CN104165898A - Large-temperature-gradient Bridgman furnace - Google Patents
Large-temperature-gradient Bridgman furnace Download PDFInfo
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- CN104165898A CN104165898A CN201410415167.4A CN201410415167A CN104165898A CN 104165898 A CN104165898 A CN 104165898A CN 201410415167 A CN201410415167 A CN 201410415167A CN 104165898 A CN104165898 A CN 104165898A
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Abstract
The invention discloses a large-temperature-gradient Bridgman furnace. The large-temperature-gradient Bridgman furnace comprises a furnace body, wherein an aerogel heat insulation ceramic layer is filled between a furnace shell and a hearth of the furnace body; the hearth sequentially comprises an upper medium-temperature zone, a middle high-temperature zone, a middle gradient zone and a lower low-temperature zone from top to bottom; temperature controlling heaters with temperature measuring thermocouples integrated in the temperature controlling heaters are arranged in the upper medium-temperature zone, the middle high-temperature zone and the lower low-temperature zone; the side wall of the middle gradient zone is wrapped with a heat insulation fireproof layer with holes; a sample rack for storing samples is also arranged in the hearth, and the top of the sample rack is connected with a single-shaft shifter. The large-temperature-gradient Bridgman furnace is capable of conveniently adjusting the controlling temperatures of the high-temperature zone and the low-temperature zone according to the physical properties of different metals to obtain growth temperature fields suitable for different metals, controlling the drawing speed by combining a single-shaft shifter controller, maintaining the interface stability of solidification of metal melts on the sample rack and stably observing the solidification process of the metals in real time.
Description
Technical field
The present invention relates to a kind of synchrotron radiation line station that is suitable for and observe solidification of metal melt large thermograde bridgman furnace for growth interface, belong to and solidify studying technological domain.
Background technology
Due to the not penetrability of the visible ray of its metal bath own, about the direct observation of its process of setting, within a very long time, be all difficult to carry out.All adopt traditionally process of setting [Timmermans J.J Phys Chem Solids 18 (1961) 1-8 of the solidification and crystallization process by using simulation metal bath of organic solute or part ammonium salt, W Huang, L Wang, Solidification Science and Technology, Brunel University Press, London, 2011,243].Yet this method is to adopt a process of setting that diverse system is simulated another system after all, it solidifies the feature that growing state can not complete reaction metal solidification process.In addition, the selection of organic solute system has also determined the degree of approximation of simulation.Up to the present, only having solute in tens to be proved to be can be for the different Solidification Characteristics of simulation metal bath.Organism and the metal material significant difference on some important physical and chemical performances, the observations that researchers can not be solidified according to organism is completely carried out the solidified structure forming process of reasoning metal alloy.
Along with the development of synchronous light source, researcher utilizes the synchrotron radiation light source of the third generation successfully the dendritic growth behavior in metal solidification process to be studied both at home and abroad.Synchrotron radiation X-ray imaging technique has the advantages such as high-energy, high brightness, high resolving power and monochromaticity are good, can meet the real time imagery requirement to dendritic growth.But observe metal solidification texture, not only light source quality is had to requirement, the establishment of coagulating environment is also had to certain requirement.Less than normal in view of the most energy in domestic synchrotron radiation light source line station, the open hour are limited, insufficient space, and auxiliary facility is perfect not, therefore to having relatively high expectations for the supporting body of heater of metal freezing research use.At present, a series of synchrotron radiations of domestic Dalian University of Technology exploitation are larger with stove or volume, or actual serviceability temperature is lower, is difficult to provide stable, reliable high-temperature gradient coagulating environment.And the synchrotron radiation that Europe and Japan [J.Crystal Growth 374 (2013) 23-30] synchrotron radiation line station provide can provide certain thermograde with bridgman furnace, small volume.But because calandria adopts the traditional approach of laying heater coil on ceramic substrate, calandria is difficult in maintenance, and reliability is low.
Summary of the invention
The object of the invention is to observe for existing synchrotron radiation line station the deficiency that solidification of metal melt growth interface exists by stove technology, provide a kind of volume little, reliable, solidify growth temperature field and the controlled small-sized bridgman furnace of the speed of growth.
For achieving the above object, technical scheme of the present invention is that solidification of metal melt large thermograde bridgman furnace for growth interface is observed at a kind of synchrotron radiation line station that is suitable for of design, comprise body of heater, between the furnace shell of described body of heater and burner hearth, be filled with aerogel heat-proof ceramic layer;
Described burner hearth from top to bottom comprises successively: warm area in top, high-temperature region, middle part, gradient zones, middle part and low-temperature space, bottom;
In described top, warm area, high-temperature region, middle part and low-temperature space, bottom are provided with the temp controlling heater of inner integrated temperature thermocouple separately;
Gradient zones, described middle part sidewall is enclosed with insulating refractory layer with holes, and described insulating refractory layer is made by aerogel ceramic wafer;
In described burner hearth, be also provided with for placing the specimen holder of sample, described specimen holder top is connected with a single shaft shifter.
Preferably, the temperature thermocouple of high-temperature region, described middle part 5mm place above gradient zones, middle part; The temperature thermocouple of low-temperature space, described bottom 5mm place below gradient zones, middle part.
Preferably, the top of described burner hearth is provided with by high aluminum fiber cotton and makes and for the insulating curtain of closed furnace, can effectively prevent the chimney effect of burner hearth, guarantees that high-temperature region keeps constant temperature high temperature, and the fusing and the temperature that are conducive to research object are even.
Preferably, low-temperature space, described bottom is also provided with for its cooling cooling water pipe.
Preferably, described temp controlling heater is provided with connection terminal.
Burner hearth is sealed by aerogel heat-proof ceramic layer, can reduce the heat interchange of burner hearth to environment temperature, prevent that heat from causing thermal loss to atmosphere transmission, maintain the temperature stabilization of each warm area, make gradient bridgman furnace of the present invention in less volume, to provide higher fire box temperature, and can reduce the surface temperature of furnace shell, can also reduce the heat transmission between each warm area, thereby increase the thermograde of gradient zones.
In top, warm area, high-temperature region, middle part and low-temperature space, bottom are provided with the temp controlling heater of inner integrated temperature thermocouple, can effectively control the thermograde of melt temperature and gradient zones, middle part.
Middle part gradient zones sidewall is enclosed with insulating refractory layer with holes, and this insulating refractory layer is for stopping that the heat of high-temperature region, middle part is to radiation, convection current and the conduction of gradient zones, middle part, to reduce the temperature difference of high-temperature region, middle part, and holding temperature field stable.Because the coefficient of heat conductivity of air is less, the middle air hole of insulating refractory layer can effectively stop the heat of high-temperature region, middle part to transmit to gradient zones, middle part, increases the thermograde of gradient zones, middle part.
Gradient zones, middle part is provided with temperature thermocouple in each 5mm place up and down, and the temperature of energy real-time monitoring hearth inside, both sides, gradient zones also provides data recording.
There is the specimen holder of placing sample burner hearth inside, can place the test button of certain size.
The top of specimen holder is connected with single shaft displacement controller, can control the setting rate of metal bath together with thermograde, and controls the growth pattern that solidifies of metal bath.
Low-temperature space, bottom is provided with for its cooling cooling water pipe, can further increase the thermograde of gradient zones, middle part.
The present invention can be according to the physical property of different metal, regulate easily the control temperature of high-temperature region, low-temperature space, obtain the growth temperature field that is applicable to different metal, and in conjunction with single shaft displacement controller restrained stretching speed, maintain the interface stability of solidification of metal melt on specimen holder.Realization is observed the real-time stabilization of metal solidification process.
Accompanying drawing explanation
Fig. 1 is schematic diagram of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is further described.Following examples are only for technical scheme of the present invention is more clearly described, and can not limit the scope of the invention with this.
The concrete technical scheme of implementing of the present invention is:
As shown in Figure 1, solidification of metal melt large thermograde bridgman furnace for growth interface is observed at a kind of synchrotron radiation line station that is suitable for, and comprises body of heater, between the furnace shell 15 of described body of heater and burner hearth, is filled with aerogel heat-proof ceramic layer 3; Burner hearth in body of heater from top to bottom comprises: in top, warm area 11, high-temperature region, middle part 12, low-temperature space, 13He bottom, gradient zones, middle part 14 4 parts.The insulating curtain 2 that the top of burner hearth is made by high aluminum fiber cotton seals, and can effectively prevent the chimney effect of burner hearth, guarantees that high-temperature region keeps constant temperature high temperature, and the fusing and the temperature that are conducive to research object are even.Burner hearth bottom is sealed by aerogel heat-proof layer, prevents that heat from, to atmosphere transmission, causing thermal loss, maintains the temperature stabilization of low-temperature space.In top, warm area 11, low-temperature space, 12He bottom, high-temperature region, middle part 14 are equipped with temp controlling heater (the top temp controlling heater 4 of inner integrated temperature thermocouple, middle part temp controlling heater 5, and connect PID thermostat calandria is carried out to accurate temperature controlling bottom temp controlling heater 9).The insulating refractory layer 7 that gradient zones, middle part 13 adopts aerogel ceramic wafer with holes to make, this flame retardant coating inside dimensions is consistent with size of burner hearth, interference-free to guarantee moving up and down of specimen holder 1, this insulating refractory layer 7 is for stopping that the heat of high-temperature region 12, middle part is to radiation, convection current and the conduction of gradient zones, middle part 13, to reduce the temperature difference of high-temperature region 12, middle part, holding temperature field stable.Because the coefficient of heat conductivity of air is less, the middle air hole of insulating refractory layer 7 can effectively stop heat 13 transmission to gradient zones, middle part of high-temperature region 12, middle part, increases the thermograde of gradient zones 13, middle part.For further increasing the thermograde of gradient zones 13, middle part, low-temperature space, bottom 14 is also connected with for cooling cooling water pipe 8, and the flow of chilled water can be controlled via temperature controller.By adjusting middle part high-temperature region 12 temperature and low-temperature space, bottom 14 temperature, can realize larger thermograde in narrower gradient zones, meet different-alloy and solidify the required temperature requirements of growth.In burner hearth, establish specimen holder 1, its top is connected with single shaft shifter 16, can realize the decline of specimen holder 1.Burner hearth is inner, and high-temperature region temperature thermocouple and low-temperature space temperature thermocouple 6 are equipped with in both sides Shang Xia 13 in gradient zones, middle part, for Real-Time Monitoring and record the thermograde of gradient zones.
The present invention can be according to the physical property of different metal, regulate easily the control temperature of high-temperature region, low-temperature space, obtain the growth temperature field that is applicable to different metal, and in conjunction with single shaft displacement controller restrained stretching speed, maintain the interface stability of solidification of metal melt on specimen holder.Realization is observed the real-time stabilization of metal solidification process.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, do not departing under the prerequisite of the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. be suitable for synchrotron radiation line station and observe solidification of metal melt large thermograde bridgman furnace for growth interface, comprise body of heater, it is characterized in that, between the furnace shell of described body of heater and burner hearth, be filled with aerogel heat-proof ceramic layer;
Described burner hearth from top to bottom comprises successively: warm area in top, high-temperature region, middle part, gradient zones, middle part and low-temperature space, bottom;
In described top, warm area, high-temperature region, middle part and low-temperature space, bottom are provided with the temp controlling heater of inner integrated temperature thermocouple separately;
Gradient zones, described middle part sidewall is enclosed with insulating refractory layer with holes, and described insulating refractory layer is made by aerogel ceramic wafer;
In described burner hearth, be also provided with for placing the specimen holder of sample, described specimen holder top is connected with a single shaft shifter.
2. large thermograde bridgman furnace according to claim 1, is characterized in that, the temperature thermocouple of high-temperature region, described middle part 5mm place above gradient zones, middle part; The temperature thermocouple of low-temperature space, described bottom 5mm place below gradient zones, middle part.
3. large thermograde bridgman furnace according to claim 2, is characterized in that, the top of described burner hearth is provided with by high aluminum fiber cotton and makes and for the insulating curtain of closed furnace.
4. large thermograde bridgman furnace according to claim 3, is characterized in that, low-temperature space, described bottom is also provided with for its cooling cooling water pipe.
5. large thermograde bridgman furnace according to claim 4, is characterized in that, described temp controlling heater is provided with connection terminal.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107419327A (en) * | 2017-07-24 | 2017-12-01 | 共慧冶金设备科技(苏州)有限公司 | Sigmatron three dimensions imaging bridgman furnace |
| CN109945642A (en) * | 2019-03-26 | 2019-06-28 | 杭州而然科技有限公司 | A kind of metal oxide ceramic Fast Sintering furnace and its sintering process |
| CN111812144A (en) * | 2020-07-22 | 2020-10-23 | 湖北戈碧迦光电科技股份有限公司 | Method for determining secondary pressing temperature range of optical glass |
| CN112710681A (en) * | 2020-12-21 | 2021-04-27 | 中南大学 | Experimental device for solidification behavior is observed to normal position |
| CN113447403A (en) * | 2021-06-11 | 2021-09-28 | 南京航空航天大学 | Heating device for measuring spectral emissivity of high-temperature particle curtain |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109945642A (en) * | 2019-03-26 | 2019-06-28 | 杭州而然科技有限公司 | A kind of metal oxide ceramic Fast Sintering furnace and its sintering process |
| CN109945642B (en) * | 2019-03-26 | 2023-10-24 | 杭州而然科技有限公司 | Rapid sintering furnace and sintering process for metal oxide ceramic material |
| CN111812144A (en) * | 2020-07-22 | 2020-10-23 | 湖北戈碧迦光电科技股份有限公司 | Method for determining secondary pressing temperature range of optical glass |
| CN112710681A (en) * | 2020-12-21 | 2021-04-27 | 中南大学 | Experimental device for solidification behavior is observed to normal position |
| CN113447403A (en) * | 2021-06-11 | 2021-09-28 | 南京航空航天大学 | Heating device for measuring spectral emissivity of high-temperature particle curtain |
| CN113447403B (en) * | 2021-06-11 | 2022-05-03 | 南京航空航天大学 | Heating device for measuring spectral emissivity of high-temperature particle curtain |
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Application publication date: 20141126 |