CN102095480A - Heating real-time weighting device of high-temperature material - Google Patents

Heating real-time weighting device of high-temperature material Download PDF

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Publication number
CN102095480A
CN102095480A CN 201010567534 CN201010567534A CN102095480A CN 102095480 A CN102095480 A CN 102095480A CN 201010567534 CN201010567534 CN 201010567534 CN 201010567534 A CN201010567534 A CN 201010567534A CN 102095480 A CN102095480 A CN 102095480A
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zirconia
temperature
grillage
thickness
quartz plate
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CN 201010567534
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CN102095480B (en
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武湛君
王智
史国栋
严佳
柳敏静
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Dalian University of Technology
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Dalian University of Technology
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Abstract

The invention belongs to the technical field of high-temperature materials, in particular to heating real-time weighting equipment of a high-temperature material, characterized in that a zirconia bracket and a multi-layer vacuum quartz grillage are sequentially arranged between the high-temperature material and a precision balance; the top and the bottom of the multi-layer vacuum quartz grillage are isolated by zirconia insulation felt, the zirconia bracket is a porous zirconia block with the thickness of 5-15 mm and the void ratio of 10-45 percent; the multi-layer vacuum quartz grillage comprises 3-10 layers of transversally arranged quartz plates and quartz plates for sealing the periphery, the transversal quartz plate on each layer has the thickness of 2-7 mm and the layer distance of 5-10 m, the transversal quartz plates and the quartz plates for sealing the periphery are adhered to form a sealed space which is vacuumized; and the zirconia insulation felt has the thickness of 5-12mm and contains 92-99 percent of zirconia. The heating real-time weighting equipment of the high-temperature material can work at a temperature of 2,000 DEGC for a long time, has high weighting accuracy and can be applied to the development of aerospace thermal protection materials and other high-temperature fields.

Description

The real-time weighing device of a kind of heating of high-temperature material
Technical field
The invention belongs to the high-temperature material technical field, relate to the real-time weighing-appliance of a kind of heating high-temperature material.
Background technology
Lifting along with the space transportation system aircraft speed, the temperature on spacecraft of future generation surface will be more high than existing aircraft surface temperature, especially nose cone, nose of wing etc. have the thermal protection structure of sharp-pointed profile, can surpass 1800 ℃ at hypersonic flight environment of vehicle underlaying surface temperature, press for research and exploitation high-temperature structural material.Present spacecraft heat protective materials mainly contains refractory metal and alloy, metal-base composites, intermetallic compound, carbon/carbon compound material, ceramic matric composite etc., wherein which kind of material is more suitable for the needs of aerospace flight vehicle of future generation, and this need carry out the experimental study of high-temperature behavior and anti-oxidant ablation property at different materials.
Under the high temperature aerobic environment, oxidative phenomena all can take place in any elevated temperature heat protective materials, and the accurate assessment of the oxidation rate of thermally protective materials is the key of thermal protection system design.In the assessment of thermally protective materials oxidation rate, if assessment result is bigger than normal, will cause the thermal protection system design that material is proposed higher requirement, increase the development difficulty of thermally protective materials, and reduced the flying speed and the flight efficiency of aircraft; If assess too smallly, will bring great hidden danger to the safety of aircraft.The mass change of the thermally protective materials that therefore real-time measurement oxidation causes, promptly oxidation rate is a very crucial experimental procedure that is related to the aircraft security operation.
Existing high temperature weighing-appliance, its working temperature interval is usually less than 500 ℃, this does not reach accurately weighing in real time of 1800 ℃ of high-temperature materials far away, makes the mass change of the thermally protective materials that measurement oxidation in real time causes become a bottleneck problem of researching high-temperature thermally protective materials.
Summary of the invention
Purpose of the present invention, be to provide a kind of to high-temperature material simply, the high temperature device of weighing in real time efficiently, be used for working long hours of environment below 2000 ℃.
Technical scheme of the present invention is: the real-time weighing device of a kind of heating of high-temperature material, be included as the induction heating equipment of high-temperature material heating, contactless pyrometer, precision balance, wherein pyrometer and precision balance respectively with signals collecting, show that computer system connects, it is characterized in that, be heated and be provided with zirconia support and the quartzy grillage of multi-layer vacuum between the high-temperature material of weighing in real time and the precision balance successively, high-temperature material is placed on the zirconia support, the zirconia support is placed on the quartzy grillage of multi-layer vacuum, the quartzy grillage of multi-layer vacuum is placed on the precision balance multi-layer vacuum English grillage and zirconia support, also be separated with the zirconia heat insulation felt between the precision balance respectively; The zirconia support is that thick 5~15mm, porosity are 10~45% porous zirconia block; The quartzy grillage of multi-layer vacuum is by 3~10 layers of transversely arranged quartz plate and seal with quartz plate all around and constitute, the thickness of every layer of horizontal quartz plate is 2~7mm, between separate with quartz wedge, interlamellar spacing is 5~10mm, and laterally quartz plate and sealing all around form confined space with bonding between the quartz plate and vacuumize; Zirconia heat insulation felt thickness is 5~12mm, and its zirconia content is 92~99%.
For the heat conduction that prevents measured material or be radiated on the balance, the employing zirconia that thermal conductivity is very low and fusing point is very high is as support, for further reducing the thermal conductivity of zirconia support, when not reducing zirconia stent support ability, reduce its density, promptly increase its porosity, can influence zirconic supporting capacity but porosity is too high, therefore the zirconia porosity adopts 10~45%, is preferably 25~40%, and zirconia support optimum thickness is 7~12mm; The multi-layer vacuum quartz plate is erected further heat insulation effect, and optimal parameter is: the transversely arranged quartz plate number of plies is 4~7 layers, every layer of quartz plate thickness 3~5mm, layer thickness 6~8mm.When making the quartzy grillage of multi-layer vacuum, can reserve during bonding and vacuumize the hole, vacuumize the heat-sealable vacuum hole that closes after the end with horizontal quartz plate and sealing all around with between the quartz plate and horizontal quartz plate with at interval with after high-temperature fusion, boning between the quartz wedge.Between the quartzy grillage of zirconia support and multi-layer vacuum, and place the zirconia heat insulation felt that thickness is 5~12mm respectively between quartzy grillage of multi-layer vacuum and the precision balance, can be further heat insulation on the basis of not obvious increase balance load, the optimum thickness of zirconia heat insulation felt is 7~10mm, and its zirconia content is preferably 95~99%;
The power of induction heating equipment can be selected 30~45kW, the temperature measurement range of pyrometer can be 1000~3000 ℃, the size of measured material can adopt length in 50mm, the upper surface diameter of zirconia support or the length of side can be 50~80mm, and the precision balance range can be 5000 grams.
Apparatus of the present invention can realize simply, quickly that the high temperature heating of high-temperature material weighs in real time, can under 2000 ℃ of temperature, work long hours, experimental cost is cheap, the accuracy rate of weighing height, not only can be applied in exploitation, research and the production of Aero-Space thermally protective materials, can also be applied in other high temperature fields.
Description of drawings
Fig. 1 is the real-time weighing device synoptic diagram of the heating of high-temperature material of the present invention, and 1 is tested high-temperature material among the figure, and 2 is the heater coil of induction heating equipment, and 3 is the zirconia support, and 4,6 is the zirconia heat insulation felt, and 5 is the quartzy grillage of multi-layer vacuum, and 7 is precision balance.
The zirconium boride-carborundum that Fig. 2 records for apparatus of the present invention-zirconium carbide ceramics based composites is the time dependent curve of quality under 1700 ± 15 ℃ of temperature, and horizontal and vertical coordinate is respectively oxidization time (s) and weight per unit area (mg/cm among the figure 2).
When the zirconium boride-carborundum that Fig. 3 records for apparatus of the present invention-zirconium carbide ceramics based composites is heated to 1700 ± 15 ℃ of temperature for the second time, the time dependent curve of quality.
Zirconium boride-carborundum ceramic matric composite time dependent curve of quality under 1700 ± 15 ℃ of temperature that Fig. 4 records for apparatus of the present invention.
Embodiment
The invention will be further described below by embodiment, and application of the present invention is not limited to material that embodiment lifts.
Embodiment 1, measures the mass change at high temperature of high-temperature material zirconium boride-carborundum-zirconium carbide ceramics based composites with real-time weighing device of the present invention.
Heat measurement mechanism as shown in Figure 1, it is 50mm that the zirconia support adopts the upper surface diameter, and thickness is that 5mm, porosity are 10% porous zirconia block; Adopt commercial oxidation zirconium heat insulation felt, its zirconia content is 92%, and thickness is 5mm; The multi-layer vacuum quartz plate number of plies is 3 layers, every layer of quartz plate thickness 2mm, interfloor distance is 5mm, with horizontal quartz plate and between the quartz plate and horizontal quartz plate and all around at interval with after high-temperature fusion, boning between the quartz wedge, reserve during bonding and vacuumize the hole, vacuumize and finish the heat-sealable vacuum hole that closes in back.The zirconia support is placed on the quartzy grillage of multi-layer vacuum, and the quartzy grillage of multi-layer vacuum is placed on the balance, and the quartzy grillage of multi-layer vacuum is separated with the zirconia heat insulation felt up and down.
Adopt the contactless radiation pyrometer of multiband (model is MR1SC), measuring temperature range is 1000-3000 ℃, the precision balance range is 5000g, and precision is 0.1mg, and pyrometer is connected with signals collecting, demonstration computer system respectively with precision balance.
Zirconium boride-carborundum-zirconium carbide ceramics based composites specimen size is 36mm * 4mm * 3mm, and adopting diamond paste that specimen surface is polished to smooth finish is below the 1 μ m.The temperature survey step is as follows:
1) sample after will polishing is placed on the zirconia support; 2) open the balance power supply, wait zero clearing after the balance balance; 3) open multiband pyrometer power supply, adjust thermometer registration coupon center; 4) open induction heating equipment, when specimen temperature was elevated to 1700 ± 15 ℃, the computer recording sample mass is curve over time, and the sample heated oxide time is controlled at 600s.Measurement result is seen Fig. 2.
As shown in Figure 2, apparatus of the present invention measurement data has higher precision, and significantly some skew does not take place.According to Theoretical Calculation, ZrB 2-SiC-ZrC compound substance oxidizing process mass change first meets the second-degree parabola rule, and curve that present embodiment measures and second-degree parabola are very identical, and the measurement result of these explanation apparatus of the present invention has higher reliability.After oxidization time under 1700 ± 15 ℃ of high temperature surpassed 200s, the mass area ratio pace of change of specimen surface obviously began to reduce, and this is because specimen surface has generated comparatively fine and close SiO 2Glassy layer can partly stop oxygen to the sample internal divergence, thereby reduce the mass area ratio pace of change.
Embodiment 2, with real-time weighing device of the present invention, measure the high-temperature oxydation mass change second time through embodiment 1 used test specimen.
Consider that high-temperature material needs to use repeatedly when practical application, for measuring repeatedly oxidation susceptibility of material, present embodiment continues the sample that use embodiment 1 measured.
The porous zirconia block porosity of weighing-appliance is 20%, and the upper surface diameter is 70mm, and thickness is 7mm; The zirconia content of zirconia heat insulation felt is 94%, and thickness is 7mm; Multi-layer vacuum quartz plate rack-layer number is 4 layers, every layer of quartz plate thickness 3mm, and interfloor distance is 6mm.
Measuring process is with embodiment 1, and heating-up temperature is 1700 ± 15 ℃ still, and measurement result is seen Fig. 3.
Because there has been the comparatively SiO of even compact of one deck in specimen surface 2Glassy layer causes the constant rate of oxygen to the sample internal divergence, thereby quality and oxidization time are linear, and data point does not have the drift of generation and unusual fluctuation yet among the figure, and this devices illustrated can realize accurate measurement in the weighing process in real time.
Embodiment 3, with real-time weighing device of the present invention, measure the mass change of high-temperature oxydation for the third time through embodiment 2 used test specimens.
The porous zirconia block porosity of weighing-appliance is 30%, and the upper surface diameter is 80mm, and thickness is 9mm; The zirconia content of zirconia heat insulation felt is 96%, and thickness is 9mm; Multi-layer vacuum quartz plate rack-layer number is 5 layers, and every layer of quartz plate thickness is 5mm, and interfloor distance is 8mm.
Measuring process is with embodiment 1, and heating-up temperature is 1700 ± 15 ℃, and measurement result and reason thereof are similar to embodiment 2, and quality and oxidization time are linear.
Embodiment 4, with real-time weighing device of the present invention, and the mass change when measuring the long-time high-temperature oxydation of zirconium boride-carborundum ceramic matric composite.
Be further examination apparatus of the present invention serviceability for a long time at high temperature, with zirconium boride-carborundum ceramic matric composite test specimen at 1700 ± 15 ℃ of following heated oxide 1800s.
The porous zirconia block porosity of weighing-appliance is 45%, and the upper surface diameter is 80mm, and thickness is 13mm; The zirconia content of zirconia heat insulation felt is 99%, and thickness is 10mm; Multi-layer vacuum quartz plate rack-layer number is 9 layers, every layer of quartz plate thickness 6mm, and interfloor distance is 9mm.
Measuring process is with embodiment 1, and heating-up temperature is 1700 ± 15 ℃, Measuring Time 1800s, in the oxidizing process quality in time change curve see Fig. 4.
As shown in Figure 4, the zirconium boride-carborundum ceramic matric composite is the quality of high-temperature oxydation-time measure of the change result first, meet the second-degree parabola rule, and there is not data point that drift or unusual fluctuation take place, proof is under long hot environment, and real-time weighing equipment of the present invention remains higher degree of accuracy.

Claims (3)

1. the real-time weighing device of the heating of a high-temperature material, be included as the induction heating equipment of high-temperature material heating, contactless pyrometer, precision balance, wherein pyrometer and precision balance respectively with signals collecting, show that computer system connects, it is characterized in that, be heated and be provided with zirconia support and the quartzy grillage of multi-layer vacuum between the high-temperature material of weighing in real time and the precision balance, high-temperature material is placed on the zirconia support, the zirconia support is placed on the quartzy grillage of multi-layer vacuum, the quartzy grillage of multi-layer vacuum is placed on the precision balance multi-layer vacuum English grillage and zirconia support, also be separated with the zirconia heat insulation felt between the precision balance respectively; The zirconia support is that thick 5~15mm, porosity are 10~45% porous zirconia block; The quartzy grillage of multi-layer vacuum is by 3~10 layers of transversely arranged quartz plate and seal with quartz plate all around and constitute, the thickness of every layer of horizontal quartz plate is 2~7mm, between separate with quartz wedge, interlamellar spacing is 5~10mm, and laterally quartz plate and sealing all around form confined space with bonding between the quartz plate and vacuumize; Zirconia heat insulation felt thickness is 5~12mm, and its zirconia content is 92~99%.
2. the real-time weighing device of the heating of high-temperature material as claimed in claim 1 is characterized in that, the porous zirconia porosity of zirconia support is 25~40%, and thickness is 7~12mm; The horizontal quartz plate number of plies of the quartzy grillage of multi-layer vacuum is 4~7 layers, every layer of quartz plate thickness 3~5mm, interfloor distance 6~8mm; The thickness of zirconia heat insulation felt is that 7~10mm, zirconia content are 95~99%.
3. as the real-time weighing device of the heating of claim 1 or described high-temperature material, it is characterized in that, the temperature measurement range of contactless pyrometer is 1000~3000 ℃, the length of measured material is all in 50mm, the upper surface diameter of zirconia support or the length of side are 50~80mm, and the precision balance range is 5000 grams.
CN2010105675344A 2010-11-30 2010-11-30 Heating real-time weighting device of high-temperature material Expired - Fee Related CN102095480B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102628183A (en) * 2012-04-18 2012-08-08 江苏协鑫软控设备科技发展有限公司 Thermal insulation structure and high-temperature furnace
CN107063423A (en) * 2017-06-01 2017-08-18 北京昆仑隆源石油开采技术有限公司 Aggregate automatic weighing method and apparatus

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000121417A (en) * 1998-10-19 2000-04-28 Kubota Corp Method for measuring weight of sample
US6189367B1 (en) * 1997-12-02 2001-02-20 Allan L. Smith Apparatus and method for simultaneous measurement of mass and heat flow changes
CN1869641A (en) * 2006-06-29 2006-11-29 上海交通大学 Detection method of ternary silicide high-temp in-situ oxidation
CN101514917A (en) * 2009-04-03 2009-08-26 天津商业大学 Electronic weighing system
CN201464314U (en) * 2009-07-21 2010-05-12 王明清 Heat-quality controllable detector

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6189367B1 (en) * 1997-12-02 2001-02-20 Allan L. Smith Apparatus and method for simultaneous measurement of mass and heat flow changes
JP2000121417A (en) * 1998-10-19 2000-04-28 Kubota Corp Method for measuring weight of sample
CN1869641A (en) * 2006-06-29 2006-11-29 上海交通大学 Detection method of ternary silicide high-temp in-situ oxidation
CN101514917A (en) * 2009-04-03 2009-08-26 天津商业大学 Electronic weighing system
CN201464314U (en) * 2009-07-21 2010-05-12 王明清 Heat-quality controllable detector

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102628183A (en) * 2012-04-18 2012-08-08 江苏协鑫软控设备科技发展有限公司 Thermal insulation structure and high-temperature furnace
CN102628183B (en) * 2012-04-18 2016-04-27 江苏协鑫软控设备科技发展有限公司 Insulation construction and High Temperature Furnaces Heating Apparatus
CN107063423A (en) * 2017-06-01 2017-08-18 北京昆仑隆源石油开采技术有限公司 Aggregate automatic weighing method and apparatus

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