CN101270959B - Quick reaction synthesis type high temperature atmosphere stove and method for synthesizing ceramic powder - Google Patents

Quick reaction synthesis type high temperature atmosphere stove and method for synthesizing ceramic powder Download PDF

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CN101270959B
CN101270959B CN200710064622A CN200710064622A CN101270959B CN 101270959 B CN101270959 B CN 101270959B CN 200710064622 A CN200710064622 A CN 200710064622A CN 200710064622 A CN200710064622 A CN 200710064622A CN 101270959 B CN101270959 B CN 101270959B
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atmosphere furnace
stove
temperature atmosphere
cold house
valve
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CN101270959A (en
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李江涛
杜吉胜
杨筠
杨术亮
杨坤
候晓奕
林志明
王健力
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Liaoning Jiayi Metals & Minerals Co ltd
Technical Institute of Physics and Chemistry of CAS
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Liaoning Jiayi Metals & Minerals Co ltd
Technical Institute of Physics and Chemistry of CAS
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Abstract

The invention relates to a method to synthesize high-temperature atmosphere furnace and ceramic powder in the way of rapid reaction. A water-cooled flange provided with a water-cooled intermediate separator board at the middle part divides an atmosphere furnace into a high temperature atmosphere furnace and a cold chamber furnace. The high temperature atmosphere furnace is provided with a horizontal heating chamber which is installed on the hearth and which consists of insulation material and heating elements. The heating elements are uniformly distributed on the upper and lower surfaces of the internal walls of the insulation material and connected with the copper electrode installed on the high temperature atmosphere furnace through leads; a heat insulation valve is mounted on the surface of the horizontal heating chamber facing the cold chamber furnace, wherein a fixed track is mounted in the heat insulation valve; the movable track in the cold chamber furnace is connected with the lower push rod in the push rod mechanism, wherein the movable track is provided with a hopper onside, and the hopper is connected with the upper push rod of the push rod mechanism; every furnace is provided with an air inlet and an air outlet with a valve, a vacuum hole and a thermocouple, etc. The invention not only realizes the rapid heating of the materials and the rapid synthesis of the atmosphere, but also realizes the rapid cooling of the products and the even growth of the crystal.

Description

The method of quick reaction synthesis type high temperature atmosphere stove and synthesizing ceramic powder
Technical field
The invention belongs to the Technique for Preparing Ceramic Powders field, the method for particularly a kind of quick reaction synthesis type high temperature atmosphere stove and synthesizing ceramic powder.
Background technology
In the ceramic powder preparation field,, be divided into liquid phase method, vapor phase method and solid phase method at present according to the difference of initiation material state.
Liquid phase method comprises coprecipitation, sol-gal process, microemulsion method and hydro-thermal method etc. again, is the common method of multiple nano-ceramic powders such as preparation oxide, nitride, carbide.The essence of liquid phase method is to adopt performance is controlled on the microcosmic level source material to replace not to be subjected in the traditional handicraft raw material of controls such as how much, chemistry, its principal character shows the following aspects: can accurately control chemical composition, add micro-active ingredient easily, make the nano-powder of multiple uniform component, but liquid phase method need carry out complicated chemosynthesis reaction, in the series of chemical process, unavoidablely with among the impurity substitution product, simultaneously, need take measures to avoid reunion and liquid and solvent pollution on the environment between the particle.
Vapor phase method is meant with the gaseous substance method of prepared in reaction superfine powder at high temperature.Gaseous substance can be that the solid matter heating evaporation generates gas phase, according to the difference of solid matter heating source, is divided into plasma method, laser method etc.; Also can adopt original gaseous feed generation chemical combustion reaction etc.With the plasma method is example, this kind vapor phase method is to adopt the arc evaporation solid material and react with atmosphere to generate needed ceramic powder material, have characteristics such as particle diameter is little, particle diameter is controlled, surface-active is high, output height, but the equipment and technology complexity of this technology, drop into greatlyyer, the industrialized production difficulty is bigger.This also is the ubiquitous problem of vapor phase method.
Solid phase method is that the employing solid matter is the preparation process that initiation material carries out in different heating furnace bodies, heating furnace body is divided into a variety of according to the difference of the difference of its high temperature heat source and mode of operation, comprising resistance furnace, high temperature converter, vacuum furnace etc.Their common characteristic is all to need the reaction raw materials powder is carried out high-temperature heat treatment under vacuum state or atmosphere protection state, and therefore, this The Application of Technology all has very high requirement to reactor material, form, mode of heating and feeding manner.Some conventional vacuum furnaces all can not satisfy the requirement of carrying out the multiple operation operation in a vacuum drying oven at present.
For example, the patent of invention CN1352375A of Li Minzhong, electric resistor heating type super high temperature vacuum sintering furnace is the equipment that satisfies the superhigh temperature sintering process of silicon carbide reaction-sintered goods, though this body of heater can bear high temperature more than 2000 ℃, can't realize the atmosphere protection in the high temperature furnace; Equally, people's such as virgin water light utility model patent CN2391155Y, a kind of device of being made up of vacuum unit, Sealing furnace tank body and burner hearth and heater is provided, this body of heater can be realized the processing request of quick-cooling and quick-warming, but the heater of body of heater is the external-heat burner, is positioned over the burner hearth side, by the connection that communicates with burner hearth of burning levelling chamber, provide in the process of heat in burning like this, impurity can be brought among reactant and the product unavoidablely.Therefore, the existing conventional body of heater can not be when realizing that material Fast Heating and product cool off fast, and many kinds of preparation ceramic powders such as accurate control of taking into account thermal treatment zone atmosphere flow and pressure prepare required technological requirement.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists and a kind of reasonable in design is provided, can satisfy the quick reaction synthesis type high temperature atmosphere stove of special process requirement, and on this body of heater, carry out the preparation of ceramic powder.
Another object of the present invention provides utilizes this quick reaction synthesis type high temperature atmosphere stove to carry out the method for synthesizing ceramic powder.
Quick reaction synthesis type atmosphere furnace of the present invention is made of high-temperature atmosphere furnace and cold house's stove two parts; Its atmosphere furnace is by the water-cooling flange that the centre has a water-cooled median septum described atmosphere furnace to be divided into high-temperature atmosphere furnace and cold house's stove two parts, and high-temperature atmosphere furnace and cold house's stove all have fire door; The one horizontal heating clamber with insulation material and heater element formation that is installed on the siege is being arranged in the high-temperature atmosphere furnace, heater element is evenly distributed on the above and below of insulation material inwall, heater element by lead be installed on the high-temperature atmosphere stove outer covering, have copper electrode in the water cooled electrode that the copper electrode of cooling jacket constitutes be connected (copper electrode adds that outward cooling jacket is collectively referred to as water cooled electrode) by the outside; At horizontal heating clamber heat insulation valve is installed on the front side wall of cold house's stove one side, in horizontal heating clamber, trapped orbit is installed;
In cold house's stove shiftable track is arranged, shiftable track is connected with the lower push-rod of movable transfer bar mechanism on being installed in cold house's fire door, is placed with the material boat on shiftable track, and this material boat links to each other with the upper push-rod of transfer bar mechanism;
All have the air inlet that has valve at the shell of high-temperature atmosphere furnace and the top of cold house's stove outer covering, the bottom all has the gas outlet that has valve; The air inlet of high-temperature atmosphere furnace and cold house's stove all links to each other with the multipath gas mass flow controller, and with the control of components and parts such as electromagnetism charge valve, guarantees stable, the controlled and accurately requirement of supply of gas flow in the synthetic furnace; The bottom is the gas outlet that has valve, is used to guarantee the stable of high-temperature atmosphere furnace and cold house's furnace interior air pressure.Electro connecting pressure gauge is housed on the high-temperature atmosphere furnace, can sees intuitively that the pressure in the stove changed when gas charging system was inflated in stove, and sending pressure signal.
All have vacuum hole in the side of the shell of high-temperature atmosphere furnace and the side of cold house's stove, the pipeline that is connected with pumped vacuum systems is installed at the vacuum hole place; This pumped vacuum systems is made up of sliding vane rotary pump, the manual flapper valve of high vacuum pressure, electromagnetism band venting pressure differential vacuum valve, high vacuum manual diaphragm valve, vacuum ripple pipe and pipeline;
Be equipped with thermometer hole on the shell of high-temperature atmosphere furnace and cold house's stove, at the thermometer hole place thermocouple temperature measurement element be installed, thermocouple links to each other with electric-control system by lead, measures and monitor the environment temperature in horizontal heating clamber and the cold house's stove.
On the fire door of quick reaction synthesis type high temperature atmosphere stove, be provided with the observation fenestra, be used for the observation of course of reaction; The top of high-temperature atmosphere stove outer covering also is provided with heating electrode hole and standby hole, is used for the installation of heating electrode.
The fire door at quick reaction synthesis type high temperature atmosphere stove two ends all adopts the double-layer water jacket structure, the environment temperature around can not influencing.Door opening and closing is manual layback opening structure, and easy to operate, fire door is provided with manual locking device.
The electric-control system of one electrical control cubicles by the transmission hunting respectively with copper electrode, pumped vacuum systems in sliding vane rotary pump, and be installed in thermocouple temperature measurement element on high-temperature atmosphere stove outer covering and the cold house's stove outer covering etc. and link to each other.Can accurately control by the temperature in the horizontal heating clambers of realization such as intelligent, a digital display temperature controller able to programme and silicon controlled crystal brake pipe pressure regulator; and realize technological operations such as vacuumizing in the ceramic powder preparation, Atmosphere Control, reaction mass turnover; take into account many control of guaranteed synthetic furnace safety operation simultaneously, for example the loss protecting of body of heater, overtemperature prote, overpressure protection and input and output material interlock protection etc.
Water-cooled median septum on heat insulation valve, the water-cooling flange, and the transfer bar mechanism on trapped orbit, shiftable track and the cold house's furnace door in the horizontal heating clamber, these assemblies are the key components that realize the quick cooling of the Fast Heating of material and product, also are the important steps that preparation ceramic powder method is implemented.
Described heat insulation valve is pneumatic unlatching, is used to stop that the radiations heat energy of horizontal heating clamber leaks, and the water-cooled median septum is installed on the water-cooling flange, is used to stop the heat of horizontal heating clamber, and cools off cold house's stove simultaneously; Transfer bar mechanism is controlled by Pneumatic control circuit; The material boat that described shiftable track is used between horizontal heating clamber and the cold house's stove is carried.
Described horizontal heating clamber is to adopt heat-resistance stainless steel to do framework, fills high quality carbon felt insulation material in 4 faces of framework up and down, and the back is uncovered, and front (facing to the one side of cold house's stove) is equipped with described heat insulation valve.
Described heater element can adopt three high graphite heaters, high frequency electric source induction coil or HIGH-POWERED MICROWAVES heating source.Can satisfy simultaneously the requirement of 1200 ℃~1600 ℃ of high temperature synthetic reactions.
Described copper electrode is separated by by the high-temperature insulation ceramic member and is installed on the high-temperature atmosphere stove outer covering.
The bottom of described shiftable track leads to cooling water, is used for directly conduction cooling shiftable track.
Quick reaction synthesis type high temperature atmosphere stove of the present invention is used for the method for synthesizing ceramic powder, may further comprise the steps:
(1). pretreated reaction raw materials is put into the material boat, open the fire door of cold house's stove one end, be placed on the shiftable track, shiftable track is closed fire door with after the upper push-rod of transfer bar mechanism is connected, at this moment, heat insulation valve closing;
(2). start pumped vacuum systems, press the sliding vane rotary pump button, the sliding vane rotary pump running; Manual unlocking is taken out valve in advance, and high-temperature atmosphere furnace and cold house's stove and loading line are vacuumized, and according to the requirement of reaction system, is evacuated to high-temperature atmosphere furnace and cold house's furnace pressure all to 10~10 -3Pa, pumped vacuum systems out of service;
(3). start gas charging system: clap vacuum continuously after 5~10 minutes, guarantee noresidue air in the gas charging system, close and take out valve in advance; Take out in advance valve close put in place after, manually open charge valve gradually, regulate the size of air inflow, requirement according to reaction system, fill reaction gas or protection gas in high-temperature atmosphere furnace and cold house's stove, high-temperature atmosphere furnace is worked as in observation and cold house's furnace pressure reaches requirement, the manual-lock charge valve;
(4). heating system starts: open the cooling water control valve, cooling water feeds water cooled electrode and water-cooling flange; On temperature controller, set heating schedule before the reaction, start heating schedule; Heating process is carried out automatically according to the curve of input in advance, and the heater element heating makes horizontal heating clamber begin to heat up, and the temperature control instrument displays temperature on the switch board changes, and waiting temperature reaches technological requirement;
(5). charging starts: start air compressor, pneumatic control is prepared; Open pneumatic operated valve, open heat insulation valve, open transfer bar mechanism, start lower push-rod earlier, promote the shiftable track motion, enter horizontal heating clamber, be connected with trapped orbit in the horizontal heating clamber; Then start the upper push-rod motion of transfer bar mechanism, promote the material boat and move in orbit, enter horizontal heating clamber; Lower push-rod counter motion subsequently, the pulling shiftable track is got back to cold house's stove, closes heat insulation valve at last, and pyroreaction begins.Question response is opened pneumatic operated valve after finishing, and opens heat insulation valve, starts the lower push-rod of transfer bar mechanism, and shiftable track is pushed horizontal heating clamber, is connected with trapped orbit; Then start upper push-rod, will expect that boat shifts out horizontal heating clamber, enter cold house's stove, the high temperature synthetic reaction finishes, and stops heating system, continues logical cooling water 30~90 minutes, treat that water cooled electrode and water-cooling flange drop to preference temperature after, close cooling water.
Compared with prior art, the invention has the advantages that:
1. reaction mass can carry out the high temperature synthetic reaction of Fast Heating, has avoided the accessory substance that is generated with in the stove temperature-rise period;
2. material is heated evenly in body of heater in the course of reaction, has guaranteed carrying out fully of synthetic reaction;
3. the synthetic product of high temperature can leave the high-temperature region fast, and realizes cooling fast, has improved the quality of product greatly.
4. synthetic furnace atmosphere is controlled, can realize the high temperature synthetic reaction of different systems, and preparation comprises the multiple high-quality ceramic powder of carbide, nitride, oxide.
Description of drawings
Fig. 1. the front view of quick reaction synthesis type high temperature atmosphere stove of the present invention.
Fig. 2. the side view of quick reaction synthesis type high temperature atmosphere stove of the present invention.
Fig. 3. the SEM photo of the SiC powder for preparing in the embodiment of the invention.
Reference numeral
1. high-temperature atmosphere furnace 2. horizontal heating clamber 3. sieges
4. heat insulation valve 5. cold house's stoves 6. shiftable tracks
7. transfer bar mechanism 8. water cooled electrodes 9. pumped vacuum systems
10. gas outlet 11. bases 12. water-cooling flanges
The specific embodiment
Further specify quick reaction synthesis type high temperature atmosphere stove of the present invention below in conjunction with drawings and Examples, and utilize this quick reaction synthesis type high temperature atmosphere stove to prepare the method for SiC ceramic powder.
Embodiment 1.
See also Fig. 1 and Fig. 2.One atmosphere furnace that is seated on the base 11 is divided into high-temperature atmosphere furnace 1 and cold house's stove 5 two parts by a middle water-cooling flange 12 that has the water-cooled median septum, and high-temperature atmosphere furnace and cold house's stove all have fire door; In that being arranged in the high-temperature atmosphere furnace, an employing heat-resistance stainless steel that is installed on the siege 3 does framework, in 4 faces of framework up and down, fill high quality carbon felt insulation material, the back is uncovered, the front is equipped with the horizontal heating clamber 2 of heat insulation valve, on the inwall of the insulation material of above and below, be uniform-distribution with heater element, heater element by lead be installed on the high-temperature atmosphere stove outer covering 1, the copper electrode that is had in the water cooled electrode 8 that the copper electrode of cooling jacket constitutes by the outside is connected; At horizontal heating clamber 2 heat insulation valve 4 is installed on the front side wall of cold house's stove one side, in horizontal heating clamber 2, trapped orbit is installed;
Shiftable track 6 is arranged in cold house's stove, and shiftable track 6 is connected with the lower push-rod of movable transfer bar mechanism 7 on being installed in cold house's fire door, is placed with the material boat on shiftable track 6, and this material boat links to each other with the upper push-rod of transfer bar mechanism 7;
All have the air inlet that has valve at the shell 1 of high-temperature atmosphere furnace and the top of cold house's stove outer covering 5, the bottom all has the gas outlet 10 that has valve; All have vacuum hole in the side of the shell of high-temperature atmosphere furnace and the side of cold house's stove outer covering, the pipeline that is connected with pumped vacuum systems 9 is installed at the vacuum hole place; This pumped vacuum systems is made up of sliding vane rotary pump, the manual flapper valve of high vacuum pressure, electromagnetism band venting pressure differential vacuum valve, high vacuum manual diaphragm valve, vacuum ripple pipe and pipeline;
Be equipped with thermometer hole on the shell of high-temperature atmosphere furnace and the cold house's stove, the thermocouple temperature measurement element be installed at the thermometer hole place;
On the fire door of quick reaction synthesis type high temperature atmosphere stove, be provided with the observation fenestra, be used for the observation of course of reaction.
The electric-control system of one electrical control cubicles is respectively by the sliding vane rotary pump in transfer wire and copper electrode, the pumped vacuum systems 9, and is installed in the shell 1 of high-temperature atmosphere furnace and the thermocouple temperature measurement element on cold house's stove 5 etc. and links to each other.
Described heater element can adopt three high graphite heaters, high frequency electric source induction coil or HIGH-POWERED MICROWAVES heating source, to satisfy the requirement of 1200 ℃~1600 ℃ of high temperature synthetic reactions.
Described copper electrode is separated by by the high-temperature insulation ceramic member and is installed on the high-temperature atmosphere stove outer covering 1.
The bottom of described shiftable track 6 leads to cooling water, is used for directly conduction cooling shiftable track.
(1). pretreated reaction raw materials Si powder and C powder are put into the material boat in proportion, open the fire door of cold house's stove 5 one ends, be placed on the shiftable track 6, shiftable track 6 is closed fire door with after the upper push-rod of transfer bar mechanism 7 is connected, and at this moment, heat insulation valve 4 is closed;
(2). start pumped vacuum systems 9, press the sliding vane rotary pump button, the sliding vane rotary pump running; Manual unlocking is taken out valve in advance, and high-temperature atmosphere furnace and cold house's stove and loading line are vacuumized, and according to the requirement of reaction system, is evacuated to high-temperature atmosphere furnace and cold house's furnace pressure all to 10Pa, pumped vacuum systems 9 out of service;
(3). start gas charging system 10: after vacuumizing 5 minutes continuously, close and take out valve in advance; Take out in advance valve close put in place after, manually open charge valve gradually, charge into inert protective gas Ar gas or inert mixed gas, observe when furnace pressure and reach 5 * 10 4~1.013 * 10 5Behind the Pa, the manual-lock charge valve;
(4). heating system starts: open the cooling water control valve, cooling water feeds water cooled electrode 8 and water-cooling flange 12; On temperature controller, set heating schedule before the reaction, start heating schedule; Heating process is carried out automatically according to the curve of input in advance, and the heater element heating makes horizontal heating clamber 2 begin to heat up, and waiting temperature reaches 1200~1500 ℃;
(5). charging starts: start air compressor, pneumatic control is prepared; Open pneumatic operated valve, open heat insulation valve 4, open transfer bar mechanism 7, start lower push-rod earlier, promote shiftable track 6 motions, enter horizontal heating clamber 2, be connected with trapped orbit in the horizontal heating clamber 2; Then start the upper push-rod motion of transfer bar mechanism 7, promote the material boat and move in orbit, enter horizontal heating clamber 2; Lower push-rod counter motion subsequently, pulling shiftable track 6 is got back to cold house's stove, closes heat insulation valve 4 at last, and pyroreaction begins.Question response is opened pneumatic operated valve after finishing, and opens heat insulation valve 4, starts the lower push-rod of transfer bar mechanism 7, and shiftable track 6 is pushed horizontal heating clamber 2, is connected with trapped orbit; Then start upper push-rod, will expect that boat shifts out horizontal heating clamber 2, enter cold house's stove, the high temperature synthetic reaction finishes, and stops heating system, continues logical cooling water 90 minutes, after treating water cooled electrode 8, water-cooling flange 12 and expecting that boat drops to preference temperature, closes cooling water.Open the fire door of cold house's one end, take out the boat material, product is carried out XRD analysis with Japan's D/MAX-IIB type X-ray diffraction analyzer of science, and test result shows, for purity greater than 98% sub-micron SiC powder, the SEM photo of the SiC powder of preparation is as shown in Figure 3.

Claims (9)

1. quick reaction synthesis type atmosphere furnace, this atmosphere furnace is made of high-temperature atmosphere furnace and cold house's stove two parts; It is characterized in that: the water-cooling flange that is had the water-cooled median septum by the centre is divided into high-temperature atmosphere furnace and cold house's stove two parts with described atmosphere furnace, and high-temperature atmosphere furnace and cold house's stove all have fire door; The one horizontal heating clamber with insulation material and heater element formation that is installed on the siege is being arranged in the high-temperature atmosphere furnace, heater element is evenly distributed on the above and below of insulation material inwall, heater element by lead be installed on the high-temperature atmosphere stove outer covering, the copper electrode that is had in the water cooled electrode that the copper electrode of cooling jacket constitutes by the outside is connected; At horizontal heating clamber heat insulation valve is installed on the front side wall of cold house's stove one side, in horizontal heating clamber, trapped orbit is installed;
In cold house's stove shiftable track is arranged, shiftable track is connected with the lower push-rod of movable transfer bar mechanism on being installed in cold house's fire door, is placed with the material boat on shiftable track, and this material boat links to each other with the upper push-rod of transfer bar mechanism;
All have the air inlet that has valve at the shell of high-temperature atmosphere furnace and the top of cold house's stove outer covering, the bottom all has the gas outlet that has valve; The air inlet of high-temperature atmosphere furnace and cold house's stove all links to each other with the multipath gas mass flow controller;
On the shell of the shell of high-temperature atmosphere furnace and cold house's stove, all have vacuum hole, the pipeline that is connected with pumped vacuum systems is installed at the vacuum hole place;
On the shell of high-temperature atmosphere furnace and cold house's stove outer covering, be equipped with thermometer hole, the thermocouple temperature measurement element be installed at the thermometer hole place;
The electric-control system of one electrical control cubicles by transfer wire respectively with copper electrode, pumped vacuum systems in sliding vane rotary pump, and the thermocouple temperature measurement element that is installed on high-temperature atmosphere stove outer covering and the cold house's stove outer covering links to each other.
2. quick reaction synthesis type atmosphere furnace according to claim 1 is characterized in that: the fire door of described quick reaction synthesis type atmosphere furnace is provided with the observation fenestra.
3. quick reaction synthesis type atmosphere furnace according to claim 1 is characterized in that: the top of described high-temperature atmosphere stove outer covering is provided with heating electrode hole and standby hole.
4. quick reaction synthesis type atmosphere furnace according to claim 1, it is characterized in that: described horizontal heating clamber is to adopt heat-resistance stainless steel to do framework, fill carbon felt insulation material in 4 faces of framework up and down, the back is uncovered, and the front is equipped with described heat insulation valve.
5. quick reaction synthesis type atmosphere furnace according to claim 1 is characterized in that: described heater element is three high graphite heaters, high frequency electric source induction coil or HIGH-POWERED MICROWAVES heating source.
6. quick reaction synthesis type atmosphere furnace according to claim 1 is characterized in that: the bottom of described shiftable track leads to cooling water, is used for directly conduction cooling shiftable track.
7. according to claim 1,2 or 3 described quick reaction synthesis type atmosphere furnace, it is characterized in that: on the described high-temperature atmosphere furnace electro connecting pressure gauge is housed.
8. quick reaction synthesis type atmosphere furnace according to claim 1 is characterized in that: described copper electrode is separated by by the high-temperature insulation ceramic member and is installed on the high-temperature atmosphere stove outer covering.
9. a quick reaction synthesis type atmosphere furnace according to claim 1 is used for the method for synthesizing ceramic powder, it is characterized in that this method may further comprise the steps:
(1). pretreated reaction raw materials is put into the material boat, open the fire door of cold house's stove one end, be placed on the shiftable track, shiftable track is closed fire door with after the upper push-rod of transfer bar mechanism is connected, at this moment, heat insulation valve closing;
(2). start pumped vacuum systems, open and take out valve in advance, high-temperature atmosphere furnace and cold house's stove and loading line are vacuumized, be evacuated to high-temperature atmosphere furnace and cold house's furnace pressure all to 10~10 -3Pa, pumped vacuum systems out of service;
(3). start gas charging system: vacuumize continuously, guarantee noresidue air in the gas charging system, close and take out valve in advance; Open charge valve, in high-temperature atmosphere furnace and cold house's stove, fill reaction gas or protection gas,, close charge valve when high-temperature atmosphere furnace and cold house's furnace pressure reach requirement;
(4). heating system starts: open the cooling water control valve, cooling water feeds water cooled electrode and water-cooling flange; Start heating schedule, the heater element heating makes horizontal heating clamber begin to be warming up to temperature and reaches technological requirement;
(5). charging starts: open pneumatic operated valve, open heat insulation valve, open transfer bar mechanism, start lower push-rod earlier, promote the shiftable track motion, enter horizontal heating clamber, be connected with trapped orbit in the horizontal heating clamber; Then start the upper push-rod motion of transfer bar mechanism, promote the material boat and move in orbit, enter horizontal heating clamber; Lower push-rod counter motion subsequently, the pulling shiftable track is got back to cold house's stove, closes heat insulation valve at last, and pyroreaction begins; Question response is opened pneumatic operated valve after finishing, and opens heat insulation valve, starts the lower push-rod of transfer bar mechanism, and shiftable track is pushed horizontal heating clamber, is connected with trapped orbit; Then start upper push-rod, will expect that boat shifts out horizontal heating clamber, enter cold house's stove, the high temperature synthetic reaction finishes, and stops heating system, continues logical cooling water, treat that water cooled electrode and water-cooling flange drop to preference temperature after, close cooling water.
CN200710064622A 2007-03-21 2007-03-21 Quick reaction synthesis type high temperature atmosphere stove and method for synthesizing ceramic powder Expired - Fee Related CN101270959B (en)

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