprises the following steps:
1) the material to be combusted and ignition powder are loaded into a loading container by the loading method, and the loading container is placed in a reaction kettle;
2) introducing nitrogen into the reaction kettle, igniting and burning to obtain the high α phase silicon nitride through synthetic reaction.
It will be understood that the above embodiments are merely exemplary embodiments taken to illustrate the principles of the present invention, which is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.
Claims (12)
1. A charge container for combustion, comprising: a charge boat for feeding, its characterized in that, charge boat is open-topped hollow out construction, and the container of charging still includes for the burning: the hollow structure of the loading boat is filled with a breathable heat insulation material, or the surface of the loading boat is provided with the breathable heat insulation material.
2. The combustion charging container as set forth in claim 1, wherein the hollowed-out structure of the charging boat is a woven mesh-like hollowed-out structure formed by connecting bar-like rods in a staggered manner, or a hollowed-out structure formed by connecting bar-like rods arranged in parallel with each other through a connecting rod.
3. The combustion charging container according to claim 2, wherein a gap between two adjacent parallel bar-shaped rods is 5 to 50 mm.
4. The combustion charging container according to claim 1, wherein the porosity of the heat insulating material is 30 to 60%.
5. The combustion charging container according to any one of claims 1 to 4, wherein the heat insulating material is one or more of a polycrystalline fiber blanket, an alumina fiber blanket, a carbon fiber blanket, and a ceramic fiber blanket.
6. The combustion charge container as set forth in any one of claims 1 to 4, wherein the charge boat comprises: the side wall rotationally connected with the bottom wall can rotate to enable one end, far away from the side wall, connected with the bottom wall to be not higher than the bottom wall.
7. The combustion charge container as set forth in claim 6, wherein the charge boat is shaped as a rectangular parallelepiped, and the charge boat includes: four lateral walls, every lateral wall all rotates with the diapire to be connected, can dismantle between four lateral walls and be connected.
8. A charging method using the charging container for combustion as set forth in any one of claims 1 to 7, characterized by comprising the steps of:
1) filling a material to be combusted in a charging container;
2) selecting an ignition area in a charging container, digging out materials to be combusted in the ignition area, adding an ignition wire in the ignition area, adding ignition powder which is not filled in the ignition area, and filling the materials to be combusted or composite powder in the ignition area, wherein the composite powder is obtained by mixing the ignition powder dug out of the ignition area with silicon powder with the weight of 1/3-2/3.
9. The method of charging a combustion charge container according to claim 8, wherein the ignition regions in step 2) are two locations when the bottom wall of the charge boat is rectangular, and wherein a first ignition region is located at 1/3 to 1/4 of the edge of the bottom wall in the longitudinal direction, and a second ignition region is located at the center of the bottom wall symmetrically with respect to the center of the bottom wall.
10. The charging method for a combustion charge container as set forth in claim 8, wherein the thickness of the material to be combusted in the step 1) is 5 to 8 cm.
11. The method of charging a combustion charge container according to claim 8, characterized in that said material to be combusted comprises: 30-65 wt% of silicon powder, 70-20 wt% of diluent and 0-15 wt% of additive;
the ignition powder comprises: one of titanium powder, aluminum powder, magnesium powder, lithium powder and phosphorus powder.
12. A method for synthesizing high α phase silicon nitride is characterized by comprising the following steps:
1) charging a material to be combusted and ignition powder into a charging container by the charging method according to any one of claims 8 to 11, and placing the charging container into a reaction kettle;
2) introducing nitrogen into the reaction kettle, igniting and burning to obtain the high α phase silicon nitride through synthetic reaction.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811345840.6A CN111174578A (en) | 2018-11-13 | 2018-11-13 | charging container for combustion, charging method thereof, and method for synthesizing high α phase silicon nitride |
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| CN201811345840.6A CN111174578A (en) | 2018-11-13 | 2018-11-13 | charging container for combustion, charging method thereof, and method for synthesizing high α phase silicon nitride |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS62162608A (en) * | 1986-01-09 | 1987-07-18 | Mitsue Koizumi | Production of silicon nitride fine powder |
| CN1799995A (en) * | 2005-12-21 | 2006-07-12 | 北京科技大学 | Method for synthesizing isotropic silicon nitride powder adopting layer type material-distribution |
| CN102219194A (en) * | 2011-05-16 | 2011-10-19 | 中国科学院唐山高新技术研究与转化中心 | Method for synthesizing silicon nitride or ferro silicon nitride by low-pressure preheating and burning |
| CN202024609U (en) * | 2011-04-20 | 2011-11-02 | 攀钢集团钢铁钒钛股份有限公司 | Material receiving device of high-temperature reduction furnace |
| CN207276201U (en) * | 2017-09-27 | 2018-04-27 | 天津纳德科技有限公司 | Cloth boat for combustion synthesizing high alpha phase silicon nitride powder |
| CN207435325U (en) * | 2017-09-01 | 2018-06-01 | 河南中汇新材科技有限公司 | Silicon nitride production micropore ceramics magazine |
-
2018
- 2018-11-13 CN CN201811345840.6A patent/CN111174578A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62162608A (en) * | 1986-01-09 | 1987-07-18 | Mitsue Koizumi | Production of silicon nitride fine powder |
| CN1799995A (en) * | 2005-12-21 | 2006-07-12 | 北京科技大学 | Method for synthesizing isotropic silicon nitride powder adopting layer type material-distribution |
| CN202024609U (en) * | 2011-04-20 | 2011-11-02 | 攀钢集团钢铁钒钛股份有限公司 | Material receiving device of high-temperature reduction furnace |
| CN102219194A (en) * | 2011-05-16 | 2011-10-19 | 中国科学院唐山高新技术研究与转化中心 | Method for synthesizing silicon nitride or ferro silicon nitride by low-pressure preheating and burning |
| CN207435325U (en) * | 2017-09-01 | 2018-06-01 | 河南中汇新材科技有限公司 | Silicon nitride production micropore ceramics magazine |
| CN207276201U (en) * | 2017-09-27 | 2018-04-27 | 天津纳德科技有限公司 | Cloth boat for combustion synthesizing high alpha phase silicon nitride powder |
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