CN103472073B - Based on iron ore analytical approach and the device of microwave resonance absorption - Google Patents

Based on iron ore analytical approach and the device of microwave resonance absorption Download PDF

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CN103472073B
CN103472073B CN201310438251.3A CN201310438251A CN103472073B CN 103472073 B CN103472073 B CN 103472073B CN 201310438251 A CN201310438251 A CN 201310438251A CN 103472073 B CN103472073 B CN 103472073B
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iron ore
magnetic field
microwave
composition
microwave resonance
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CN103472073A (en
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闻心怡
王磊
陈虹
钱家昌
赵爱国
肖前进
张辉意
夏兴隆
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719th Research Institute of CSIC
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Abstract

The present invention relates to the iron ore analytical approach based on microwave resonance absorption and device, described method comprises: iron ore powdered sample to be measured is placed in magnetic field space, and described magnetic field space comprises the orthogonal low frequency magnetic field of magnetic direction and high-frequency microwave magnetic field; Detect the microwave energy after iron ore powder absorption of sample under different low frequency magnetic field intensity; The microwave resonance absorption curve of iron ore powdered sample and the typical curve of various composition are compared, thus draws the ratio of composition in iron ore powdered sample and each composition.Described device comprises: microwave circulator, incident waveguide, the waveguide of detection waveguide short, three sections of waveguides connect into " T " font by microwave circulator.The present invention is by the microwave resonance absorption curve of described iron ore powdered sample under the different low frequency magnetic field of measurement, then the typical curve of microwave resonance absorption curve and each composition is compared, thus draw the ratio of composition in described iron ore powdered sample and each composition.

Description

Based on iron ore analytical approach and the device of microwave resonance absorption
Technical field
The present invention relates to the material phase analysis of composition in iron ore, refer to a kind of iron ore analytical approach based on microwave resonance absorption and device particularly.
Background technology
Iron ore is the mineral matter of iron content for refining the simple substance pig iron, steel-making, and its principal ingredient comprises: magnetic iron ore (Fe 3o 4), haematite (Fe 2o 3), limonite (FeO (OH)), ilmenite (FeTiO 3), siderite (FeCO 3), pyrite (FeS 2).Because the iron ore composition of Different sources exists huge difference, therefore, in exploitation, smelting or foreign trade checkout procedure, the composition determining iron ore is needed.
Traditional iron ore method of inspection mainly contains wet chemical analysis method and X-ray fluorescence spectra analytic approach.
Wherein, first wet chemical analysis method uses strong acid or highly basic to dissolve ore, re-use that different chemical reagent transforms, in precipitation solution different valence state mineral ion to measure.This method is at substantial time and energy not only, and relate to toxic chemical, to environment and operator ' s health unfavorable.
X-ray fluorescence spectra analytic approach is the principle that X ray characteristic spectrum fine structure can be caused to change based on different valence state element ion, the x-ray bombardment mineral dust of different-energy or different frequency is used when analyzing, the change of the X ray characteristic spectral line in detection of reflected light, then the composition of iron ore is quantitatively calculated in conjunction with corresponding software.But, the usual volume of XRF equipment is larger, be made up of the expensive accessory such as X-ray tube, high-voltage power supply and stable-pressure device, analyzing crystal, collimating apparatus, detecting device, impulse radiation analyzer, calibration meter, timer, integrator, register, vacuum pump, liquid nitrogen cooling system, operation and maintenance cost is all very high.
Therefore, be necessary to study a kind of can simply, the method for composition in quick, accurate analysis iron ore.
Summary of the invention
The object of the invention is overcome above-mentioned the deficiencies in the prior art and provide a kind of iron ore analytical approach based on microwave resonance absorption and device, and this analytical approach is simple, and analysis result is accurate, and this apparatus structure is simple, easy to use.
The technical scheme realizing the object of the invention employing is: a kind of iron ore analytical approach based on microwave resonance absorption, comprises the following steps:
Iron ore powdered sample to be measured is placed in magnetic field space, and described magnetic field space comprises the orthogonal low frequency magnetic field of magnetic direction and a high-frequency microwave magnetic field;
Change the intensity of described low frequency magnetic field, detect the microwave energy after described iron ore powder absorption of sample under different low frequency magnetic field intensity;
Integration is carried out to the microwave energy after described iron ore powder absorption of sample, obtains the microwave resonance absorption curve of described iron ore powdered sample;
The microwave resonance absorption curve of described iron ore powdered sample and the typical curve of various composition to be compared the composition obtained in described iron ore powdered sample, and obtain the ratio of each composition in described iron ore powdered sample compared with the microwave resonance curve of standard model.
In described acquisition described iron ore powdered sample, the ratio of each composition comprises:
Measure the standard microwave resonance curve of the heterogeneity of equal in quality respectively;
Calculate the typical ratio of each composition homologous thread institute area coverage in described standard microwave resonance curve;
With reference to the horizontal ordinate corresponding to described standard microwave resonance curve, each tie element in the microwave resonance absorption curve of described iron ore powdered sample is demarcated;
Use the peak of multimodal approximating method to each composition of microwave resonance absorption curve of described iron ore powdered sample to be separated, calculate the actual measurement ratio of each peak area coverage;
After being compared with identical component in actual measurement ratio by typical ratio again compared with other composition, thus obtain the mass ratio of each composition.
In addition, the present invention also provides a kind of iron ore analytical equipment based on microwave resonance absorption, and this device comprises:
One microwave circulator, it comprises three ports, described three ports being connected to incident waveguide, detecting waveguide and the short circuited waveguide for placing iron ore powdered sample to be measured, and described incident waveguide is located on a straight line with detection waveguide, described short circuited waveguide and described linear vertical;
One microwave source, is connected with described incident waveguide;
One electromagnet, comprises two iron cores, in the gap of described short circuited waveguide between described two iron cores; And
One detector diode, is connected with described detection waveguide;
The high-frequency microwave that described microwave source produces enters microwave circulator from incident waveguide, microwave circulator controls the transmission direction of high-frequency microwave, high-frequency microwave in incident waveguide is imported in short circuited waveguide, high-frequency microwave imports detection waveguide into through circulator again after short circuited waveguide bottom reflection, and the high-frequency microwave entered in short circuited waveguide is spatially mutually vertical with the low frequency magnetic field that electromagnet produces.
Further, described electromagnet also comprises:
One Helmholtz's modulation coil, is around on described two iron cores; And
One note amplifier, its output terminal is connected with described Helmholtz's modulation coil.
The present invention is according to the principle of microwave resonance absorption, iron ore powdered sample to be measured is placed in the magnetic field space in the orthogonal low frequency magnetic field of magnetic direction and high-frequency microwave magnetic field, by changing the intensity of described low frequency magnetic field, obtain the microwave resonance absorption curve after described iron ore powder absorption of sample under different low frequency magnetic field intensity, then the typical curve of microwave resonance absorption curve and each composition is compared, thus draw the ratio of composition in described iron ore powdered sample and each composition.
Accompanying drawing explanation
Fig. 1 is the structural representation of the iron ore analytical equipment that the present invention is based on microwave resonance absorption.
Number in the figure is: 1-microwave source, and 2-first coaxially turns waveguide adapter, 3-first isolator, the incident waveguide of 4-, 5-microwave circulator, 6-detects waveguide, 7-second isolator, 8-second coaxially turns waveguide adapter, 9-short circuited waveguide, 10-testing sample, 11-detector diode, 12-isolated amplifier, 13-gaussmeter, 14-hall probe, 15-electromagnet (wherein, 15.1-iron core, 15.2-modulation coil, 15.3-direct supply, 15.4-gap), 16-note amplifier, 17-lock-in amplifier, 18-computing machine, 19-GPIB card.
Fig. 2 is typical m (H dc) function curve diagram.
Fig. 3 is typical P abs(H dc) curve map.
Fig. 4 is the curve of the microwave resonance absorption power of testing sample and the absorption curve comparison chart of standard model.
Embodiment
Below in conjunction with meeting the drawings and specific embodiments, the present invention is described in further detail.
As shown in Figure 1, the iron ore analytical equipment that the present invention is based on microwave resonance absorption comprises: microwave circulator 5, incident waveguide 4, detection waveguide 6 and short circuited waveguide 9, microwave circulator 5 comprises three ports, three ports being connected to incident waveguide, detecting waveguide and the short circuited waveguide for placing iron ore powdered sample to be measured, three sections of waveguides connect into " T " font by three ports, i.e. described incident waveguide and to detect waveguide located on a straight line, described short circuited waveguide and described linear vertical thus form " T " font;
Microwave source 1 coaxially turns waveguide adapter 2 by first successively and is connected with incident waveguide 4 with the first isolator 3.
Detection waveguide 6 coaxially turns waveguide adapter 8 by the second isolator 7 and second successively and is connected with detector diode 9.
Testing sample 10 is housed in short circuited waveguide 9, and testing sample 10 is positioned at the low frequency magnetic field centre that electromagnet 15 produces.
Microwave source 1 is for generation of high-frequency microwave magnetic field, the frequency in this high-frequency microwave magnetic field is at X-band (in the present embodiment, X-band is according to IEEE521-2002 standard, frequency is at the radio waveband of 8-12GHz), the high-frequency microwave that microwave source 1 produces enters microwave circulator 5 from incident waveguide 4, microwave circulator 5 is for controlling the transmission direction of high-frequency microwave, high-frequency microwave in incident waveguide 4 is imported in short circuited waveguide 9, high-frequency microwave imports into through circulator again and detects waveguide 6 after short circuited waveguide 9 bottom reflection, the high-frequency microwave entered in short circuited waveguide 9 is spatially mutually vertical with the low frequency magnetic field that electromagnet 15 produces.
In the present embodiment, the low frequency magnetic field H that electromagnet 15 produces dc, H dcfor constant bias magnetic field, low frequency magnetic field H dcintensity is continuously adjustabe within the scope of 0 ~ 3500Oe, changes H dcsize, at each H dcunder value, by microwave circulator 5 control the microwave transmission that absorbs by testing sample 10 in detection waveguide 6, detect waveguide 6 and export detector diode 9 to, detector diode 9 detects at each H dcunder value, the microwave power P that testing sample 10 absorbs abs(H dc).
Power input P in incident waveguide 4 incbe expressed as:
P inc=P ref+P abs+P los+P det
In formula, P reffor the microwave power of reflection in incident waveguide 4, P absfor the microwave power that testing sample 10 absorbs in short circuited waveguide 9, P losfor the microwave power of loss, P detfor detector diode 11 is at the microwave power detecting waveguide 6 absorption.
Detector diode 11 output voltage V dbe proportional to the microwave power that testing sample 10 absorbs, that is:
V d=K dP det=K d(P inc-P ref-P abs-P los)
Because testing sample 10 is at constant external magnetic field H dceffect issues magnetisation, and the first magnetic moment in material can take external magnetic field as axle precessional motion.Owing to there is damping, this precessional motion can attenuate very soon, makes final first magnetic moment direction consistent with outer magnetic field direction.If but in precession plane be and constant external magnetic field H dcvertical plane applies a high-frequency microwave magnetic field, magnetic moment motion can absorb energy with the damping that contends with from high-frequency microwave magnetic field.When high-frequency microwave magnetic field is consistent with magnetic moment precession frequency, can resonate in magnetic moment precession and high-frequency microwave magnetic field, and now material absorbs high-frequency microwave magnetic field energy and reaches maximum.High-frequency microwave magnetic field can drive magnetic moment precessional motion in testing sample 10, therefore can absorb the microwave energy identical with its precessional motion frequency.The magnetic moment of each composition in testing sample 10, can be characterized by an absorption peak.Therefore, because the precession frequency of the different magnetic moment of an orbital electron of atoms outermost is different, by the microwave absorption peak of test material, the composition of material can be differentiated.The present invention detects detector diode 11 output voltage V dobtain the curve of the microwave resonance absorption power of testing sample 10, thus realize the discriminating to each composition of testing sample 10.
The microwave resonance absorption curve of described iron ore powdered sample can also be drawn the ratio of each composition in described iron ore powdered sample by the present invention compared with the microwave resonance curve of standard model, specifically comprises the following steps:
1) the standard microwave resonance curve of the standard model of certain mass heterogeneity is measured respectively.
2) the index plane ratio of each composition homologous thread institute area coverage in described standard microwave resonance curve is calculated; Suppose that in step 1), composition of getting is A, B, C..., then the typical ratio of A, B, C... standard microwave resonance curve area coverage is a1: b1: c1: ....
3) with reference to the horizontal ordinate corresponding to described standard microwave resonance curve, each tie element in the microwave resonance absorption curve of described iron ore powdered sample is demarcated.
4) use the peak of multimodal approximating method to each composition of microwave resonance absorption curve of described iron ore powdered sample to be separated, calculate the actual measurement ratio of each peak area coverage; After typical ratio is compared with identical component in actual measurement ratio again compared with other composition, thus obtain the mass ratio of each composition, namely suppose that in testing sample 10, composition A, B, C... corresponding peak area coverage is than being a2: b2: c2..., then each composition quality ratio is (a2/a1): (b2/b1): (c2/c1) ....
In the present invention, the microwave power absorbed due to testing sample 10 is very small and weak, cannot effectively directly be measured by prior art means, therefore, the iron ore analytical equipment that the present invention is based on microwave resonance absorption also provides a kind of preferred implementation, the microwave energy namely by adopting the method Measurement accuracy testing sample 10 of modulation /demodulation to absorb.In the present embodiment, electromagnet 15 comprises: two iron cores 15.1, the modulation coils 15.2 be around on two iron cores 15.1, and provide the direct supply 15.3 of power supply for electromagnet 15, wherein there is a gap 15.4 between two iron cores 15.1, the testing sample be positioned in short circuited waveguide 9 is arranged in this gap 15.4.In the present embodiment, modulation coil 15.2 used is Helmholtz's modulation coil.
The two ends of modulation coil 15.2 are connected with two output terminals of note amplifier 16 respectively, the input end of note amplifier 16 is connected with the reference frequency output terminal of lock-in amplifier 17, being connected with detector diode 11 by isolated amplifier 12 of lock-in amplifier 17, detector diode 5 is used for detecting the microwave power after testing sample 10 absorbs, and isolated amplifier 12 is used for the output signal of pre-amplification detector diode 11.
In this preferred embodiment, the reference frequency of lock-in amplifier 17 exports the input end connecting note amplifier 15, makes the frequency in amplitude modulation(PAM) magnetic field consistent with the reference frequency of lock-in amplify.The output of note amplifier 16 is connected on modulation coil 15.2, produces amplitude modulation(PAM) magnetic field to drive modulation coil 15.2 amplitude modulation(PAM) magnetic field H hthe low frequency magnetic field H produced with electromagnet 15 dcsuperposition forms low frequency magnetic field H t, H t=H t=H dc+ H hcos (ω t+ θ).In the present embodiment, amplitude modulation(PAM) magnetic field intensity is less than 100Oe, and the frequency of modulated magnetic field is 10 ~ 100Hz.
As the amplitude H in amplitude modulation(PAM) magnetic field hmuch smaller than Constant charge soil H dctime, changes of magnetic field Δ H tcaused absorption of sample changed power Δ P absmeet following linear relationship:
ΔP abs=mΔH t+C
In formula, m is P abs(H dc) slope under a certain stationary magnetic field, i.e. m=dP abs/ dH dc, typical m (H dc) function curve as shown in Figure 2.
Detector diode is exported V dwith the modulation signal H of low frequency magnetic field hcos (ω t+ θ) inputs lock-in amplifier 17 simultaneously, lock-in amplifier 17 output valve V qbe proportional in detector diode 11 output signal and the signal amplitude of modulating frequency same frequency part, that is:
V Q=-mK psdK d(V 0/2)H hsin(φ)
In formula, K psdfor the constant with the inner phase detector circuit relating to parameters of lock-in amplifier 17, φ is the difference of input signal and lock-in amplifier internal reference signal, and when lock-in amplifier 17 working stability, φ is a constant, V 0for the signal gain of the inner phase detector of lock-in amplifier 17.
The present invention uses detector diode 11 to pick up the microwave magnetic field after absorption of sample, and use lock-in amplifier 17 detects the slope that microwave magnetic field power changes with modulated magnetic field, by changing low frequency magnetic field H th dcpart, measures different H respectively dcm value corresponding to value, detects different H dcm value corresponding to value, by m to H dccarry out integration, draw the microwave resonance absorption power P of testing sample 10 abs(H dc), typical P abs(H dc) curve as shown in Figure 3.
The present embodiment is according to detector diode 11 output voltage V dobtain the curve of the microwave resonance absorption power of testing sample 10, by the curve of the microwave resonance absorption power of testing sample 10 and standard model (as Fe 3o 4, Fe 2o 3, FeO (OH), FeTiO 3, FeCO 3, FeS 2deng composition) absorption curve compare, the composition that each absorption peak is corresponding can be marked, as shown in Figure 4.
Conveniently Real-time Obtaining data, this embodiment also comprises gpib bus and connects computing machine 18, lock-in amplifier 17, direct supply 15.3 are connected on gpib bus, computing machine 18 is provided with for carrying out the GPIB card 19 of data communication with gpib bus, adopts Labview control survey system and image data.Hall probe 14 inserts in the gap 15.4 of two electromagnetic core middles, for measuring the magnetic field intensity of two pairs of electromagnetic core middles.The output terminal of hall probe 14 is connected with the input end of gaussmeter 13, and the output terminal of gaussmeter 13 is connected on gpib bus.

Claims (4)

1., based on an iron ore analytical approach for microwave resonance absorption, it is characterized in that, comprising:
Iron ore powdered sample to be measured is placed in magnetic field space, and described magnetic field space comprises the orthogonal low frequency magnetic field of magnetic direction and a high-frequency microwave magnetic field;
Change the intensity of described low frequency magnetic field, detect the microwave energy after described iron ore powder absorption of sample under different low frequency magnetic field intensity;
Integration is carried out to the microwave energy after described iron ore powder absorption of sample, obtains the microwave resonance absorption curve of described iron ore powdered sample;
The microwave resonance absorption curve of described iron ore powdered sample and the typical curve of various composition to be compared the composition obtained in described iron ore powdered sample, and obtain the ratio of each composition in described iron ore powdered sample compared with the microwave resonance curve of standard model.
2. according to claim 1 based on the iron ore analytical approach of microwave resonance absorption, it is characterized in that, in described acquisition described iron ore powdered sample, the ratio of each composition comprises:
Measure the standard microwave resonance curve of the heterogeneity of equal in quality respectively;
Calculate the typical ratio of each composition homologous thread institute area coverage in described standard microwave resonance curve;
With reference to the horizontal ordinate corresponding to described standard microwave resonance curve, each tie element in the microwave resonance absorption curve of described iron ore powdered sample is demarcated;
Use the peak of multimodal approximating method to each composition of microwave resonance absorption curve of described iron ore powdered sample to be separated, calculate the actual measurement ratio of each peak area coverage;
After being compared with identical component in actual measurement ratio by typical ratio again compared with other composition, thus obtain the mass ratio of each composition.
3. according to claim 1 or 2 based on the iron ore analytical approach of microwave resonance absorption, it is characterized in that: the magnetic direction of described low frequency magnetic field also superposes another amplitude modulation(PAM) magnetic field.
4., according to claim 3 based on the iron ore analytical approach of microwave resonance absorption, it is characterized in that:
Described low frequency magnetic field intensity continuously adjustabe within the scope of 0 ~ 3500Oe, described modulated magnetic field intensity is less than 100Oe;
The frequency in described high-frequency microwave magnetic field is within the scope of X-band, and X-band is the radio waveband of frequency at 8-12GHz; The frequency of described modulated magnetic field is 10 ~ 100Hz.
CN201310438251.3A 2013-09-24 2013-09-24 Based on iron ore analytical approach and the device of microwave resonance absorption Expired - Fee Related CN103472073B (en)

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CN106124529A (en) * 2016-07-07 2016-11-16 曹蕊 Iron content measurement apparatus in iron ore deposit
CN106996967B (en) * 2017-04-28 2023-08-22 成都哈工智传科技有限公司 Magnetic ore grade detection method and detection equipment

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