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.
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.