CN1479093A - Pyroelectric coefficient measuring method of tourmaline and its device - Google Patents
Pyroelectric coefficient measuring method of tourmaline and its device Download PDFInfo
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- CN1479093A CN1479093A CNA031282946A CN03128294A CN1479093A CN 1479093 A CN1479093 A CN 1479093A CN A031282946 A CNA031282946 A CN A031282946A CN 03128294 A CN03128294 A CN 03128294A CN 1479093 A CN1479093 A CN 1479093A
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Abstract
A device and method for measuring the pyroelectric coefficient of tourmaline is disclosed. Said method includes such steps as electrically and sequentially connecting two electrodes, operating amplifier and digital multimeter, heating tourmaline specimen to 130-170 deg.c, making its two end faces in contact with said two electrodes while making it in touch with contact-type digital thermometer, recording the measured data, and calculating its pyroelectric coefficient.
Description
Technical field
The present invention relates to a kind of pyroelectric coefficient measuring method and device thereof of measuring the method and the device thereof, particularly tourmaline of pyroelectric coefficient.
Background technology
Pyroelectricity field of detecting such as that pyroelectricity material is mainly used at present is infrared, laser are also used widely at the various types of radiation meter, spectrometer, and aspect such as infrared, laser detector.And pyroelectric coefficient is one of major parameter of measuring the infrared eye operating characteristic, so the method for testing of pyroelectric coefficient more and more is subjected to the great attention of Chinese scholars.The method of measurement pyroelectric coefficient has multiple, and the early stage method of usefulness once is the spontaneous polarization strength P in the ferroelectric hysteresis loop of measuring under the different temperatures
S, draw P
SWith the relation curve of T, obtain pyroelectric coefficient P by rate of curve
iValue, this method is also referred to as electric reversal process.People have proposed the basic skills of multiple measurement pyroelectric coefficients such as static method, constant speed heating, charge integration method, hot dynamic current method and dielectric heating since the seventies.Wherein comparatively simple, accurately with the charge integration method, and can satisfy the measurement of zero current field condition.Another kind of measuring method is the dynamic current method, adopts the modulation technology of heat source, studies under specific temperature conditions the dynamic pyroelectric response of measured material.This test macro such as can measure under constant temperature from the ferroelectric ceramics to the polymkeric substance at the pyroelectricity current-responsive of multiple material, also can be used for measuring the characteristic of lithium tantalate and the multiple geometric configuration sample of lithium niobate.Yet there are no report at the very little proving installation of tourmaline material pyroelectricity electric current.
Summary of the invention
The object of the present invention is to provide a kind of pyroelectric coefficient measuring method and measurement mechanism thereof of tourmaline, it can carry out pyroelectric coefficient to the very little tourmaline of pyroelectricity electric current and measure.
Technical scheme of the present invention is: the pyroelectric coefficient measuring method of tourmaline is characterized in that comprising the steps:
1), prepare the detection output unit of electric current: 2 electrodes 2 are connected with amplifying circuit with the integrated computing of electric current by lead respectively, and the integrated computing of electric current and the output terminal of amplifying circuit are connected with the sensitive multimeter that has digital watch;
2), tourmaline sample 3 is heated 130 ℃-170 ℃ in temperature control equipment;
3), from temperature control equipment, trip out the tourmaline sample 3 after the heating, the both ends of the surface of tourmaline sample 3 contact with 2 electrodes 2 respectively, the digitizing contact tehermometer is contacted with tourmaline sample 3 by sense line;
4), digitizing contact tehermometer, the respective value when the sensitive general-purpose that has a digital watch records tourmaline sample 3 air coolings, during data recording, be benchmark with the constant interval 10s end points of each time, the value of record pairing temperature this moment and electric current; With the constant interval of variation of temperature divided by the time, then obtain variation of temperature gradient delta T/ Δ t, the current value in should the interval when corresponding again certain temperature rate of change stablize by calculating, then can obtain the size of the pyroelectric coefficient value of tourmaline;
5), the pyroelectric coefficient of tourmaline calculates:
The parameter that characterizes tourmaline pyroelectricity characteristic is pyroelectric coefficient P.Its computing formula is:
P＝ΔPs/ΔT，
Be P=1/A * I * dt/dT,
Wherein, I is the current value of pyroelectricity, and unit is A; A is the area of tourmaline sample, and unit is m2; P is a pyroelectric coefficient, and unit is C/cm2K; Dt/dT is the ratio of time and temperature change amount, i.e. temperature rate of change.
Described 2 electrodes 2 are placed a glass sheet 5 on its top electrode 2, place a counterweight 1 on the glass sheet 5; Its bottom electrode 2 is placed on the marble slab 4.
Described electrode 2 is the aluminium flake electrode, the size of aluminium flake electrode and tourmaline sample big or small identical.
Described temperature control equipment is controllable temperature stove or electric hot plate.
The pyroelectric coefficient measuring device of tourmaline, it is characterized in that it is made up of detection output unit two parts of temperature control equipment and electric current, the detection output unit of electric current mainly is made up of integrated computing and amplifying circuit, the electrode 2 of digitizing contact tehermometer, the sensitive multimeter that has digital watch, electric current, 2 electrodes 2 are connected with amplifying circuit with the integrated computing of electric current by lead respectively, and the integrated computing of electric current and the output terminal of amplifying circuit are connected with the sensitive multimeter that has digital watch; The both ends of the surface of tourmaline sample 3 contact with 2 electrodes 2, and the digitizing contact tehermometer is contacted with tourmaline sample 3 by sense line; Described tourmaline sample 3 takes out air cooling for heat 130 ℃-170 ℃ in temperature control equipment after.
Linear basically because of electric sample temperature being reduced in below 100 ℃ in time, method of the present invention can be carried out pyroelectric coefficient to the very little tourmaline of pyroelectricity electric current and measured, and the present invention is simple in structure, and is easy to use.
Description of drawings
Fig. 1 is the detection output unit structural representation of electric current of the present invention
Fig. 2 is the influence curve figure of granularity to pyroelectricity
Wherein 1-counterweight, 2-electrode, 3-tourmaline sample, 4-marble slab, 5-glass sheet.
Embodiment
The pyroelectric coefficient measuring method of tourmaline comprises the steps:
1), prepare the detection output unit of electric current: 2 electrodes 2 are connected with amplifying circuit with the integrated computing of electric current by lead respectively, and the integrated computing of electric current and the output terminal of amplifying circuit are connected with the sensitive multimeter that has digital watch;
2), tourmaline sample 3 is heated 130 ℃-170 ℃ in temperature control equipment;
3), from temperature control equipment, trip out the tourmaline sample 3 after the heating, the both ends of the surface of tourmaline sample 3 contact with 2 electrodes 2 respectively, the digitizing contact tehermometer is contacted with tourmaline sample 3 by sense line;
4), digitizing contact tehermometer, the respective value when the sensitive general-purpose that has a digital watch records tourmaline sample 3 air coolings, during data recording, be benchmark with the constant interval 10s end points of each time, the value of record pairing temperature this moment and electric current; With the constant interval of variation of temperature divided by the time, then obtain variation of temperature gradient delta T/ Δ t, the current value in should the interval when corresponding again certain temperature rate of change stablize by calculating, then can obtain the size of the pyroelectric coefficient value of tourmaline;
5), the pyroelectric coefficient of tourmaline calculates:
The parameter that characterizes tourmaline pyroelectricity characteristic is pyroelectric coefficient P.Its computing formula is:
P＝ΔPs/ΔT，
Be P=1/A * I * dt/dT,
Wherein, I is the current value of pyroelectricity, and unit is A; A is the area of tourmaline sample, and unit is m
2P is a pyroelectric coefficient, and unit is C/cm
2K; Dt/dT is the ratio of time and temperature change amount, i.e. temperature rate of change.
As shown in Figure 1, the pyroelectric coefficient measuring device of tourmaline, it is made up of detection output unit two parts of temperature control equipment and electric current, the detection output unit of electric current mainly is made up of integrated computing and amplifying circuit, the electrode 2 of digitizing contact tehermometer, the sensitive multimeter that has digital watch, electric current, 2 electrodes 2 are connected with amplifying circuit with the integrated computing of electric current by lead respectively, and the integrated computing of electric current and the output terminal of amplifying circuit are connected with the sensitive multimeter that has digital watch; Tourmaline sample 3 takes out air cooling heat 130 ℃-170 ℃ in temperature control equipment after, and is contacted with 2 electrodes 2 by its both ends of the surface, and the digitizing contact tehermometer is contacted with tourmaline sample 3 by sense line.Described 2 electrodes 2 are placed a glass sheet 5 on its top electrode 2, place a counterweight 1 on the glass sheet 5, and its bottom electrode 2 is placed on the marble slab 4.Described electrode 2 is the aluminium flake electrode, the size of aluminium flake electrode and tourmaline sample big or small identical.The integrated computing and the amplifying circuit of electric current are prior art.
Described temperature control equipment is controllable temperature stove or electric hot plate, is prior art.1, design concept
Pyroelectricity electric current at tourmaline is very little by (10
-15-10
-12A), and the characteristics that are directly proportional with the temperature rate of change dT/dt of himself, its test macro can be divided into that temperature control part divides and the detection output of electric current.The temperature variation of sample heats it with the controllable temperature stove, makes the linear growth of one-tenth of its temperature.Adopted the method opposite with heat temperature raising---the air cooling method, in the hope of obtaining more stable chilling temperature gradient.Prove also below 100 ℃ that through experiment test sample temperature being reduced in certain temperature range in time is linear basically, so the method for alternating temperature is feasible.
For the detection output of pyroelectricity electric current, be 10 owing to there is not ready-made reometer can record the order of magnitude
-12The electric current of A, the design's device is directly exported results of weak current on digital multimeter through after the processing and amplifying to low current signal, so can obtain corresponding current value size.The measuring accuracy of this system is 10
-12A, and the size of measuring current value is generally at 10*10
-12More than the A, so because the labile factor of circuit can be similar to the influence of the pyroelectricity electric current that produced ignores, thereby reliability of testing result increased.2, assembling
The tourmaline sample is thickness 5mm, the disk of d=40mm, the heavy 13.5g of sample dry powder.Use aluminium flake as contact electrode during test, put a counterweight in the upper end of electrode top glass sheet, so that electrode contacts well with sample.Lower end electrode is isolated with marble slab.Sample is heated to about 150 ℃ back air cooling with the electric hot plate that can heat up more than 300 ℃.Because tested electric current is very faint, very easily be subjected to external interference, so big or small identical with the size of aluminium flake electrode and sample specially places the two ends of electric flag, can play screened effect, with the error that reduces to test.As shown in Figure 1.3, testing procedure
According to the basic demand of dynamic current method, connect peripheral test circuit (Fig. 1) earlier,, and stablize more than 1 minute the instrument zeroing.Simultaneously, the tourmaline sample is put on the electric hot plate heats, (more than 130 ℃) install sample rapidly by Fig. 1 when temperature is higher, treat that circuit stablizes more than 1 minute, and read-around ratio opening entry data during than steady change.During data recording, be benchmark with constant interval (10s) end points of each time, the value of record pairing temperature this moment and electric current.With the constant interval of variation of temperature divided by the time, then obtain variation of temperature gradient delta T/ Δ t, the current value in should the interval when corresponding again certain temperature rate of change is stablized by certain calculating, then can obtain the size of the pyroelectric coefficient value of tourmaline.4, the pyroelectric coefficient of tourmaline calculates
The parameter that characterizes tourmaline pyroelectricity characteristic is pyroelectric coefficient P.Its computing formula is:
P＝ΔPs/ΔT，
Be P=1/A * I * dt/dT,
Wherein, I is the current value (unit is A) of pyroelectricity, and A is the area (m of tourmaline sample
2), P is pyroelectric coefficient (C/cm
2K), dt/dT is the ratio (being temperature rate of change) of time and temperature change amount.
In the measuring process, taking 10s is a time period, writes down each point instantaneous temperature and the current value corresponding with it, thereby obtains the Changing Pattern of electric current with thermograde.In the test experiments of pyroelectricity electric current, sample I, the II of S, the mean grain size of III are followed successively by 28.65m, 19.15m and 4.94m; The mean grain size of sample I, the III of N is respectively 25.14m, 6.30m; Sample I, the II of X, the mean grain size of III are followed successively by 14.81m, 10.66m and 6.66m, I, II, three groups of samples of III are combination from coarse to fine, by repeatedly repeated measurement, with the error that maximum possible reduces to measure, the pyroelectric coefficient data after obtaining handling are as shown in table 1:
The pyroelectric coefficient test knot result of the different samples of table 1
| Sample | ??P ? ??(10 -7C/m 2·K) | Sample | ????P ? ????(10 -7C/m 2·K) | Sample | ????P ? ????(10 -7C/m 2·K) |
| ??S-I | ??0.843 | ??N-I | ????1.69 | ??X-I | ????1.96 |
| ??S-II | ??1.76 | ??X-II | ????2.48 | ||
| ??S-III | ??2.04 | ??N-III | ????2.37 | ??X-III | ????2.84 |
As known from Table 1, in same particle size range, compare, the pyroelectric coefficient maximum of X tourmaline, promptly for same temperature rate of change, the pyroelectricity electric current maximum that the X tourmaline produces, it is best that instant heating is released electrical effect, is N and S tourmaline secondly.5, the pyroelectricity characteristic of different grain size tourmaline
As shown in Table 1, sample in same particle size range, descending X, N and the S of being followed successively by of pyroelectric coefficient.For the tourmaline in every group of same place of production (as shown in Figure 2), along with diminishing of granularity, the pyroelectric coefficient of X, N and S three ground tourmaline is all increasing, but the amplitude that increases is slowed down gradually.6, temperature is to the influence of tourmaline pyroelectric property
Though the value of pyroelectric coefficient is only proportional with the variation of temperature rate, can see that by experiment the height of temperature is tangible to the influence of tourmaline pyroelectric effect.When the initial temperature variation was very fast, the pyroelectricity electric current can reach 10
-10More than the A.In the experimentation, if when the tourmaline sample is heated to maximum temperature 150-170 ℃, in the time of in temperature drops to same constant interval, the value of pyroelectricity electric current is apparently higher than being heated to maximum temperature when being 110-130 ℃, and this may be because the influence of the labile factor of the electric hysteresis effect of electric current or circuit.Although during measuring current, initial temperature and all conditions are consistent as far as possible, still, carried out repetitious experiment respectively to 7 groups of samples (every group 2 of the same race) of tourmaline, just determined the size of its pyroelectric coefficient.7, granularity is to the influence of tourmaline pyroelectric property
Though in the ultra-fine grinding process of tourmaline, the changes in crystal structure of tourmaline is little.But for pyroelectric coefficient, the sample granularity size has certain influence.Pyroelectric coefficient measurement result from X, N and S tourmaline, along with diminishing of granularity, pyroelectric coefficient is all increasing basically, but the amplitude that increases slows down gradually, reason wherein belongs to changes of crystal after the tourmaline ultra-fine grinding possibly, and this reason of going deep into tourmaline crystal structure inside is still waiting to analyze.
Claims (5)
1, the pyroelectric coefficient measuring method of tourmaline is characterized in that comprising the steps:
1), prepare the detection output unit of electric current: 2 electrodes (2) are connected with amplifying circuit with the integrated computing of electric current by lead respectively, and the integrated computing of electric current and the output terminal of amplifying circuit are connected with the sensitive multimeter that has digital watch;
2), tourmaline sample 3 is heated 130 ℃-170 ℃ in temperature control equipment;
3), from temperature control equipment, trip out the tourmaline sample (3) after the heating, the both ends of the surface of tourmaline sample (3) contact with 2 electrodes (2) respectively, the digitizing contact tehermometer is contacted with tourmaline sample (3) by sense line;
4), digitizing contact tehermometer, the respective value when the sensitive general-purpose that has a digital watch records tourmaline sample (3) air cooling, during data recording, be benchmark with the constant interval 10s end points of each time, the value of record pairing temperature this moment and electric current; With the constant interval of variation of temperature divided by the time, then obtain variation of temperature gradient delta T/ Δ t, the current value in should the interval when corresponding again certain temperature rate of change stablize by calculating, then can obtain the size of the pyroelectric coefficient value of tourmaline;
5), the pyroelectric coefficient of tourmaline calculates:
The parameter that characterizes tourmaline pyroelectricity characteristic is pyroelectric coefficient P.Its computing formula is:
P＝ΔPs/ΔT，
Be P=1/A * I * dt/dT,
Wherein, I is the current value of pyroelectricity, and unit is A; A is the area of tourmaline sample, and unit is m
2P is a pyroelectric coefficient, and unit is C/cm
2K; Dt/dT is the ratio of time and temperature change amount, i.e. temperature rate of change.
2, the pyroelectric coefficient measuring method of tourmaline according to claim 1 is characterized in that described 2 electrodes (2), and its top electrode (2) is gone up and placed a glass sheet (5), and glass sheet (5) is gone up and placed a counterweight (1); Its bottom electrode (2) is placed on the marble slab (4).
3, the pyroelectric coefficient measuring device of tourmaline, it is characterized in that it is made up of detection output unit two parts of temperature control equipment and electric current, the detection output unit of electric current mainly is made up of integrated computing and amplifying circuit, the electrode (2) of digitizing contact tehermometer, the sensitive multimeter that has digital watch, electric current, 2 electrodes (2) are connected with amplifying circuit with the integrated computing of electric current by lead respectively, and the integrated computing of electric current and the output terminal of amplifying circuit are connected with the sensitive multimeter that has digital watch; The both ends of the surface of tourmaline sample (3) contact with 2 electrodes (2), and the digitizing contact tehermometer is contacted with tourmaline sample (3) by sense line; Described tourmaline sample (3) takes out air cooling for heat 130 ℃-170 ℃ in temperature control equipment after.
4, the pyroelectric coefficient measuring device of tourmaline according to claim 3 is characterized in that described 2 electrodes (2), and its top electrode (2) is gone up and placed a glass sheet (5), and glass sheet (5) is gone up and placed a counterweight (1); Its bottom electrode (2) is placed on the marble slab (4).
5, the pyroelectric coefficient measuring device of tourmaline according to claim 3 is characterized in that described electrode (2) is the aluminium flake electrode, the size of aluminium flake electrode and tourmaline sample big or small identical.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102621400A (en) * | 2012-03-22 | 2012-08-01 | 河北工业大学 | Spontaneous polarization performance testing device for tourmaline powder materials |
| CN103558475A (en) * | 2013-11-08 | 2014-02-05 | 中国科学院上海硅酸盐研究所 | Method for detecting energy storage characteristic of ferroelectric ceramics |
-
2003
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102621400A (en) * | 2012-03-22 | 2012-08-01 | 河北工业大学 | Spontaneous polarization performance testing device for tourmaline powder materials |
| CN102621400B (en) * | 2012-03-22 | 2014-02-19 | 河北工业大学 | Spontaneous polarization performance testing device for tourmaline powder materials |
| CN103558475A (en) * | 2013-11-08 | 2014-02-05 | 中国科学院上海硅酸盐研究所 | Method for detecting energy storage characteristic of ferroelectric ceramics |
| CN103558475B (en) * | 2013-11-08 | 2016-05-18 | 中国科学院上海硅酸盐研究所 | A kind of method for detection of ferroelectric ceramics energy storage characteristic |
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