CN205934002U - Mechanical testing device is moved in online gas -solid - Google Patents

Mechanical testing device is moved in online gas -solid Download PDF

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Publication number
CN205934002U
CN205934002U CN201620827607.1U CN201620827607U CN205934002U CN 205934002 U CN205934002 U CN 205934002U CN 201620827607 U CN201620827607 U CN 201620827607U CN 205934002 U CN205934002 U CN 205934002U
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China
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reaction
gas
vacuum
vacuum furnace
solid
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CN201620827607.1U
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Chinese (zh)
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杨峰
刘静
熊茫茫
祝圆圆
马亚芹
杨闯
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Guizhou Education University
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Guizhou Education University
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Abstract

The utility model discloses a mechanical testing device is moved in online gas -solid, mix the gas system and connect the more than one gas cylinder on the gas system is mixed to the quality including the quality, the quality mix the gas system through the admission valve with preheat the vacuum furnace and be connected, preheat that the vacuum furnace passes through hot oil line and controllable solenoid valve is connected with the reaction vacuum furnace, react the vacuum furnace and pass through controllable discharge valve and is connected with vacuum system, be provided with pressure sensor and temperature sensor in reacting the vacuum furnace, controllable solenoid valve, controllable discharge valve, pressure sensor and temperature sensor pass through the control line and all be connected with control system. The utility model discloses can be accurate, the high efficiency measures reacting weight and time curves among the gas -solid reaction sequence, reaction mark and time curves, unit area reacting weight and time and concerns that isokinetic learns the test result, provides the theoretical direction for industrial production and scientific experiment.

Description

A kind of online gas-solid kinetic test device
Technical field
This utility model is related to a kind of online gas-solid kinetic test device, belongs to gas-solid reaction kinetic technical field.
Background technology
In the engineering fields such as metallurgy, material, chemical industry and the energy, gas-solid reaction has universality and importance.But for big For most gas-solid reaction processes, it is difficult to online dynamics data is monitored and record, so that we are to many reactions Process mechanism lacks understanding.The following is method employed in gas-solid reaction kinetic test and research for some researcheres:Yin Generation friend et al. have studied the research of austenite stainless steel melt nitrogen solubility behavior, is respectively by arranging experimental temperature:1550 DEG C, Take 2 in experimentation respectively, 5,10,15,20,25,40, the sample of 45min time, weigh with scale rustless steel nitriding process nitrogen The change of content, so that it is determined that whole process nitriding dynamic variation.All Pan Bing et al. have studied oxide layer to nitriding kinetics Impact, its nitriding method is:Reaction temperature is set to 550 DEG C, nitriding time be respectively 30min, 60min, 120min and 240min gas nitriding, is then weighed to the sample after pre-oxidation and different time nitriding with electronic balance, by the curve that increases weight To determine nitriding kinetics.Saeed N Ghali et al. is studied to alloy nitriding kinetics, reacts true in experimentation Empty stove needs to reach preset temperature in 1500-2100s, and four kinds of temperature must read pressure and exist:300、900、1800、3600、 7200th, 14400,21600, the 28800s stage, afterwards in H2Cool down under atmosphere, by using Kjeldahl method analysis measurement N2 Content.The dynamics research that Zhang Jinzhu et al. nitrogenizes to manganese metal, experimental temperature is 1143K;Vacuum resistance heating furnace enters Row nitrogen treatment, is respectively divided into 6 groups of samples, numbering 1-6, constant temperature nitriding time is followed successively by:0.5th, 1,2,3,4,6h, constant temperature nitriding Power-off after 0.5-6 hour, sample is cooled to below 500K in nitrogen containing atmosphere, by nitridation after sample take out from stove be placed in dry It is cooled further to room temperature in dry bottle, weighed with ten thousand/analytical balance, the gain in weight of Accurate Determining sample.
It follows that above-mentioned kinetic test is mostly using taking a little one by one, the method for areal survey is that is to say, that its power Learning curve is to be stacked up by the result of the test of multiple different time points.There are following some problems in such method of testing: Test process complicated and time consumption, each time point needs individually to test value, greatly reduces testing efficiency;Test error is big, Although the test to each testing site is same test conditions in theory, actually many tiny inherences and extrinsic factor Change can be superimposed and cause the amplification further of experimental error;There is no monitor in real time to course of reaction, for dynamic process, Often due to the property of reactant and surrounding medium is undergone mutation and is caused the mutation of reaction mechanism in course of reaction, traditional method Monitor in real time can not be carried out to these phenomenons, thus correct dynamic information cannot be obtained;Data processing complex, tradition is one by one The method of access point testing needs the dynamics data that each is put to calculate, and the actually sample of each time point, medium It is all incomplete same etc. parameter, so the process to data is also more complicated.
Utility model content
Utility model is directed to that the experimental data that traditional power method of testing exists is not accurate, efficiency is low, cannot be real-time The problem of monitoring, proposes that one kind is immediately online, simple and effective online gas-solid kinetic test device, this device can precisely, High efficiency measure gas-solid reaction during response magnitude and time curve, fraction reacted and time curve, unit plane Long-pending response magnitude and the dynamic test results such as time relationship, are commercial production and scientific experimentation provides theoretical direction.
The technical solution of the utility model:A kind of online gas-solid kinetic test device, including quality mix gas system and It is connected to the more than one gas cylinder that quality is mixed in gas system, described quality is mixed gas system and passed through intake valve and pre- heating vacuum furnace Connect, pre- heating vacuum furnace is passed through utilidor and controllable electromagnetic valve and is connected with reaction vacuum drying oven, and reaction vacuum drying oven passes through controlled row Air valve is connected with vacuum system, is provided with pressure transducer and temperature sensor in reaction vacuum drying oven, described controllable electric Magnet valve, controllable outlet valve, pressure transducer and temperature sensor are all connected with control system by data wire.
In said apparatus, described pre- heating vacuum furnace and reaction vacuum drying oven are vacuum tube furnace.
Due to adopting technique scheme, the utility model has the advantage of:It is real-time that this utility model passes through control system The data such as the temperature in collection reaction vacuum drying oven, pressure and time, and enter data in self-editing Excel data processing form Calculated, the weight by measuring the actual increase of sample is modified to result of calculation processing simultaneously, finally can obtain test Response magnitude in whole course of reaction for the system is anti-with time curve, fraction reacted and time curve, unit area Should measure and time relationship, be commercial production and scientific experimentation offer theoretical direction, reach experimental data during kinetic test Accurately, the purpose of efficiency high, monitor in real time.
Brief description
Fig. 1 is the structural representation of online gas-solid kinetic test device in this utility model;
Fig. 2 is TA2 industrially pure titanium thin plate carbo-nitriding kinetic curve in embodiment;
Fig. 3 is the independent nitriding kinetic curve of TA2 industrially pure titanium thin plate in embodiment.
Description of reference numerals:1- gas cylinder, 2- mixes gas system, 3- intake valve, the pre- heating vacuum furnace of 4-, 5- utilidor, and 6- can Control electromagnetic valve, 7- reacts vacuum drying oven, 8- controllable outlet valve, 9- control system, 10- pressure transducer, 11- temperature sensor, 12- Vacuum system.
Specific embodiment
In order that this utility model purpose, technical scheme and advantage are clearer, below in conjunction with the accompanying drawings to this utility model It is described in further detail.
Embodiment of the present utility model:The structural representation of online gas-solid kinetic test device is as shown in figure 1, include matter Amount is mixed gas system 2 and is connected to the more than one gas cylinder 1 that quality is mixed in gas system 2, and described quality is mixed gas system 2 and passed through Intake valve 3 is connected with pre- heating vacuum furnace 4, and pre- heating vacuum furnace 4 passes through utilidor 5 and controllable electromagnetic valve 6 with reaction vacuum drying oven 7 even Connect, reaction vacuum drying oven 7 is connected with vacuum system 12 by controllable outlet valve 8, in reaction vacuum drying oven 7, be provided with pressure transducer 10 and temperature sensor 11, described controllable electromagnetic valve 6, controllable outlet valve 8, pressure transducer 10 and temperature sensor 11 All it is connected with control system 9 by data wire.Described pre- heating vacuum furnace 4 and reaction vacuum drying oven 7 are vacuum tube furnace.
Using action of low-voltage pulse compound carbonitriding method and independent nitriding, TA2 industrially pure titanium is surface-treated in the present embodiment Two kinds of different process, its principle is as follows:
In titanium alloy nitriding process, Ti and N2Chemical reaction is occurred to generate titanium nitride, reactant N2It is gas, Ti is Solid, product titanium nitride is solid, and equally, it is also solid that N atom is solid-solution in-Ti.Therefore from the point of view of this reaction, It is the chemical reaction that a gas is constantly consumed.Ignore the change of solid volume before and after reaction, then volume before and after reaction Change the N that reacts of amount2Content.Therefore, if we can accurately monitor online in good time in airtight vacuum reaction tube Pressure it is possible to simply calculate the amount of the nitrogen being reacted away according to The Ideal-Gas Equation, and then acquires titanium alloy The amount of the actual growth in surface.
Specific experiment method is as follows:The cavity volume measuring reaction vacuum drying oven 7 is needed as known parameters before experiment.Test TA2 titanium alloy sample density, measure its surface area, then the pretreatment such as be ground, polish and clean;Sample is weighed It is placed in after (being accurate to 0.1mg) in the reaction vacuum drying oven 7 in response system, close the bell of reaction vacuum drying oven 7 and hunted leak Process;Inflation/deflation, with emptying furnace air, is subsequently vacuumed out repeatedly, and the experimental temperature of reaction vacuum drying oven 7 is respectively set as 800 ℃、850℃、900℃.Consistent with fire box temperature in order to ensure to be filled into every time the gas temperature in reaction vacuum drying oven 7, need by Question response gas carries out the pre-heat treatment, that is to say and gas is first passed through the pre- thermal vacuum consistent with reacting vacuum drying oven 7 design temperature Heated in stove 4, when pre- heating vacuum furnace 4 reaches design temperature, start for quality to mix the N that gas system 2 prepares2Or N2+C2H2 It is passed through in stove, pressure is -25kpa, after half an hour to be heated, the pre- heating vacuum furnace of connection 4 is opened by control system 9 true with reaction Controllable electromagnetic valve 6 between empty stove 7, gas is filled with the reaction vacuum drying oven 7 holding sample, in reaction vacuum drying oven 7 Pressure reaches setting value, now control system 9 start recording initial pressure value, temperature value and time;After 30min, inflation reaction Stage terminates, and data stores automatically;Control system 9 opens the controlled aerofluxuss between coupled reaction vacuum drying oven 7 and vacuum system 12 Valve 8, the gas in reaction vacuum drying oven 7 is discharged and is constantly in evacuation state;Circulation 24 hour pulse period of measurement successively The data such as the pressure value of each inflation section interior, temperature value and time;The furnace temperature of reaction vacuum drying oven 7 is dropped to room after terminating by experiment Temperature, takes out titanium alloy sample and weighs and record data.
After experiment terminates, at the data inputs such as the temperature of each experimental stage, pressure and time to self-editing Excel data Calculated in reason form;Result of calculation is modified process by measuring the sample actual weight that increases simultaneously.
The embodiment of self-editing Excel data processing Form Handle dynamics data:
Table 1 is applied to the Excel data processing table of thin plate nitridation reaction
Taking the pulse Vacuum nitridation reaction of thin titanium board material as a example:In form, known parameters include the initial weight of sample, end weighs, Length and tubular type furnace volume.Remainder parameter and meaning are as follows:
Area:Amassed by the specimen surface participating in reaction that the length of sample calculates;
Actual weightening:Before and after experiment, sample is carried out weighing and record weight after initial weight and test, calculate actual weightening;
Nitrogen response magnitude:Relative molecular mass (m=(△ PV/RT) the * M of pressure reduction * furnace volume/R* reaction temperature * nitrogenN2), Wherein △ P represents pressure reduction (Pa) before and after reaction, and V represents furnace volume (m3), R represents constant (8.314), and T represents reaction temperature (K), MN2Represent nitrogen relative molecular mass.
Unit area response magnitude:Nitrogen response magnitude (g)/titanium alloy plate area (m2).
Overall reaction amount:The superposition of pulse period nitrogen response magnitude, is equivalent to theoretical weight gain every time.
Unit area response magnitude (after correction):Actual weightening/the theoretical weight gain of unit area response magnitude *.
Overall reaction amount (after correction):Actual weightening/the theoretical weight gain of overall reaction amount *.
Fraction reacted (ξ):Overall reaction amount (after correction)/theory overall reaction amount.
These experimental datas will voluntarily calculate after inputting self-editing Excel data processing form, shows desired parameters value.
Referring to Fig. 2 and Fig. 3, the most at last the data input such as the temperature of each experimental stage, pressure and time to self-editing Excel In data processing form, response magnitude in vacuum pulse nitridation process for the titanium alloy and time curve, reaction point can be obtained Number and time curve, unit area response magnitude and time chart.

Claims (2)

1. a kind of online gas-solid kinetic test device, mixes gas system (2) including quality and is connected to the mixed gas system (2) of quality On more than one gas cylinder (1) it is characterised in that:Described quality is mixed gas system (2) and is passed through intake valve (3) and pre- thermal vacuum Stove (4) connects, and pre- heating vacuum furnace (4) is passed through utilidor (5) and controllable electromagnetic valve (6) and is connected with reaction vacuum drying oven (7), reaction Vacuum drying oven (7) is connected with vacuum system (12) by controllable outlet valve (8), is provided with pressure sensing in reaction vacuum drying oven (7) Device (10) and temperature sensor (11), described controllable electromagnetic valve (6), controllable outlet valve (8), pressure transducer (10) and Temperature sensor (11) is all connected with control system (9) by data wire.
2. online gas-solid kinetic test device according to claim 1 it is characterised in that:Described pre- heating vacuum furnace (4) and reaction vacuum drying oven (7) be vacuum tube furnace.
CN201620827607.1U 2016-08-02 2016-08-02 Mechanical testing device is moved in online gas -solid Expired - Fee Related CN205934002U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107904551A (en) * 2017-12-30 2018-04-13 贵州大学 Electromagnetic induction vacuum rapid carburization automation equipment

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107904551A (en) * 2017-12-30 2018-04-13 贵州大学 Electromagnetic induction vacuum rapid carburization automation equipment

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