CN109521043A - A kind of electromagnetic heating metal phase diagram experimental method and test tube - Google Patents
A kind of electromagnetic heating metal phase diagram experimental method and test tube Download PDFInfo
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- CN109521043A CN109521043A CN201811538454.9A CN201811538454A CN109521043A CN 109521043 A CN109521043 A CN 109521043A CN 201811538454 A CN201811538454 A CN 201811538454A CN 109521043 A CN109521043 A CN 109521043A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/04—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of melting point; of freezing point; of softening point
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Abstract
The present invention relates to heater technical fields, more particularly to a kind of electromagnetic heating metal phase diagram experimental method and test tube, the present invention is initialized in system, the temperature of sample heating is set, whether there is the validity of load and load in single-chip microcontroller scanning heating furnace, avoids because of the excessive damage electronic component of electric current.After all input signals of system detection are normal, self-test passes through.After self-test passes through, instrument, which starts formally to export electric current, heats sample, and system acquires sample temperature in real time, and compared with temperature is arranged, and when lower than setting temperature, system continues to heat.After being higher than setting temperature, stop heating, start to cool down, while starting timing function, count down time is set as needed, and remind operator to write down temperature in corresponding interval, until experiment terminates.The present invention measures the relationship of temperature and time in temperature-fall period, draws inflection point and Cooling events in temperature-fall period, accurate phase transition temperature can be obtained.
Description
Technical field
The present invention relates to heater technical fields, and in particular to a kind of electromagnetic heating metal phase diagram experimental method and experiment
Test tube.
Background technique
Thermal analysis system is one of physical chemistry analytic approach, is one of basic skills of drawing diagram, it is based on object
With the principle of fuel factor when matter is undergone phase transition.Melt (metal, alloy or compound) is when uniform cooling, if not occurring to appoint
Then system temperature uniformly declines for what phase transformation.If phase transformation has occurred in cooling procedure, system temperature variation is just showed not
Equilibrium, and to will appear horizontal line section or turning point on cooling (or heating) curve (one time curve of temperature).Physics
In chemical experiment, Binary Alloy System phasor is obtained often through the cooling curve for making sample.By system from high temperature under level pressure
It gradually cools down, makees temperature to the change curve of time, as cooling curve.It, must be along with fuel factor, i.e., if system has phase transformation
It will appear turning point from cooling curve.
The previous way of cooling curve: method 1: sample cell is placed in hot plate, slow heating, completely molten to sample
Sample cell is clamped after change to be gently agitated for, and makes to form uniformity in pipe everywhere, one layer is also all equably covered on sample surfaces
Graphite powder.Thermocouple is fixed on sample cell center, about 3cm under sample liquid level is inserted into hot end, but should be not less than with tube bottom distance
1cm influences to avoid the external world.Control for Kiln Temperature increases 50 DEG C after with sample all fusing again to be advisable.Electric furnace is controlled with pressure regulator
Cooling rate, usually per minute decline 6 one 8 DEG C.A temperature is read every 30s, until temperature drops to 110 DEG C of end.
Method 2: as shown, using hyaloid quality control (be added metal to be measured among sample cell, upper envelope atoleine, every
Anoxybiotic gas), there is closed glass inner hole in centre, for being inserted into thermocouple, measures the temperature of sample mixed metal.Sample is put into and is added
In hot stove, using resistance heating, is transmitted by heat and carry out sample heating.The variation of sample temperature is observed, Control for Kiln Temperature is with sample
Product increase 50 DEG C after all melting again to be advisable.With the cooling rate of pressure regulator control electric furnace, usually 3 one 5 DEG C of decline per minute.
A temperature is read every 30s, until temperature drops to 150 DEG C of end.
This method 1 has the drawback that:
1, it when the temperature that sensor is shown reaches 80-90 DEG C it is necessary to turn off hot plate, is allowed using the residual temperature of hot plate
Sample is completely melt.The purpose for the arrangement is that in order to protect thermocouple.However the fact is that, for using the people of this instrument for the first time
For, even if drumming in prompting to them, the temperature that they heat can all be much higher than predetermined temperature, cause each time with a large amount of
Thermocouple is burned, scraps；
2, two component alloy phase diagram devices of current market sale, it is not only on the high side, and design relative complex.Mechanical part
When machine operation, noise is big, abrasion is big, has pollution to environment；
3, original equipment does not have fast-refrigerating program, this makes every group of plan that must acquire five groups of experimental datas in the original plan,
It is compressed to two groups.And experimental period is too long, does not meet demand rapidly and efficiently at present.
This method 2 has the drawback that:
1, resistance heating thermal inertia is big, and temperature control is relatively difficult, it is easy to be heated on design temperature, atoleine is caused to boil
It rises, sample is rotten.
If closing heating in advance 2, for temperature control, it be easy to cause heating insufficient in this way, sample melts uneven.
3, this is emphasis: it is heated, as long as sample melts, we mainly measure in temperature-fall period temperature and when
Between relationship, draw figure line temperature-fall period in inflection point and Cooling events.But due to stopping after heating, between sample and room temperature
The temperature difference is formed, since the temperature difference increases, the rate of temperature fall of unit time sample is possible to cause sample (to coagulate to transformation temperature than very fast
Solid point) temperature when, have little time to undergo phase transition temperature and just lower down.Occur surfusion on cooling curve, is unable to get
Accurate phase transition temperature, the error for causing phasor to be drawn are larger.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of electromagnetic heating metal phase diagram experimental method and test tube,
Temperature can be more accurately controlled, improved test tube is matched with electromagnetic heating metal phase diagram experiment instrument, reduces waste heat to system
Influence, can be obtained accurate phase transition temperature, the error that phasor is drawn is smaller, and substantially reduces experimental period, reduces experiment
The spoilage of instrument.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of electromagnetic heating metal phase diagram experimental method, it is characterised in that: the described method comprises the following steps:
S1 system initialization, and the temperature of sample heating is set；
Whether there are load, and the validity of load in S2 single-chip microcontroller scanning heating furnace；
After all input signals of S3 system detection are normal, self-test passes through；
After S4 self-test passes through, instrument starts formally to export electric current to sample progress electromagnetic heating；
S5 system acquires sample temperature in real time, and when collecting temperature value is lower than setting temperature, system continues to heat；
After S6 collecting temperature value is higher than setting temperature, stops heating, start to cool down, while starting timing function；
Count down time is set as needed in S7, reminds operator to write down temperature in corresponding interval, until experiment terminates.
Preferably, in the S1, single-chip microcontroller adds according to the direct relationship of size and the two for outputting and inputting electric current, scanning
Whether load, and the validity of load are had in hot stove.
Preferably, in the S3, if breaking down, system stops output electric current, shows screen display event in instrument panel
Hinder type, help the timely inspection apparatus of user there are the problem of.
Preferably, in the S5, the sample temperature that thermocouple detects is transferred to single-chip computer control system by AD capture card.
A kind of electromagnetic heating metal phase diagram test tube, including test tube, it is characterised in that: including test tube inner tube and cast iron sleeve
Pipe, the test tube inner tube are arranged in the test tube, and atoleine is equipped in the test tube, is soaked with metal in the atoleine
Sample, the test tube and offers test tube entrance, and temperature sensor is equipped in the test tube inner tube.
Preferably, after the test tube being put into heating furnace, under electromagnetic heating effect, cast-iron socket starts to generate heat, then with
The form of heat transfer heats sample in pipe, and armoured thermocouple gos deep into sample interior, detection sample temperature and Real-time Feedback, reaches
When set temperature, host stops output electric current, and heating stops.
Preferably, the test tube is matched with electromagnetic heating metal phase diagram experiment instrument, and cast-iron socket drops simultaneously with sample
Temperature.
(3) beneficial effect
1, it solves to allow sample to be completely melt due to the residual temperature using hot plate, the temperature of heating all can be much higher than regulation temperature
Degree, causes the problem of being burned, scrap each time with a large amount of thermocouples.
2, experiment duration is greatly shortened, increases conventional efficient, has the characteristics that rapidly and efficiently.
3, temperature control is more accurate, and sample will not be made rotten.
4, the relationship of temperature and time in temperature-fall period is measured, inflection point and Cooling events in figure line temperature-fall period are drawn,
Accurate phase transition temperature can be obtained, the error that phasor is drawn is smaller.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is flow chart of the method for the present invention；
Fig. 2 is the structural schematic diagram of test tube of the present invention；
Fig. 3 is the cooling curve of sample；
Label in figure respectively represents:
1-temperature sensor；2-test tube inner tubes；3-atoleines；4-cast-iron sockets；5-test buttons；6-test tubes enter
Mouthful.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without creative efforts, shall fall within the protection scope of the present invention.
Embodiment 1
System is initialized when this method as shown in Figure 1 starts, the temperature that setting sample heats, not due to electromagnetic heating technique
There are waste heat, temperature setting is generally being higher than 40 ~ 50 DEG C of sample fusing point of position in this experiment.Single-chip microcontroller according to input and
The size and the direct relationship of the two of electric current are exported, whether in heating furnace have load, and the validity of load if scanning, avoids
Because of the excessive damage electronic component of electric current.
The sample temperature that thermocouple detects is transferred to single-chip computer control system, all inputs of system detection by AD capture card
After signal is normal, self-test passes through.As broken down, system stops output electric current, shows screen display failure classes in instrument panel
Type, help the timely inspection apparatus of user there are the problem of.
After self-test passes through, instrument, which starts formally to export electric current, heats sample, and system acquires sample temperature in real time, and
Compared with temperature is arranged, when lower than setting temperature, system continues to heat.After being higher than setting temperature, stops heating, start to drop
Temperature, while starting timing function, count down time is set as needed, and remind operator to write down temperature in corresponding interval
Degree, until experiment terminates.
Embodiment 2
A kind of electromagnetic heating metal phase diagram test tube as shown in Figure 2, including test tube, further include test tube inner tube and cast iron sleeve
Pipe, the test tube inner tube are arranged in the test tube, and atoleine is equipped in the test tube, is soaked with metal in the atoleine
Sample, the test tube and offers test tube entrance, and temperature sensor is equipped in the test tube inner tube.
Electromagnetic heating requires heated body to be necessary for magnetic conductive material.The outside of teat glass is measured in original metal phase diagram,
Nested cast-iron socket can satisfy electromagnetism since cast iron has preferable magnetic conductivity, higher resistance and high heat conductivity
The receptor requirements of heating.After improved test tube is put into heating furnace, under electromagnetic heating effect, cast-iron socket starts to generate heat,
Sample in pipe is heated in the form of heat transfer again, armoured thermocouple gos deep into sample interior, detection sample temperature and Real-time Feedback,
When reaching set temperature, host stops output electric current, and heating stops.Cast-iron socket cools down simultaneously with sample.Improved test tube with
Electromagnetic heating metal phase diagram experiment instrument matches, hence it is evident that reduces influence of the waste heat to system, can satisfy requirement of experiment.
To verify beneficial effects of the present invention, using a kind of electromagnetic heating metal phase diagram experimental method and test tube pair
Metallic tin (Sn) is heated, and surveys and draws the cooling curve of the metal, is included the following steps:
1, sample is configured
Metallic tin 50g is weighed with precision balance and is added to common pure glass metal phasor sample cell 1, weighs 50g metallic tin and 10g
Metal iron powder is added to after mixing in the metal phase diagram sample cell 2 equipped with cast-iron socket, is separately added into 20mL atoleine
Into sample cell sample 1,2, metal oxidation deterioration is prevented.
2, sample test
Metal phase diagram sample cell 1 is put into traditional metal phase diagram heating instrument heating furnace, insertion temperature sensor to sample
Quality control, open metal phase diagram experiment instrument, be arranged heating temperature to 280 DEG C, instrument is begun to warm up, and use manual time-keeping, due to biography
The metal phase diagram heating device of system uses electric-heating-wire-heating technology, and electrothermal wire heating's temperature increases first after energization, utilizes temperature
Difference generates heat transfer, successively transfers heat to burner hearth, sample cell, sample and is inserted into the sensor of sample interior, there are hysteresis.
When sample is warming up to setting temperature, stops heating and record the time.Due to the presence of thermal inertia, sample will continue to heat up, and see
Sample ramp case is examined, the maximum temperature of heating is recorded, records the time.When sample starts to cool to 280 DEG C, opens and fall to count
When, 30s timing records temperature every 30s, cools to 150 DEG C, terminates test.
Metal phase diagram sample cell 2 is put into the heater dedicated electromagnetic heating furnace of a kind of metal phase diagram of the invention, is adopted
It is tested with a kind of electromagnetic heating metal phase diagram experimental method and test tube.Temperature sensor is inserted into sample cell,
It opens corresponding metal phase diagram experiment instrument, is arranged 360 DEG C of heating temperature, instrument is begun to warm up, and with manual time-keeping, electromagnetic heating
The high frequency magnetic field that furnace generates acts on the iron powder of the outer cast-iron socket of sample cell and dispersion in the sample, and the magnetic line of force is cut, and is produced
Raw countless micro cyclone streams keep casing and iron powder itself heating up rapidly, and are conducted to sample to be tested, since electromagnetic heating is non-
Contact heating has the characteristics that the rate of heat addition is fast, thermal inertia is small.When sample is warming up to setting temperature, electromagnetic heating stops.
After waste heat slightly promotes sample temperature, sample i.e. start to cool down, at this time when temperature be lower than set temperature when, electromagnetic heating furnace after
Continuous low-power heating stops again after reaching set temperature.Electromagnetic heating furnace intermittent work, maintain sample setting temperature, 3 points
Zhong Hou closes electromagnetic heating furnace.Radiator fan continues working in this process, dispels the remaining of electromagnetic heating furnace and sample cell rapidly
Heat prevents further heating up for sample.After sample starts cooling, countdown 30s is opened, temperature is recorded every 30s, sees simultaneously
Rate of temperature fall is examined, if rate of temperature fall is more than 3 ~ 5 DEG C/min, closes radiator fan, and adjust heating power, sample is cooled down fast
Rate controls after 3 ~ 5 DEG C/min, maintains instrument standing state, by prompt record temperature data, and observes the variation of sample temperature
Situation.When cooling to 150 DEG C, terminate test.
3, cooling curve is drawn
According to the sample temperature value that experiment obtains, in origin software, using the time as abscissa, sample temperature is ordinate,
Draw the time of sample and the change curve of temperature, i.e. cooling curve.Due to pure metal tin system, when sample reaches in temperature-fall period
To when solid-liquid biphase equilibrium, system freedom degree is 0, and sample temperature does not change over time, and horizontal line section occurs in cooling curve, until
Until sample solidifies completely, system temperature continues to decline.Inflection point and the corresponding temperature of platform on cooling curve occur solid for sample
The temperature value that liquid phase becomes.
1 metal phase diagram sample of table heats used time and heating rate table
| Sample type | Heating method | Sample initial temperature (DEG C) | It is heated to 280 DEG C of time-consumings (second) | Heating rate (DEG C/sec) | Highest heats up (DEG C) |
| Sample cell 1 | Electric-heating-wire-heating | 20 | 213 | 1.28 | 342 |
| Sample cell 2 | Electromagnetic heating | 20 | 62 | 4.2 | 315 |
Seen from table 1, the sample cell 1 measured using the metal phase diagram analyzer of traditional electric-heating-wire-heating, due to thermal conduction rate
Relatively slow, there are certain hysteresis, are heated to 280 DEG C of time-consumings at 213 seconds, higher than the sample cell 2 of electromagnetic heating from room temperature.Electricity
The heating rate of magnetic heating reaches 3.28 times of electric-heating-wire-heating.Simultaneously because the thermal inertia of electric-heating-wire-heating is larger, temperature control effect
Fruit is poor, stop heating after, inertia heat up 60 ~ 70 DEG C, and electromagnetic heating due to temperature control precisely and radiator fan effect, inertia liter
30 ~ 40 DEG C of temperature.
From the cooling curve of Fig. 3 sample it can be seen that conventional metals phasor analyzer is unable to accurately control rate of temperature fall, lead
Cause its rate of temperature fall very fast, apparent surfusion occurs in curve A, causes the phase transition temperature error read larger.And electromagnetism adds
Thermography instrument can accelerate cooling using fan in temperature-fall period or be slowed down using the electromagnetic heating of low-power as compensation heat
Rate of temperature fall achievees the effect that control cooling.There is apparent platform in curve B, and phase transition temperature measurement accuracy is high, and error is small.This
A kind of electromagnetic heating metal phase diagram experimental method and test tube of invention, by the way of electromagnetic heating, experimental method step
It is rapid reasonable, it is easy to operate, the accuracy of experiment is improved, there is very strong creativeness.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (7)
1. a kind of electromagnetic heating metal phase diagram experimental method, it is characterised in that: the described method comprises the following steps:
S1 system initialization, and the temperature of sample heating is set；
Whether there are load, and the validity of load in S2 single-chip microcontroller scanning heating furnace；
After all input signals of S3 system detection are normal, self-test passes through；
After S4 self-test passes through, instrument, which starts formally to export electric current, heats sample；
S5 system acquires sample temperature in real time, and when collecting temperature value is lower than setting temperature, system continues to heat；
After S6 collecting temperature value is higher than setting temperature, stops heating, start to cool down, while starting timing function；
Count down time is set as needed in S7, reminds operator to write down temperature in corresponding interval, until experiment terminates.
2. electromagnetic heating metal phase diagram experimental method according to claim 1, it is characterised in that: in the S1, single-chip microcontroller
Whether according to the direct relationship of size and the two for outputting and inputting electric current, scanning has load in heating furnace, and load have
Effect property.
3. electromagnetic heating metal phase diagram experimental method according to claim 1, it is characterised in that: in the S3, if occurring
Failure, system stop output electric current, show screen display fault type in instrument panel, the timely inspection apparatus of user is helped to deposit
The problem of.
4. electromagnetic heating metal phase diagram experimental method according to claim 1, it is characterised in that: in the S5, thermocouple
The sample temperature detected is transferred to single-chip computer control system by AD capture card.
5. a kind of electromagnetic heating metal phase diagram test tube, including test tube, it is characterised in that: including test tube inner tube and cast iron sleeve
Pipe, the test tube inner tube are arranged in the test tube, and atoleine is equipped in the test tube, is soaked with metal in the atoleine
Sample, the test tube and offers test tube entrance, and temperature sensor is equipped in the test tube inner tube.
6. electromagnetic heating metal phase diagram test tube according to claim 5, it is characterised in that: be put into the test tube and add
After hot stove, under electromagnetic heating effect, cast-iron socket starts to generate heat, then is heated in the form of heat transfer to sample in pipe, armouring
Thermocouple gos deep into sample interior, detection sample temperature and Real-time Feedback, and when reaching set temperature, host stops output electric current, adds
Heat stops.
7. electromagnetic heating metal phase diagram test tube according to claim 5, it is characterised in that: the test tube adds with electromagnetism
Thermometal phase diagram experimental instrument matches, and cast-iron socket cools down simultaneously with sample.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811538454.9A CN109521043A (en) | 2018-12-17 | 2018-12-17 | A kind of electromagnetic heating metal phase diagram experimental method and test tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811538454.9A CN109521043A (en) | 2018-12-17 | 2018-12-17 | A kind of electromagnetic heating metal phase diagram experimental method and test tube |
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Application publication date: 20190326 |