CN2844896Y - High temperature weight analyzer for large sample of refractory material - Google Patents

High temperature weight analyzer for large sample of refractory material Download PDF

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Publication number
CN2844896Y
CN2844896Y CN 200520030323 CN200520030323U CN2844896Y CN 2844896 Y CN2844896 Y CN 2844896Y CN 200520030323 CN200520030323 CN 200520030323 CN 200520030323 U CN200520030323 U CN 200520030323U CN 2844896 Y CN2844896 Y CN 2844896Y
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temperature
resistant
hanging basket
heat
sample
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黄少平
钟香崇
徐恩霞
王澎
叶方保
钟焰
刘新红
贾全利
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CHANGSHA HIGH-TECH DEVELOPMENT ZONE JINGDA SCIENCE AND TECHNOLOGY Co Ltd
Zhengzhou University
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CHANGSHA HIGH-TECH DEVELOPMENT ZONE JINGDA SCIENCE AND TECHNOLOGY Co Ltd
Zhengzhou University
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Abstract

本实用新型涉及一种大试样耐火材料高温热重分析仪,属于测试耐火材料试样在高温和不同气氛下质量变化的大试样耐火材料高温质量变化测定仪,包括真空气氛炉、质量测量系统,该质量测量系统包括质量传感器,质量传感器通过连接装置与设在真空气氛炉中的耐高温吊篮相连接,在质量传感器下方连有耐热丝,在耐热丝下端连有耐高温连接杆,耐高温吊篮又与耐高温连接杆相连,在耐高温吊篮上设有可拆卸的耐高温吊篮底板,本实用新型可以实施动态的测定试样在升温过程中的质量-温度关系,也可测定试样在某一温度下的质量-时间关系,测试温度范围为常温到1700℃,测试气氛可以是氧化气氛、还原气氛、中性气氛和惰性气氛,质量测量范围为20~5000g,分辨率为0.1~100mg。

Figure 200520030323

The utility model relates to a large-sample refractory material high-temperature thermogravimetric analyzer, which belongs to a large-sample refractory material high-temperature quality change measuring instrument for testing refractory material samples under high temperature and different atmospheres, including a vacuum atmosphere furnace and a quality measurement instrument. system, the quality measurement system includes a quality sensor, the quality sensor is connected with the high-temperature-resistant hanging basket installed in the vacuum atmosphere furnace through a connecting device, a heat-resistant wire is connected under the quality sensor, and a high-temperature-resistant connection is connected at the lower end of the heat-resistant wire The high-temperature-resistant hanging basket is connected with the high-temperature-resistant connecting rod, and a detachable bottom plate of the high-temperature-resistant hanging basket is arranged on the high-temperature-resistant hanging basket. The utility model can implement dynamic measurement of the mass-temperature relationship of the sample during the heating process. It can also measure the mass-time relationship of the sample at a certain temperature. The test temperature range is from room temperature to 1700°C. The test atmosphere can be oxidizing atmosphere, reducing atmosphere, neutral atmosphere and inert atmosphere. The mass measuring range is 20-5000g , the resolution is 0.1 ~ 100mg.

Figure 200520030323

Description

Large test sample fireproof material high temperature thermogravimetric analyzer
Technical field:
The invention belongs to a kind of tester, relate in particular to a kind of large test sample fireproof material high temperature thermogravimetric analyzer of testing fire resistive material sample mass change under high temperature and different atmosphere.
Background technology:
The mass change of fire resistive material under high temperature and different atmosphere will directly have influence on its production and application, and the relation that the measurement refractory quality changed with temperature, time is the important research method of research fire resistive material high temperature physicochemical property.But because fire resistive material is many things phase, inhomogeneous material, usually contain a large amount of aggregates and pore, the too little performance that can not truly represent fire resistive material of sample mass in experiment, the measurement range of present normally used micro-thermogravimetric instrument is mostly at 0-100mg, the maximum capacity scope also has only 20g, can not satisfy the needs of fire resistive material research, make the research of simulation properties of refractories dynamic change under high temperature and different atmosphere seem difficult.For example owing to there is not the bigger thermogravimetric instrument of range, the test of the inoxidizability of non-oxidized substance fire resistive material and carbon containing refractory at present can only be confined to operate complicated, longer static heat reanalysis method of time, and the relation that can not the kinetic measurement sample mass changes with temperature or time.
Summary of the invention:
The objective of the invention is to overcome the deficiencies in the prior art and a kind of bulk specimen fire resistive material high temperature mass change analyzer that can implement the bigger fire resistive material sample piece of kinetic measurement quality-temperature relation and quality-time relationship under a certain temperature in the temperature-rise period of different atmosphere is provided.
The object of the present invention is achieved like this: comprise vacuum atmosphere oven and be arranged on mass measurement system on the vacuum atmosphere oven, this mass measurement system comprises mass sensor, and mass sensor is connected with high temperature resistance basket in being arranged on vacuum atmosphere oven by coupling arrangement.Be connected with heat-resisting silk below mass sensor, be connected with high temperature resistant connecting link in heat-resisting silk lower end, high temperature resistance basket is connected with high temperature resistant connecting link again, and high temperature resistance basket is provided with dismountable high temperature resistance basket base plate.Mass sensor be sealed in one with seal box that body of heater is connected in.Mass sensor is placed on the base plate of seal box, and the range of weighing of mass sensor is 0~5000g, and resolution is 0.1~100mg.The high and low position of high temperature resistance basket in burner hearth can be realized by the length that changes heat-resisting silk.Heat-resisting silk is connected with high temperature resistant connecting link by heat-resisting silk abutment ring, heat-resisting silk, heat-resisting silk abutment ring adopt heating resisting metal to make, high temperature resistant connecting link, high temperature resistance basket and high temperature resistance basket base plate are made by heat-resisting corundum, and high temperature resistance basket can be put the sample of sectional area less than 70.1 * 70.1mm into.Its mass measurement system can bear the gravity less than 5000g, and Range of measuring temp is 25 ℃~1700 ℃, and test atmosphere can be air atmosphere, reducing atmosphere and inert atmosphere.
The present invention has increased by a cover mass measurement system on a high-temperature vacuum atmosphere furnace, this mass measurement system comprises a mass sensor, this mass sensor can be a kind of weighing balance, mass sensor (or weighing balance) is positioned in the seal box that furnace roof portion and body of heater link together, and its signal wire links to each other with external control system by the terminals on the seal case.Heat-resisting silk respectively has a hook that mass sensor and high temperature resistant connecting link are coupled together up and down.High temperature resistant connecting link is a tubulose, and there is the skewer groove of a symmetry its lower end.There is the breach of symmetry the both sides of high temperature resistance basket base plate, can be stuck on the framework of hanging basket handle type when the hanging basket base plate is put on the hanging basket.Heat-resisting silk is made by heat-resistance stainless steel silk or the heating wire of Φ 1~Φ 3mm.High temperature resistant connecting link and hanging basket by stability at elevated temperature preferably corundum material make.The external diameter Φ 10mm of connecting link, the gross mass of connecting link and hanging basket is no more than 500g.
Good effect of the present invention is:
1, the present invention organically combines heating system, atmosphere control system and mass measurement system, and the range of weighing of measuring system is bigger, has realized the big quality kinetic measurement of fire resistive material sample in heating process.The production application reality that more meets fire resistive material.
2, the suspension type mass measurement system of the present invention's employing is measured accurately, and installation and easy to maintenance can be applied to the hot environment about 1600 ℃.
3, the present invention can finish in different atmosphere the test to sample.
Description of drawings:
Fig. 1 is a cross-sectional view of the present invention.
The structural representation that Fig. 2 is assembled into one for the present invention and body of heater and each operating system.
Fig. 3 is the cut-open view of hanging basket framework of the present invention.
Fig. 4 is the vertical view of hanging basket framework of the present invention.
Fig. 5 is the side view of hanging basket framework of the present invention.
Fig. 6 is hanging basket base plate figure of the present invention.
Fig. 7 is connecting link figure of the present invention.
Fig. 8 is a connecting link sectional view of the present invention.
Embodiment
Shown in Fig. 1,2,3,4,5,6,7,8, the present invention includes vacuum atmosphere oven and be arranged on mass measurement system on the vacuum atmosphere oven, this mass measurement system comprises mass sensor 12, and mass sensor 12 is connected with high temperature resistance basket 5 in being arranged on vacuum atmosphere oven by coupling arrangement.Be connected with heat-resisting silk 9 below mass sensor 12, be connected with high temperature resistant connecting link 7 in heat-resisting silk 9 lower ends, high temperature resistance basket 5 is connected with high temperature resistant connecting link 7 again, and high temperature resistance basket 5 is provided with dismountable high temperature resistance basket base plate 3.Mass sensor 12 is sealed in the seal box 10 that is connected with body of heater 16.Mass sensor 12 is placed on the base plate of seal box 10, and the range of weighing of mass sensor 12 is 0~5000g, and resolution is 0.1~100mg.The high and low position of high temperature resistance basket 5 in burner hearth 14 can be realized by the length that changes heat-resisting silk 9.Heat-resisting silk 9 is connected with high temperature resistant connecting link 7 by heat-resisting silk abutment ring 8, heat-resisting silk 9, heat-resisting silk abutment ring 8 adopt heating resisting metal to make, high temperature resistant connecting link 7, high temperature resistance basket 5 and high temperature resistance basket base plate 3 are made by heat-resisting corundum, and high temperature resistance basket 5 can be put the sample of sectional area less than 70.1 * 70.1mm into.Its mass measurement system can bear the gravity less than 5000g, and Range of measuring temp is 25 ℃~1700 ℃, and test atmosphere can be air atmosphere, reducing atmosphere and inert atmosphere.Mass sensor is positioned in the seal box that furnace roof portion and body of heater link together, and its signal wire links to each other with external control system by the terminals on the seal case.High temperature resistant connecting link is a tubulose, and there is the skewer groove of a symmetry its lower end.There is the breach of symmetry the both sides of high temperature resistance basket base plate, can be stuck on the framework of hanging basket handle type when the hanging basket base plate is put on the hanging basket.
By Fig. 1, Fig. 2 structure of large test sample fireproof material high temperature thermogravimetric analyzer of the present invention as can be seen.
By Fig. 3,4,5 as can be seen the hollow space of hanging basket framework 5 can put the sample of sectional area into less than 70.1 * 70.1mm.
Hanging basket base plate 3 can be positioned in the hanging basket framework 5 as seen from Figure 6, and can be stuck on the hanging basket framework 5 and can not drop.
By Fig. 7,8 as can be seen, there is a via hole connecting link 7 tops, can be connected with heat-resisting silk 9, and connecting link 7 belows have the skewer groove of a symmetry to be connected with hanging basket 5.
As seen from Figure 1, mass measurement system is by weighing balance 12 and hang on the heat-resisting silk 9 in its below, heat-resisting abutment ring 8, connecting link 7, hanging basket 5, hanging basket base plate 3 are formed, and weighing balance 12 is fixed on the base plate of seal box 10, is placed in the seal box 10.When the quality of the sample 4 in being placed on hanging basket 5 changed, weighing balance 12 can reach computers outward by connection terminal 11 with test signal, thereby measured the dynamic changing value of quality of sample 4.
As seen from Figure 1, if adjust hanging basket 5 high and low position of 14 in stove, the length that only needs to adjust heat-resisting silk 9 just can realize.
As seen from Figure 2, the seal box 10 of placing weighing balance 12 links to each other with body of heater 16, and pressure in the stove and atmosphere are by air intake opening 2 and gas outlet 17 controls.
As seen from Figure 1, the hanger 3,5,7,8,9 of mass measurement system has certain quality, and it can be deducted as blank in computing machine.So can directly measure the true value of the quality of sample.
As seen from Figure 1, change the range of weighing that different weighing balances 12 can change measuring system, the hanging basket 5 of changing different sizes also can satisfy the needs of different quality and different volumes sample.
By Fig. 1,2 as can be seen: body of heater 16 back that links to each other with seal box 10 forms one, and body of heater is sealable, and sample 4 is positioned over the center of hanging basket base plate 3, and is in the interior uniform temperature zone of burner hearth 14, and burner hearth 14 internal heat generation bodies 15 are electric heating body; Temperature in the burner hearth 14 reaches as high as 1700 ℃, and the uniform temperature zone temperature difference is in ± 5 ℃, and gaseous tension is-0.097~0.6Mpa in the burner hearth 14, and the shell of this heating furnace body 16 is a metal shell.
Detection method
Thermogravimetry (TG): many materials except that producing thermal effect, often have the variation of quality in heating or cooling procedure, and the size of its variation and the temperature that occurs are closely related with chemical composition.Therefore, utilize the characteristics that material mass changes in heating or the cooling procedure, can distinguish and identify different materials.This method just is thermogravimetry (TG).
Principle: thermogravimetric analysis has two kinds of methods usually, and promptly quiet method and moving method, quiet method are to be heated to constant weight under each given temperature, changes mapping by the quality time then.Moving method is to heat up continuously in heating process and weigh, by the mapping of quality temperature variation.
The thermogravimetric instrument:
Vacuum atmosphere oven: the electrothermal furnace that adopts molybdenum silicide heating element; Can heat high temperature resistance basket and sample simultaneously, and can speed in accordance with regulations heat up; The thermopair that the process calibration should be set adopts temperature programmed control to note down temperature automatically with the experiment with measuring temperature; Can form oxidation or nonoxidizing atmosphere by testing requirements.
Apparatus for measuring quality: various forms of high temperature resistant connecting link and high temperature resistance basket that mass measurement system can adopt mass sensor (or weighing balance) and cooperate, and satisfy following requirement: heat-resisting silk is made by heat-resistance stainless steel silk or the heating wire of Φ 1-Φ 3mm; High temperature resistant connecting link and hanging basket must have stability at elevated temperature preferably material make; The gross mass of connecting link and hanging basket is no more than 500g; The range of weighing of mass sensor (or weighing balance) is 0-5000g, and resolution is 0.1-100mg.
Computer control system: computer control system is furnished with special-purpose instrumentation and Control Software, thes contents are as follows: the control of guide instrument shows control procedure and record result; Test and description that the measurand quality changed with temperature, time.
Sample:
Sample weight: experimentally increase, weightless situation, determine the weight of sample, require sample weight to be no more than the apparatus measures range.
Specimen shape and size: sample can be block or powder, and the volume that requires block is less than the hanging basket volume, and powder must hold with crucible.
Experimental procedure:
The energising preheating: power supply and control computer must be opened before opening test instrument, experiment instrument is carried out preheating, the time is no less than 30 minutes.
The dress sample: block sample is directly put into and is hung indigo plant, and the powder sample should be positioned over to put into then in the corundum crucible and hang indigo plant.
Test parameters is provided with: the elevated temperature heat of the opening computing machine control system of resurveying, carry out parameter setting.
Atmosphere is selected: require to have following operation steps according to experiment atmosphere.
If test is for oxidizing atmosphere, the gas admittance valve of trial furnace is connected air compressor, with flow blowing air in stove of 2-6L/min, treat system stability after, measure and the initial mass M of record sample 1
If test for nitriding atmosphere, will be evacuated down in the stove-0.097Mpa earlier, then the gas admittance valve of trial furnace is connected nitrogen cylinder, with flow logical nitrogen in stove of 2-64L/min, treat system stability after, measure and the initial mass M of record sample 1
The heating schedule of test will be determined with experiment type:
If test is continuous temperature-raising method, then the heating rate with 3-5 ℃/min heats up heating furnace, up to test temperature, measures and the temperature variant relation curve of record sample mass.
If test is intensification-constant temperature method, at first want confirmed test temperature and temperature retention time, the heating rate with 5-8 ℃/min heats up heating furnace then, is incubated after test temperature, and measurement and record sample are at the time dependent relation curve of insulation beginning back quality
Result and analysis:
According to the relation curve of quality-temperature in the experimental result or quality-time variation, judge the oxidation or the nitrogenize situation of sample.

Claims (10)

1、一种大试样耐火材料高温热重分析仪,包括真空气氛炉以及设置在真空气氛炉上的质量测量系统,其特征在于:该质量测量系统包括质量传感器(12),质量传感器(12)通过连接装置与设置在真空气氛炉中的耐高温吊篮(5)相连接。1. A high-temperature thermogravimetric analyzer for large sample refractory materials, comprising a vacuum atmosphere furnace and a quality measurement system arranged on the vacuum atmosphere furnace, characterized in that: the quality measurement system includes a mass sensor (12), a mass sensor (12 ) is connected with the high-temperature-resistant hanging basket (5) arranged in the vacuum atmosphere furnace through the connecting device. 2、根据权利要求1所述的一种大试样耐火材料高温热重分析仪,其特征在于:在质量传感器(12)下方连接有耐热丝(9),在耐热丝(9)下端连接有耐高温连接杆(7),耐高温吊篮(5)又与耐高温连接杆(7)相连接,在耐高温吊篮(5)上设置有可拆卸的耐高温吊篮底板(3)。2. A high-temperature thermogravimetric analyzer for large sample refractory materials according to claim 1, characterized in that: a heat-resistant wire (9) is connected below the mass sensor (12), and a heat-resistant wire (9) is connected to the lower end of the heat-resistant wire (9). The high temperature resistant connecting rod (7) is connected, the high temperature resistant hanging basket (5) is connected with the high temperature resistant connecting rod (7), and the high temperature resistant hanging basket (5) is provided with a detachable high temperature resistant hanging basket bottom plate (3 ). 3、根据权利要求1或2所述的一种大试样耐火材料高温热重分析仪,其特征在于:质量传感器(12)被密封在一个与炉体(16)相连接的一密封箱(10)内。3. A large-sample refractory high-temperature thermogravimetric analyzer according to claim 1 or 2, characterized in that: the mass sensor (12) is sealed in a sealed box ( 10) Inside. 4、根据权利要求3所述的一种大试样耐火材料高温热重分析仪,其特征在于:质量传感器(12)安置于密封箱(10)的底板上,质量传感器(12)的称量范围为0~5000g,分辨率为0.1~100mg。4. A high-temperature thermogravimetric analyzer for large sample refractories according to claim 3, characterized in that: the mass sensor (12) is placed on the bottom plate of the sealed box (10), and the weighing of the mass sensor (12) The range is 0~5000g, and the resolution is 0.1~100mg. 5、根据权利要求4所述的一种大试样耐火材料高温热重分析仪,其特征在于:耐高温吊篮(5)在炉膛(14)中的高低位置可以通过改变耐热丝(9)的长短来实现。5. A high-temperature thermogravimetric analyzer for large-sample refractory materials according to claim 4, characterized in that: the high and low positions of the high-temperature-resistant hanging basket (5) in the furnace (14) can be changed by changing the heat-resistant wire (9 ) length to achieve. 6、根据权利要求5所述的一种大试样耐火材料高温热重分析仪,其特征在于:耐热丝(9)通过耐热丝连接环(8)与耐高温连接杆(7)相连接,耐热丝(9)、耐热丝连接环(8)采用耐热金属制成,耐高温连接杆(7)、耐高温吊篮(5)及耐高温吊篮底板(3)由耐热刚玉制成,耐高温吊篮(5)可以放进截面积小于70.1×70.1mm的试样。6. A high-temperature thermogravimetric analyzer for large sample refractory materials according to claim 5, characterized in that: the heat-resistant wire (9) is connected to the high-temperature-resistant connecting rod (7) through the heat-resistant wire connecting ring (8) Connection, heat-resistant wire (9), heat-resistant wire connecting ring (8) are made of heat-resistant metal, high-temperature-resistant connecting rod (7), high-temperature-resistant hanging basket (5) and high-temperature-resistant hanging basket bottom plate (3) are made of heat-resistant Made of hot corundum, the high-temperature-resistant hanging basket (5) can be put into a sample whose cross-sectional area is less than 70.1×70.1mm. 7、根据权利要求6所述的一种大试样耐火材料高温热重分析仪,其特征在于:其质量测量系统可以承受小于5000g的重力,测试温度范围为25℃~1700℃,测试气氛可以是空气气氛、还原气氛和惰性气氛。7. A large-sample refractory high-temperature thermogravimetric analyzer according to claim 6, characterized in that: its mass measurement system can withstand a gravity of less than 5000g, the test temperature range is 25°C to 1700°C, and the test atmosphere can are air atmosphere, reducing atmosphere and inert atmosphere. 8、根据权利要求7所述的一种大试样耐火材料高温热重分析仪,其特征在于:质量传感器放置于炉顶部与炉体连接在一起的密封箱内,其信号线通过密封箱体上的接线端与外部控制系统相连。8. A large sample refractory high-temperature thermogravimetric analyzer according to claim 7, characterized in that: the mass sensor is placed in a sealed box connected to the furnace top and the furnace body, and its signal line passes through the sealed box The terminals on the board are connected to the external control system. 9、根据权利要求7所述的一种大试样耐火材料高温热重分析仪,其特征在于:耐高温连接杆是管状的,其下端有一对称的扦槽。9. A high-temperature thermogravimetric analyzer for large-sample refractory materials according to claim 7, characterized in that: the high-temperature-resistant connecting rod is tubular and has a symmetrical skewer groove at its lower end. 10、根据权利要求7所述的一种大试样耐火材料高温热重分析仪,其特征在于:耐高温吊篮底板的两侧有对称的缺口,当吊篮底板放到吊篮上时可以卡在吊篮提手型的框架上。10. A high-temperature thermogravimetric analyzer for large-sample refractory materials according to claim 7, characterized in that: there are symmetrical gaps on both sides of the bottom plate of the high-temperature resistant hanging basket, when the bottom plate of the hanging basket is placed on the hanging basket, it can Clamps on the handle-type frame of the gondola.
CN 200520030323 2005-03-29 2005-03-29 High temperature weight analyzer for large sample of refractory material Expired - Fee Related CN2844896Y (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103148892A (en) * 2013-02-01 2013-06-12 太原理工大学 Constant-pressure briquette coal carbonization process quality and volume measuring device
CN105067470A (en) * 2015-07-20 2015-11-18 重庆大学 Surface reaction detector and detection method thereof
CN111781085A (en) * 2020-07-23 2020-10-16 安徽中科磐信环保检测技术有限公司 Coal thermal behavior analysis testing arrangement

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103148892A (en) * 2013-02-01 2013-06-12 太原理工大学 Constant-pressure briquette coal carbonization process quality and volume measuring device
CN103148892B (en) * 2013-02-01 2015-03-04 太原理工大学 Constant-pressure briquette coal carbonization process quality and volume measuring device
CN105067470A (en) * 2015-07-20 2015-11-18 重庆大学 Surface reaction detector and detection method thereof
CN105067470B (en) * 2015-07-20 2017-08-25 重庆大学 A kind of surface reaction detection device and its method for detection
CN111781085A (en) * 2020-07-23 2020-10-16 安徽中科磐信环保检测技术有限公司 Coal thermal behavior analysis testing arrangement

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Granted publication date: 20061206