CN1128355C - Method and device for measuring resistivity of carbon-contained refractory material - Google Patents
Method and device for measuring resistivity of carbon-contained refractory material Download PDFInfo
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- CN1128355C CN1128355C CN 99122288 CN99122288A CN1128355C CN 1128355 C CN1128355 C CN 1128355C CN 99122288 CN99122288 CN 99122288 CN 99122288 A CN99122288 A CN 99122288A CN 1128355 C CN1128355 C CN 1128355C
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Abstract
The present invention relates to a method suitable for continuously measuring the resistivity of refractory material along with temperature changes, and equipment thereof. The present invention belongs to the field of the measurement of refractory material. The equipment is formed by that a measured test sample coated with oxidation prevention paint is clamped on a fixed seat in a stove body, a proper amount of pressure is applied to the test sample by a machine conducting mechanism according to the requirements of the designer, and heating is protected by protective gas in order to prevent the test sample from oxidizing during measurement. Compared with the prior art, the test method and the equipment of the present invention have the advantages of wide measuring range, high measuring precision, strong comparability, comparative time saving and economy.
Description
Technical field
The invention belongs to the fields of measurement of fire resistive material.Be specially adapted to the method and apparatus of the resistivity continuous coverage of carbon containing refractory the time with temperature change.
Background technology
Along with smelting technique constantly develops, the fire resistive material of smelting body of heater is also in continuous improvement, and the carbon material that for example adds in fire resistive material has graphite or coke etc., and the electrical property of its refractory aggregate is improved.In the prior art, use the conducting Mg-C brick of content of graphite on some direct current electric arc furnace and the tundish, be used as electrode and used at 8-20%.It is good that its reason is that this refractory brick itself has usability, and the life-span is long, and being used in the high temperature resistant furnace lining electrode is good conduction refractory.In the main operation parameter of such fire resistive material, key is to measure the temperature variant resistivity of fire resistive material at present.In the prior art, measuring method to resistivity of carbon-contained refractory material is very simple, for preventing the oxidation of charcoal element in the fire resistive material, earlier sample to be tested is embedded in that pre-burning stops burning in the charcoal element such as coke to design temperature, treat to measure again behind the sample cool to room temperature resistivity value of sample.Adopting the major defect of the measured fire resistive material resistivity value of said method is to reflect the resistivity value of fire resistive material with temperature change the time continuously truly, and measurement range is narrow, can't get rid of extraneous protection charcoal to the interference of sample measurement value etc.
Summary of the invention
Resistivity value when the objective of the invention is to propose a kind of can the continuous coverage fire resistive material varying with temperature, and measuring accuracy height, wide ranges and economic measuring method and equipment.
According to purpose of the present invention; the method of testing of the fire resistive material resistivity that we proposed and equipment must be measured in anti-oxidation protective atmosphere; testing apparatus should guarantee that tested sample raises with furnace temperature and test resistance rate under pressure constant state when sample expands, so measured value has comparability.Accompanying drawing according to the present invention below comes method and apparatus of the present invention is described in detail, this accompanying drawing is the structural representation of resistivity of carbon-contained refractory material testing apparatus of the present invention, can find out with reference to the accompanying drawings, the composition of present device is a dress heating furnace 5 on furnace body support 12, calandria 8 and thermometric galvanic couple 10 should link with temperature controller 7, it is characterized in that the sample to be tested 6 two ends cards in heating furnace 5 have holder 9, one end holder 9 should fixedly mount with the furnace wall, and other end holder 9 should with curved push rod 3 front end suits, the middle part of curved push rod 3 should be by stationary shaft 4 location, counterweight weights 2 should be equipped with in the rear end of curved push rod 3, and the high temperature resistant test lead 13 that is equipped with respectively in the inboard of the outside, the two ends of sample to be tested 6 and holder 9 should link with direct current bridge 1.Also have at the further feature of method of testing of the present invention and equipment and to be equipped with in the heating furnace 5 and the gas piping 11 of protecting source of the gas to communicate; all stud with high temperature ceramic material at the curved push rod 3 of Contact Heating stove 5 and the front end of gas piping 11; holder 9 is high temperature ceramic material and makes, and above-mentioned high temperature ceramic material should comprise Al
2O
3, MgO, SiO
2, ZrO
2, any one or two or more the compound ceramic material product among SiC, the SiN.For improving testing precision; what adopted in accompanying drawing of the present invention is direct-flow double bridge test structure synoptic diagram; this method of testing be holder 9 inboard with sample to be tested 6 two ends outside respectively accompany fire-resistant material sample with sample to be tested 6 identical materials; the measurement port of every block of material standard specimen should with holder 9; the measurement port of sample to be tested 6 parallels; and by high temperature resistant test lead order A; a; B; b; C; c; D; the d sequence number is corresponding to be connected; adopting employed blanket gas in the method for testing of direct-flow double bridge in the present invention is any one gas in argon gas or the nitrogen; in test sample to be tested 6 exert pressures are 0.1MPa-2.0MPa, applying method is to reach the size that adjusting is exerted pressure to sample by changing counterweight weights 2 amounts.Should scribble one deck antioxidation coating coating on the surface of sample to be tested 6, this coating should include Al
2O
3, B
2O
3, SiO
2, any one or two or more composite dopes among the SiC.
The test implementation of method of testing of the present invention and equipment is that the sample to be tested surface is evenly scribbled antioxidizing paint; after treating the coating drying; again sample is loaded in the holder; and clamp high temperature resistant test lead test side in order respectively; the end in addition of high temperature resistant test lead also should insert on the registering instrument of direct-flow double bridge in order; load an amount of counterweight counterweight by deviser's requirement at curved push rod end then; by curved push rod set pressure is applied on holder and the sample to be tested; heat this moment under protective atmosphere; simultaneously can measure and be recorded under the constant pressure, the variation of sample resistivity value at that time when different temperatures.
Adopt method of testing of the present invention and equipment to have following characteristics compared with prior art, measurement range is wide, can be from the resistivity value of the high-temperature continuous measurement sample more than the room temperature to 1600 ℃.Measuring accuracy is high and comparability is strong, to sample to be tested is to carry out relative static measurement in the environment of constant temperature and pressure and eliminating conduction external interference, because sample to be tested two ends port and the contact force of measuring lead, be to adopt present device to exert pressure according to the desired mechanical conductive of deviser, therefore the way of contact of high temperature resistant measurement lead and sample is the measuring method of exerting pressure, can avoid like this, because of volume of sample is changed, cause the change of measuring point place pressure and the increase of measuring error factor.
Description of drawings
1 is the direct current bridge registering instrument in the accompanying drawings, and 2 is the counterweight counterweight, and 3 is curved push rod, and 4 is stationary shaft, and 5 is heating furnace, 6 is sample to be tested, and 7 is temperature controller, and 8 is heater, and 9 is holder, 10 is the thermometric galvanic couple, and 11 is gas piping, and 12 is furnace body support, and 13 is high temperature resistant test lead.A, B, C, D and a, b, c, d are corresponding each union end label in the high temperature resistant test lead.
Embodiment
Deviser of the present invention is the Performance Detection contrast test that the graphite magnesia carbon brick sample of employing carbon containing 14% is done; the high temperature resistant test lead that various experiment is adopted is siderochrome matter test lead; the SiN ceramic that various high temperature ceramic materials are then selected for use; the blanket gas that adopts when adding thermal measurement is an argon gas; the detection method of contrast test is the charcoal method of burying of the prior art; because survey cumbersome; so we have only detected five temperature spots; be cooled to the resistivity of room temperature, and list in and compare below the table 2.Table 1 be under the normal temperature contact pressure to 14% graphite magnesium charcoal sample resistivity measurement result.Table 2 is the measured result contrast of the present invention and prior art.Sequence number 1,2,3 is the embodiment of the invention in table 2, and sequence number 4 is the control methods example.From experiment comparing result and actual production, can find out and adopt the repeatable error of method of testing testing result of the present invention to be about below 3%, and prior art measuring method error is approximately greater than 30%.Therefore, the comparability of the inventive method and testing apparatus obviously is better than prior art.
Table 1 contact pressure is to containing the influence of 14% graphite magnesium charcoal sample resistivity measurement value
Contact pressure/MPa | 0.10 | 0.15 | 0.20 | 0.25 | 0.30 | 0.35 | 0.40 | 0.45 |
Resistivity relative value % | 448 | 276 | 132 | 108 | 102 | 101 | 100 | 100 |
Table 2 the present invention and the contrast of prior art measured result
Temperature/* 100 ℃ sequence number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 1 0 | 12 | 14 | 16 | Exert pressure/MPa | |
1 | Intensification Ω m | 47 | 41 | 33 | 24 | 17 | 12 | 2.6 | 1.6 | 1.37 | 1.2 | 1.28 | 1.3 | 1.33 | 0.3 |
Cooling Ω m | 1.6 | 1.57 | 1.53 | 1.5 | 1.47 | 1.43 | 1.43 | 1.4 | 1.35 | 1.29 | 1.31 | 1.33 | 1.34 | ||
2 | Intensification Ω m | 46.2 | 41 | 33.1 | 24.2 | 16.8 | 11.8 | 2.6 | 1.59 | 1.35 | 1.21 | 1.28 | 1.31 | 1.33 | 1.1 |
Cooling Ω m | 1.61 | 1.57 | 1.53 | 1.51 | 1.45 | 1.43 | 1.42 | 1.39 | 1.36 | 1.30 | 1.31 | 1.32 | 1.33 | ||
3 | Intensification Ω m | 46.5 | 40.7 | 33.3 | 24.5 | 16.9 | 11.9 | 2.57 | 1.58 | 1.36 | 1.2 | 1.27 | 1.31 | 1.34 | 1.7 |
Cooling Ω m | 1.59 | 1.56 | 1.54 | 1.52 | 1.46 | 1.43 | 1.42 | 1.38 | 1.35 | 1.31 | 1.31 | 1.33 | 1.34 | ||
4 | Ωm | 22 | 17 | 2.9 | 2.6 | / |
Annotate: (1) above resistivity measurement unit * 10
-4Ω m (2) sample to be tested all is coated with uses the SiC antioxidizing paint
Claims (9)
1; resistivity measurement equipment during a kind of can the continuous coverage fire resistive material varying with temperature; the composition of this equipment is that heating furnace (5) is housed on furnace body support (12); calandria (8) and thermopair (10) should link with temperature controller (7); it is characterized in that sample to be tested (6) the two ends card in heating furnace (5) has holder (9); one end holder (9) should fixedly mount with the furnace wall; and other end holder (9) should with curved push rod (3) front end suit; the middle part of curved push rod (3) should be located by stationary shaft (4); counterweight weights (2) should be equipped with in the rear end of curved push rod (3); the high temperature resistant test lead (13) that is equipped with respectively in the inboard of the outside, the two ends of sample to be tested (6) and holder (9) should link with direct current registering instrument electric bridge (1); in heating furnace (5), be equipped with and the gas piping of protecting source of the gas to communicate (11), all stud with high temperature ceramic material at the curved push rod (3) of Contact Heating stove (5) and the front end of gas piping (11).
2,, it is characterized in that direct current bridge registering instrument 1 can be the direct-flow double bridge registering instrument according to the described equipment of claim 1.
3,, it is characterized in that holder (9) makes for high temperature ceramic material according to the described equipment of claim 1.
4,, it is characterized in that above-mentioned high temperature ceramic material should comprise Al according to the described equipment of claim 1
2O
3, SiC, MgO, SiN, SiO
2, ZrO
2In any one stupalith goods.
5,, it is characterized in that comprising in the described stupalith goods two or more compound ceramic material product according to the described equipment of claim 4.
6; measuring equipment according to claim 1; the method of testing of this resistivity measurement equipment is that sample to be tested (6) surface is evenly scribbled antioxidizing paint; after treating the coating drying; outside holder (9) inboard and sample to be tested (6) two ends, respectively accompany fire-resistant material sample with the identical material of sample to be tested (6); the measurement port of every block of material standard specimen should with holder (9); the measurement port of sample to be tested (6) parallels; and by high temperature resistant test lead order A; a; B; b; C; c; D; the d sequence number is corresponding to be connected; it is characterized in that adopting Using Direct Current Bridge Method in test, sample to be tested (6) exert pressure to be 0.1MPa-2.0MPa; applying method is to reach the size that adjusting is exerted pressure to sample by changing counterweight weights (2) amount; the surface of sample to be tested (6) should scribble antioxidizing paint, should be connected with the blanket gas protection during sample (6) heating.
7,, it is characterized in that blanket gas should be any one in argon gas and the nitrogen according to the described method of claim 6.
8,, it is characterized in that should be Al at sample to be tested (6) the surface antioxidizing paint that is coated with according to the described method of claim 6
2O
3, B
2O
3, SiO
2, any one coating among the SiC.
9, described according to Claim 8 method is characterized in that comprising two or more the composite dope in the described coating.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 99122288 CN1128355C (en) | 1999-11-10 | 1999-11-10 | Method and device for measuring resistivity of carbon-contained refractory material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 99122288 CN1128355C (en) | 1999-11-10 | 1999-11-10 | Method and device for measuring resistivity of carbon-contained refractory material |
Publications (2)
Publication Number | Publication Date |
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CN1250874A CN1250874A (en) | 2000-04-19 |
CN1128355C true CN1128355C (en) | 2003-11-19 |
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CN 99122288 Expired - Fee Related CN1128355C (en) | 1999-11-10 | 1999-11-10 | Method and device for measuring resistivity of carbon-contained refractory material |
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Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101315343B (en) * | 2007-05-29 | 2012-12-12 | 上海比亚迪有限公司 | Apparatus and method for measuring volume resistivity of powder |
CN101949959B (en) * | 2010-09-13 | 2012-09-05 | 中国科学院物理研究所 | High-temperature resistivity measuring stand |
CN107721440B (en) * | 2017-10-26 | 2020-04-17 | 盐城工学院 | Forsterite-spinel-carbon conductive refractory material and preparation method thereof |
CN115420952B (en) * | 2022-11-04 | 2023-03-24 | 之江实验室 | High temperature piezoresistive property measurement platform and method |
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1999
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