CN104105239B - Microwave heating equipment and microwave heating method - Google Patents
Microwave heating equipment and microwave heating method Download PDFInfo
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- CN104105239B CN104105239B CN201410100661.1A CN201410100661A CN104105239B CN 104105239 B CN104105239 B CN 104105239B CN 201410100661 A CN201410100661 A CN 201410100661A CN 104105239 B CN104105239 B CN 104105239B
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Abstract
The object of the present invention is to provide and a kind ofly can reduce the damage that causes because of heat and heat microwave heating equipment and the microwave heating method of desired treated object simultaneously.The feature of microwave heating equipment involved in the present invention is to possess: for keeping the cylinder of treated object; To the microwave applicator of described cylinder internal radiation microwave; Make the whirligig of described drum rotating; Be arranged on the stirring piece in described cylinder; To the cooling device that described cylinder cools.
Description
Technical field
The present invention relates to microwave heating equipment and microwave heating method.
Background technology
Microwave heating technique is as the technology of heated food and development.Microwave heating, compared with the common heating undertaken by infrared ray, hot blast etc., has as inferior feature:
■ optionally can heat the material easily absorbing microwave;
The ■ efficiency of heating surface is high, and heating time is short.
At present, owing to having above-mentioned such feature, microwave heating technique is industrially applied to the field widely such as the sintering of drying, sterilization, pottery etc., the synthesis of macromolecular material of timber etc.Wherein, the example be used in the burning disposal of discarded object is described (such as with reference to patent documentation 1) microwave heating equipment.
Fig. 5 is the key diagram of the structure of the microwave heating equipment represented described in patent documentation 1.The barrel 10 and backing roll 11 that can rotate is provided with in shell 2.The inner side of barrel 10 is provided with multi-disc stirring vane 19, the discarded object 40 put in barrel 10 is stirred.Be connected with suction mechanism 31 in the bottom of shell 2, be connected with waste gas cleaning mechanism 35 on the top of shell 2.The microwave irradiation radiated from magnetron 21 is to the discarded object 40 in barrel 10.Thus can heat waste 40.
[patent documentation 1] Japanese Unexamined Patent Publication 2004-No. 183989 publications
But, when treated object is the mixture being difficult to absorb the material of microwave and the material of easy absorption microwave, is desirably in and the material combustion only making easily to absorb microwave when fire damage is not caused to the material being difficult to absorb microwave.
But, in device in the past, there is following problem: the heat from the material easily absorbing microwave is conducted to the material being difficult to absorb microwave by heat transfer, and causes fire damage to the material being difficult to absorb microwave.
Summary of the invention
The present invention, for solving above-mentioned problem, its object is to provide the microwave heating equipment of fire damage and the microwave heating method of a kind of minimizing to being difficult to the material absorbing microwave.
To achieve these goals, the feature of microwave heating equipment of the present invention is to possess: for keeping the cylinder of treated object; To the microwave applicator of described cylinder internal radiation microwave; Make the whirligig of described drum rotating; Be arranged on the stirring piece in described cylinder; To the cooling device that described cylinder cools.
In addition, microwave heating method of the present invention, by heating described treated object to the treated object irradiating microwaves in stirring in cylinder, is characterized in that, cools described cylinder while irradiating microwaves.
[invention effect]
As mentioned above, according to the present invention, the temperature of treated object can be suppressed to rise, reduce the phenomenon producing fire damage in treated object.
Accompanying drawing explanation
Fig. 1 is the process chart representing silicon reutilization system.
Fig. 2 is the generalized section of the microwave heating equipment involved by execution mode 1.
Fig. 3 is the cylinder schematic diagram of the microwave heating equipment involved by execution mode 1.
Fig. 4 is the cutaway view of the microwave heating equipment involved by other example of execution mode 1.
Fig. 5 is the key diagram of the structure of the microwave heating equipment represented described in patent documentation 1.
[symbol description]
100,101 microwave heating equipments
300 microwave generators
310 tuners
320 waveguide pipe
330 metal chambers
340 rotating mechanisms
350 cylinders
360 silicon mud
370 stirring pieces
380 cooling devices
390 water cooling tubes
391 air cooling mechanisms
400 air entries
410 exhaust outlets
420 thermometers
430 control parts
Embodiment
Below, with reference to accompanying drawing, embodiments of the present invention are described.
(execution mode 1)
As the accessory substance of the manufacturing process of silicon for solar cell wafer, generate mixture and the silicon mud of silicon, water and carbon.Silicon is the material being difficult to absorb microwave, and water and carbon are the materials easily absorbing microwave.Therefore, if the removing of moisture and the selective combustion of carbon can be realized when not causing when fire damage the silicon in silicon mud, the recycling silicon of high-quality can so be obtained.
When having irradiated microwave to silicon mud, although the silicon being difficult to absorb microwave is not easy to be heated because of microwave itself, owing to absorbing the water of microwave, the heat transfer of carbon from easy, the temperature of silicon rises sometimes.On the other hand, the microwave heating equipment involved by present embodiment optionally can only heat the material easily absorbing microwave while suppressing the fire damage of the material being difficult to absorption microwave.Therefore, this microwave heating equipment is useful for obtaining recycling silicon from silicon mud.Below, the example being applicable to the operation obtaining recycling silicon from silicon mud is used to be described this microwave heating equipment.
First, the wafer fabrication sequence of Fig. 1 to silicon for solar cell is used to be described.At first, in silicon materials preparatory process (S110), prepare the few initial silicon of impurity, next, make in operation (S120) at silicon ingot and make silicon ingot.Silicon ingot is made by cutting krousky (CZ) method etc.In silicon ingot processing, bonding process (S130), the silicon ingot made is processed, this silicon ingot is bonded and fixed to beam.In slice processing operation (S140), use scroll saw to carry out slice processing to the silicon ingot be adhesively fixed on beam.Then, silicon for solar cell wafer is produced via wafer cleaning operation (S150).
Next, silicon recycling operation (S200) is described.Silicon recycling operation (S200) refers to, the silicon mud that will generate as accessory substance in slice processing operation (S140) is separated by separation, recovery process (S210), is reclaimed, and via carbon, moisture removal step (S220), melting, solidify operation (S230) and make recycling silicon, then return a series of operation that silicon ingot makes operation (S120).
In slice processing operation (S140), to silicon ingot add man-hour produce silicon chip be bonded with the beam material of silicon ingot, the water containing cooling fluid (organic system) mixes and discharges in large quantities as silicon mud.Being separated, such as filter press is utilized in recovery process (S210) to carry out being separated of solid state component and liquid component, recovery to this silicon mud.The solid state component of the silicon mud after separation is recovered as the silicon mud of powdery.The DIC composition of the residue such as organic carbon constituents, the graphite as the material of beam, the abrasive particle as diamond fretsaw containing residual cooling fluid composition in the silicon mud of this powdery.Contained organic carbon component, inorganic carbon component are about the 7at% of the silicon mud entirety of powdery.The moisture containing ratio of the silicon mud of powdery is about 50% ~ 60% of entirety.
The silicon mud of the powdery after reclaiming is imported microwave heating equipment involved by present embodiment as treated object, carries out heat treated about a few minutes to dozens of minutes to implement carbon, moisture removal step (S220).By suppressing the oxidation of silicon and remove carbon component and moisture in this operation simultaneously, thus the high and recycling silicon that fire damage is low of purity can be obtained.
At this, the details of Fig. 2 to the microwave heating equipment 100 involved by present embodiment is used to be described.
Microwave heating equipment 100 possesses microwave generator 300, tuner 310, waveguide pipe 320, metal chamber 330, for keeping the cylinder 350 of treated object (silicon mud 360), the rotating mechanism 340 as the whirligig of cylinder 350, the stirring piece 370 for stir silicon mud 360, has cooling device 380 to the water cooling tube 390 that cylinder 350 cools.In addition, microwave heating equipment 100 possesses the thermometer 420 of the air entry 400 air or gas being taken into metal chamber 330, the exhaust outlet 410 be exhausted, measurement temperature.
Metal chamber 330 is arranged from the tilt mode of 30 ° of horizontal direction with central shaft, thus easily stirs treated object.Be provided with in the inside of metal chamber 330 and rotate and by the metal cylinder 350 of thermal endurance to paper depth direction under the effect of rotating mechanism 340.
The microwave produced by microwave generator 300 is irradiated to the silicon mud 360 remained in cylinder 350 by waveguide pipe 320.At this, as an example of microwave applicator, enumerate the device of combination microwave generator 300, tuner 310, waveguide pipe 320.
The lower surface of metal chamber 330 is provided with the air entry 400 from air introduction air.The exhaust outlet 410 of being discharged by the gas produced when the steam produced when heating silicon mud 360 or carbon burning is provided with at the upper surface of metal chamber 330.The flow adjustment of inspiratory capacity, discharge rate can be carried out by air entry 400 and exhaust outlet 410.
At this, the details of cylinder 350 is described.Fig. 3 (a) is from generalized section during horizontal observation cylinder 350, and (b) is the schematic diagram after being amplified by the opening of cylinder 350.Be provided with stirring piece 370 abreast at the medial surface of cylinder 350 and the rotating shaft of cylinder 350, become the structure that can be stirred treated object by swing roller 350.Stirring piece 370 is made up of the metal with thermal endurance, can enumerate stainless plate as an example.At this, show following state: about 3/4 times of the degree of depth that the degree of depth (depth) of stirring piece 370 is cylinder 350, about 1/8 times of the diameter that the height (height from the medial surface of cylinder 350) of stirring piece 370 is cylinder 350, and stirring piece 370 is provided with 4 at the medial surface of cylinder 350 in the mode being positioned at cross direction.This configuration can reduce not to the shaded portions of treated object irradiating microwaves, is therefore useful for carrying out uniform process.Due to metal stirring piece 370 blocking microwave, easily produce shaded portions, therefore can reduce shaded portions as much as possible as above-mentioned configuration like this.
Treated object can be stirred efficiently by this stirring piece 370, even the different powder of particle diameter is treated object, also can not only stir at the direction of rotation of cylinder 350 (depth direction in figure), can also stir at opening and direction, inner portion (left and right directions in figure).
It should be noted that, preferred stirring piece 370 by quartz such there is thermal endurance and the material of microwave transmissive is formed.This is because, if form stirring piece 370 by the material of microwave transmissive, then can not be formed not to the shaded portions of treated object irradiating microwaves, can treatment effeciency be improved.
In addition, be provided with by plated water cooling tube 390 (magnetism servo-electric motor water-cooling) in the madial wall of cylinder 350, the inner side of stirring piece 370.That is, cooling device 380 (Fig. 2) has the magnetism servo-electric motor water-cooling carrying out cooling and stirring sheet 370 by cooling fluid.By making cooling fluid flow in water cooling tube 390, thus can the inner side of chilling roll 350 and stirring piece 370.Thereby, it is possible near the central authorities of the cylinder 350 that chilling temperature is the highest effectively, improve the cooling effectiveness of treated object.And then the chance contacted with treated object due to stirring piece 370 is more, therefore, it is possible to more efficiently cool treated object.It should be noted that, can suitable water or grease etc. as cooling fluid.
In the present embodiment, in order to suppress paradoxical discharge, the localized heating during microwave heating of the silicon mud 360 of Fig. 2, by machine for decomposing and smashing, silicon mud 360 is processed into the shot-like particle of below 5mm.This silicon mud 360 of a few kg is imported cylinder 350, by rotating mechanism 340, cylinder 350 is rotated with 3 ~ 20rpm.
Control part 430 is possessed in microwave heating equipment 100.Control part 430 is computer.Control part 430 carries out the drived control of rotating mechanism 340.And then, control part 430 with when microwave irradiation also to the mode controlled cooling model device 380 that cylinder 350 cools.Further, control part 430 is connected with microwave generator 300, (radiation) thermometer 420, with the mode controlled cooling model device 380 and the microwave generator 300 that make the surface temperature of the silicon mud 360 in process become less than 600 DEG C.The surface temperature of silicon mud 360 is measured by thermometer 420.This surface temperature is different from the temperature of the part that silicon mud 360 at utmost heats up by microwave heating (core).When the temperature of the part at utmost heated up rises to about 900 DEG C, the oxidation reaction aggravation of silicon, is unsuitable for silicon recycling.Experiment as a result, discoveries such as inventors, if surface temperature is remained on less than 600 DEG C, then can suppress the oxidation of the silicon in silicon mud 360.
At this, the carbon of Fig. 1, moisture removal step (S220) are described in detail.
In carbon, moisture removal step (S220), while the cooling of cylinder 350 inside carrying out Fig. 2, irradiate the microwave of such as about 3 ~ 9kW to silicon mud 360.So the organic carbon component in silicon mud 360, inorganic carbon component, moisture absorption microwave and being heated, first, produce steam, and the steam produced is discharged to metal chamber 330 from exhaust outlet 410.Then, become organic carbon component at higher temperature, the evaporation of inorganic carbon component or with the oxygen generation combustion reaction in air, produce organic system gas or CO
2.The organic system gas produced or CO
2also discharge from exhaust outlet 410.So, by prolonged exposure microwave, the moisture concentration in silicon mud 360, concentration of carbon are reduced.By carrying out the irradiation of the microwave of a few minutes, thus the moisture concentration in silicon mud 360 can be made to be reduced to such as less than 1.5%, and concentration of carbon can be made to be reduced to such as about 0.1at%.
Originally, because silica flour is difficult to absorb the material of microwave, be thus difficult to directly be heated by microwave, but due to the heat transfer of the carbon from high temperature, and the temperature of silicon may be made to increase.When applying heat to silicon, existence rotten (rising because being oxidized the oxygen concentration caused) and damage are accumulated and are made the situation that the quality of recycling silicon reduces.Therefore, in the present embodiment, in order to prevent the temperature of silicon from rising, while cooling the inner side of cylinder 350 and stirring piece 370, by the moisture in silicon mud 360, carbon burning removing.Thereby, it is possible to suppress the temperature of silicon to rise, the rotten of silicon and fire damage can be reduced.
It should be noted that, be preferably configured to the conductive coefficient of conductive coefficient lower than inner side in the outside of cylinder 350.More specifically, preferably adopt and use thermal endurance high in the inner side of cylinder 350 and the material that conductive coefficient is high (such as, stainless steel and other metal materials, or conductive coefficient is 15Wm
-1k
-1above and 500Wm
-1k
-1following material), to use in outside and be difficult to absorb microwave and the such double-decker of the low material (such as quartz, zirconia, refractory plate etc.) of conductive coefficient.Particularly, the conductive coefficient of the inner side of preferred cylinder 350 is more than 2 times of conductive coefficient of outside and less than 100 times.By making the conductive coefficient of the inner side of cylinder 350 be more than 2 times of conductive coefficient in outside, thus the temperature of the metal chamber 330 surrounding cylinder 350 can also be suppressed to rise.If temperature rises, then metal may become and easily absorb microwave, but by suppressing the temperature of metal chamber 330 to rise, and can reduce the energy of the microwave absorbed by metal chamber 330 thus.In addition, owing to using different materials in the inner side and outer side of cylinder 350, the processing that (side of cylinder 350) imbeds water cooling tube 390 therefore between which also becomes easy, can easily make cylinder 350.By cooling device 380 being imbedded the side of cylinder 350, cooling can be implemented efficiently.
In addition, microwave heating treatment also can under reduced pressure be implemented.And then, also can to oxygen gas-supplying in metal chamber 330 and the mist of inactive gas (nitrogen, argon gas etc.) or the mist etc. of hydrogen and inactive gas.Thereby, it is possible to suppress the oxidation of silicon.
It should be noted that, this microwave heating equipment also goes for the mud produced when substrate manufactures such as sapphire substrate, gallium nitride (GaN) substrate, GaAs (GaAs) substrates.In these mud, also comprise the material easily absorbing microwave and the material being difficult to absorb microwave, this microwave heating equipment can perform microwave heating treatment while not causing fire damage to the material being difficult to absorb microwave.
It should be noted that, the material (the first material) easily absorbing microwave represents polar substances, dielectric loss angle (Tan δ) be more than 0.01 material or conductance be 10
-2above and 10
4any one material in following material.And, be difficult to absorb microwave material (the second material) represent with polar substances, dielectric loss angle Tan δ be more than 0.01 material or conductance be 10
-2above and 10
4any one all different material in following material.Comprise above-mentioned the first material of any one and the treated object of this two side of the second material is suitable for being processed by the microwave heating equipment 100 involved by present embodiment.In this case, the first material can be heated when not causing when fire damage the second material.
At this, Fig. 4 is used to be described the microwave heating equipment 101 involved by other example of present embodiment.In the diagram, identical with Fig. 2 inscape uses prosign and omits the description.Be with the difference of Fig. 2, cooling device 380 has the air cooling mechanism 391 of spraying refrigerating gas to cylinder 350.Air cooling mechanism 391 is formed through and imports cooled refrigerating gas from air entry 400 and be sprayed onto the lateral surface of cylinder 350, thus to the structure that the cylinder 350 in microwave irradiation cools.It should be noted that, sometimes also by illustrate in fig. 2 come the mechanism of chilling roll 350 by cooling fluid and water cooling tube 390 is recited as magnetism servo-electric motor water-cooling.Refrigerating gas uses oxygen or their mist of the burning of air, inactive gas, promotion carbon.
With regard to magnetism servo-electric motor water-cooling, cooling effectiveness is high, and accurately can carry out temperature control, is therefore applicable to make to want the material heated become the situation of high temperature (more than 600 DEG C) or do not want the situation etc. of the temperature of doing one's utmost ground elevated material.But, in order to arrange magnetism servo-electric motor water-cooling in cylinder 350, make complex structureization thus manufacturing cost rising.On the other hand, with regard to air cooling mechanism 391, although cooling effectiveness declines compared with magnetism servo-electric motor water-cooling, the structure of cylinder 350 can be simplified, can also manufacturing cost be suppressed low.Therefore, air cooling mechanism 391 is applicable to the situation wanting treated substance in temperature lower below 600 DEG C.
But, preferably magnetism servo-electric motor water-cooling and air cooling mechanism 391 are combined configuration.That is, preferred cooling device 380 also has air cooling mechanism 391 except having magnetism servo-electric motor water-cooling (water cooling tube 390).Thereby, it is possible to raising cooling effectiveness, therefore, it is possible to the temperature of doing one's utmost to suppress to be difficult to the material absorbing microwave rises.In addition, due to the temperature of metal chamber 330 entirety can also be reduced, therefore can also reduce the microwave absorbed by metal chamber 330, treated object can be heated efficiently.
And then, control by two systems (magnetism servo-electric motor water-cooling and the air cooling mechanism 391) cooling body utilizing control part 430 pairs of cooling devices 380 to possess, thus quick cooling can be realized.Specifically, either party making in magnetism servo-electric motor water-cooling or air cooling mechanism 391 while making the microwave irradiation silicon mud 360 from microwave generator 300 cools.In this case, control part 430 controls microwave generator 300 and cooling device 380 in the mode making the surface temperature of silicon mud 360 and become less than 600 DEG C.During before moisture in silicon mud 360 evaporates completely, because heat is captured in the evaporation of moisture, the temperature that therefore there is silicon mud 360 hardly rises, and easily remains on less than 600 DEG C.But in the stage after moisture evaporates completely, the temperature of silicon mud 360 sharply rises.Now, the temperature cannot tackled sharply by means of only the cooling of a system in magnetism servo-electric motor water-cooling or air cooling mechanism 391 rises, and there is the danger that the temperature in silicon mud 360 rises.Therefore, while the temperature of silicon mud 360 sharply rises, also to control by the mode that magnetism servo-electric motor water-cooling and air cooling mechanism 391 implement to cool fast.By and with both come to cool fast, thus when there occurs variations in temperature sharply, also the temperature of treated object can be maintained the temperature of expectation.In this case, magnetism servo-electric motor water-cooling (water cooling tube 390) and this two side of air cooling mechanism 391 is made to cool when the temperature of control part 430 in cylinder 350 (temperature of silicon mud 360) becomes the temperature preset.With regard to the temperature preset, be such as 500 degree when treated object is silicon mud, and be pre-stored in control part 430.
[industrial applicibility]
The present invention can be used in the heat treatment step of the various industrial circles such as the synthesis of the Reuse of materials operation of solar cell or semiconductor etc., functional material or macromolecular material.
Claims (13)
1. a microwave heating equipment, is characterized in that, possesses:
For keeping the cylinder of treated object;
To the microwave applicator of described cylinder internal radiation microwave;
Make the whirligig of described drum rotating;
Be arranged on the stirring piece in described cylinder;
To the cooling device that described cylinder cools,
Described cooling device has the magnetism servo-electric motor water-cooling cooling described cylinder by cooling fluid,
The mode that described magnetism servo-electric motor water-cooling is located at described stirring piece for the pipe that described cooling fluid is passed through is formed.
2. microwave heating equipment according to claim 1, is characterized in that,
Described magnetism servo-electric motor water-cooling is embedded to the side of described cylinder.
3. microwave heating equipment according to claim 1, is characterized in that,
Described cooling device also has the air cooling mechanism to described roller spray refrigerating gas.
4. microwave heating equipment according to claim 3, is characterized in that, possesses:
Thermometer, it measures the temperature in described cylinder;
Control part, its make in described magnetism servo-electric motor water-cooling or described air cooling mechanism while making described microwave applicator irradiating microwaves either party cool, make described magnetism servo-electric motor water-cooling and this two side of described air cooling mechanism cool when the temperature in described cylinder becomes the temperature preset.
5. microwave heating equipment according to claim 1, is characterized in that,
Described cylinder is formed in the mode of the conductive coefficient in outside lower than the conductive coefficient of inner side.
6. microwave heating equipment according to claim 1, is characterized in that,
Possess and make described cooling device carry out the control part cooled while making described microwave applicator irradiating microwaves.
7. microwave heating equipment according to claim 1, is characterized in that,
Described stirring piece is made up of the material of microwave transmissive.
8. microwave heating equipment according to any one of claim 1 to 7, is characterized in that,
Described treated object comprises the first material and the second material,
Described first material is polar substances, dielectric loss angle Tan δ be more than 0.01 material or conductance be 10
-2above and 10
4any one in following material,
Described second material and polar substances, dielectric loss angle Tan δ be more than 0.01 material or conductance be 10
-2above and 10
4any one in following material is all different.
9. a microwave heating method, the treated object irradiating microwaves in stirring in cylinder heats described treated object, it is characterized in that,
Described cylinder is cooled while irradiating microwaves,
Described cylinder be cooled through the stirring piece of cooling settings on described cylinder to carry out.
10. microwave heating method according to claim 9, is characterized in that,
The cooling of described cylinder uses cooling fluid to carry out.
11. microwave heating methods according to claim 10, is characterized in that,
The cooling of described cylinder also uses refrigerating gas to carry out.
12. microwave heating methods according to claim 11, is characterized in that,
The cooling of described cylinder use in described cooling fluid or described refrigerating gas while irradiating microwaves any one carry out, use described cooling fluid and this two side of described refrigerating gas to carry out when the temperature in described cylinder becomes the temperature preset.
13. microwave heating methods according to any one of claim 9 to 12, is characterized in that,
Described treated object comprises the first material and the second material,
Described first material is polar substances, dielectric loss angle Tan δ be more than 0.01 material or conductance be 10
-2above and 10
4any one in following material,
Described second material and polar substances, dielectric loss angle Tan δ be more than 0.01 material or conductance be 10
-2above and 10
4any one in following material is all different.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
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| JP2013-080936 | 2013-04-09 | ||
| JP2013080936A JP6106848B2 (en) | 2013-04-09 | 2013-04-09 | Microwave heating apparatus and microwave heating method |
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| CN104105239A CN104105239A (en) | 2014-10-15 |
| CN104105239B true CN104105239B (en) | 2016-02-17 |
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| EP3210439B1 (en) | 2014-10-23 | 2019-07-10 | Harold Dail Kimrey Jr | Radio frequency heating system |
| CN109668185B (en) * | 2018-12-28 | 2020-06-30 | 广东美的厨房电器制造有限公司 | Microwave cavity assembly and microwave oven |
| CN109668187B (en) * | 2018-12-28 | 2020-06-30 | 广东美的厨房电器制造有限公司 | Microwave oven with a heat exchanger |
| CN109668186B (en) * | 2018-12-28 | 2020-07-14 | 广东美的厨房电器制造有限公司 | Microwave cavity assembly and microwave oven |
| JP2022186067A (en) * | 2021-06-04 | 2022-12-15 | トヨタ自動車株式会社 | Method for producing guest-free silicon clathrate, and apparatus for producing guest-free silicon clathrate |
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Also Published As
| Publication number | Publication date |
|---|---|
| JP6106848B2 (en) | 2017-04-05 |
| JP2014203762A (en) | 2014-10-27 |
| CN104105239A (en) | 2014-10-15 |
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