CN101949959B - High-temperature resistivity measuring stand - Google Patents
High-temperature resistivity measuring stand Download PDFInfo
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- CN101949959B CN101949959B CN2010102809421A CN201010280942A CN101949959B CN 101949959 B CN101949959 B CN 101949959B CN 2010102809421 A CN2010102809421 A CN 2010102809421A CN 201010280942 A CN201010280942 A CN 201010280942A CN 101949959 B CN101949959 B CN 101949959B
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- boron nitride
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- hexagonal boron
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Abstract
The invention provides a high-temperature resistivity measuring stand, comprising a metal sample table, a hexagonal boron nitride ceramic substrate, a first thermocouple and a second thermocouple. The metal sample table is provided with a first circular hole and a second circular hole; the hexagonal boron nitride ceramic substrate is embedded in the metal sample table; and the measuring end of the first thermocouple is arranged in the first circular hole of the metal sample table, the second thermocouple passes through the second circular hole of the metal sample table, and the measuring end of the second thermocouple is arranged above the hexagonal boron nitride ceramic substrate and is pressed on the surface of a sample. The hexagonal boron nitride ceramic substrate is provided with four metal sheets with holes, which are respectively fixed by screws, and the four metal sheets with holes are respectively connected with four single-core metal wires through pure silver soldering. Before measuring, one ends of the four metal wires are wound and pressed out on the screws while the other ends are adhered on the surface of the sample. The invention has the advantages of high resisted temperature, good thermal conductivity, accurate temperature measurement and easy process and formation.
Description
Technical field
The present invention relates to a kind of high-temperature resistivity measurement mechanism, particularly a kind of device of four leads method measured resistivity is used for the measurement of the electricity transport property of material under the high temperature.
Background technology
The measurement of material electricity transport property is crucial to the character of research material.In semi-conductor industry, along with the rising of sample temperature, huge variation can take place in the resistivity of sample, and this variation has fundamental influence to the precision with safety and instrument etc. of selecting for use of device.In scientific research field, material often is accompanied by the sudden change of electricity transport property in the phase transformation of high-temperature region, and this sudden change is characterized, can be to exploring and understanding material physical property and play directive function.
The high temperature electrical properties is measured the restriction receive test desk unavoidably, and existing test desk roughly can be divided into two types of metal test desk and nonmetal test desks.
1, metal test desk.
Metal has good electrical conductivity, so when being made into electrical measurement platform lift-launch sample, must consider Insulation Problems.At first will insulate between sample and the test desk, will insulate with sample stage in lead of secondly drawing on the sample and the wire interconnecting piece position on the test desk.And the existing test desk insulating medium that arrives generally commonly used, such as teflon etc., its high-temperature resistant temperature is no more than 500 ℃, and temperature that like this can big limitations test desk is used interval.And but if use the material of high-temperature insulations such as quartzy or adamas, its processing technology is complicated, with high costs, has therefore limited the exploitation and the use of this type test desk.In addition, utilize thermocouple measuring temperature under the high temperature usually, and need insulate in the thermocouple assay top with the metal test desk,, therefore have the inaccurate problem of thermometric so in existing equipment, thermopair does not often directly contact with the metal test desk.
2, nonmetal test desk.
Nonmetal test desk commonly used often uses high molecular polymers such as engineering plastics, though can solve Insulation Problems, existing the engineering plastics heatproof is the highest is merely 600 ℃, and its thermal conductivity and resistant to elevated temperatures character can limit the temperature of test desk and use the interval.
In addition, existing various test desks, lead of drawing on the sample and the wire interconnecting piece position on the test desk generally all use the mode of scolding tin welding or spring pressuring plate to connect.But the problem that exists melts soldering tin, spring pressuring plate to follow the string under the high temperature makes the coupling part become flexible landing, causes and measures failure.
So seek suitable material and rational total scheme, go to solve the problem that existing test desk exists, obtain one still can the good support electrical properties in up to 800 ℃ temperature range test desk have crucial meaning.
Summary of the invention
The objective of the invention is to solve that existing test desk heatproof temperature is low, poor thermal conductivity, inaccurate, the processing technology complicated problems of thermometric.
The present invention provides a kind of high-temperature resistivity test desk, comprising: the metal sample platform has first circular hole and second circular hole; The hexagonal boron nitride ceramic substrate is embedded on the metal sample platform; First thermopair and second thermopair, the measuring junction of first thermopair are arranged in first circular hole of metal sample platform, and second thermopair passes second circular hole of metal sample platform, and its measuring junction is positioned at hexagonal boron nitride ceramic substrate top, and is crushed on the sample surfaces.
According to high-temperature resistivity test desk provided by the invention, wherein have 4 perforated metal sheets on the hexagonal boron nitride ceramic substrate, 4 perforated metal sheets are fixed on the hexagonal boron nitride ceramic substrate through 4 screws respectively.4 perforated metal sheets are connected with 4 single core metal lines through the fine silver welding respectively, are with ceramic pipe respectively on 4 single core metal lines.Before the test, an end of 4 one metal wires twined on screw compress, the other end is bonded to sample surfaces, 4 single core copper cash are connected on the suitable electrical measurement instrument (such as Keithley 2400), so that measuring current to be provided.
According to high-temperature resistivity test desk provided by the invention, wherein the metal sample platform is processed by red copper.
Compared with prior art, high-temperature resistivity test desk provided by the present invention has heatproof temperature height, thermal conductivity is good, thermometric is accurate, the advantage of easy machine-shaping, can satisfy the requirement of resistivity measurement under the high temperature (≤800 ℃).
Description of drawings
Followingly the embodiment of the invention is described further with reference to accompanying drawing, wherein:
Fig. 1 is the vertical view of high-temperature resistivity test desk of the present invention.
Fig. 2 is that high-temperature resistivity test desk among Fig. 1 is along the diagrammatic cross-section of A-A line.
Fig. 3 is the schematic rear view of the high-temperature resistivity test desk among Fig. 1.
The content of each digital representative is among the figure: 401, substrate; 402, sample stage; 4021, sample stage first; 4022, sample stage second portion; 101, single core copper cash; 102, ceramic pipe; 103, copper sheet with holes; 104, brass screws; 105, copper wire; 201, circular hole; 202, thermopair; 203, circular hole; 204, thermopair; 301, screw; 302, copper sheet; 303, hexagonal boron nitride pottery compressing tablet; 304, screw.
Embodiment
Embodiment 1
Like Fig. 1,2, shown in 3, the high-temperature resistivity test desk of present embodiment comprises the red copper sample stage 402 with groove, is inlaid with hexagonal boron nitride ceramic substrate 401 in the groove.Red copper sample stage and hexagonal boron nitride ceramic substrate are fixing with the screw that is with copper sheet 302 301.Wherein the red copper sample stage has the first 4021 that is parallel to the hexagonal boron nitride ceramic substrate and perpendicular to the second portion 4022 of hexagonal boron nitride ceramic substrate.Have circular hole 203 in the first 4021 of above-mentioned red copper sample stage, the bearing of trend of circular hole 203 is basically perpendicular to the hexagonal boron nitride ceramic substrate.The second portion 4022 of above-mentioned red copper sample stage has circular hole 201, and the bearing of trend of circular hole 201 is basically parallel to the hexagonal boron nitride ceramic substrate.Be filled with boron nitride powder in the circular hole 201, the high-temperature cement shutoff is used at two ends, uses so that the measuring junction of thermopair 202 is fixed in the circular hole 201, to read the temperature of sample stage.Circular hole 203 is used to pass thermopair 204, and the measuring junction of thermopair 204 is positioned at hexagonal boron nitride ceramic substrate top, and gently is pressed on the sample surfaces by hexagonal boron nitride pottery compressing tablet 303, to read the actual temperature of sample surfaces.Hexagonal boron nitride pottery compressing tablet is fixed on hexagonal boron nitride ceramic substrate surface through screw 304.The non-measuring junction of thermopair 202 and thermopair 204 is fixed on the red copper sample stage by copper sheet 302 and screw 301.
Having 103,4 copper sheets with holes of 4 copper sheets with holes on the hexagonal boron nitride ceramic substrate is fixed on the hexagonal boron nitride ceramic substrate through 4 brass screwss 104 respectively.4 copper sheets with holes are connected with 4 single core copper cash 101 respectively through the fine silver welding.Be with ceramic pipe 102 respectively on 4 single core copper cash.4 single core copper cash are connected on the suitable electrical measurement instrument (such as Keithley 2400), so that measuring current to be provided.
Before the test, respectively an end of 4 copper wires 105 is bonded in sample surfaces with high temperature silver slurry, the other end of 4 copper wires twines on 4 brass screwss respectively and compresses.During measurement, but sample stage integral body put into the high temperature furnace (≤800 ℃) of alternating temperature.104,4 copper sheets 103 with holes of 105,4 brass screwss of 4 copper wires and 4 single core copper cash 101 are formed conductive path; The electric current of electrical measurement instrument (such as Keithley 2400) is incorporated on the sample; Thermopair 202 and the temperature of thermopair 204 difference measuring samples platforms and the actual temperature of sample surfaces, thus can accurately obtain the resistance of sample under different temperatures with four leads method.
According to high-temperature resistivity test desk provided by the invention, its substrate is made up of the hexagonal boron nitride pottery.Hexagonal boron nitride has good insulation performance property; And at high temperature have the thermal conductivity that is similar to metal, be limited to 1000 ℃ on the working temperature of hexagonal boron nitride, can satisfy the requirement of resistivity measurement under the high temperature (≤800 ℃); The hexagonal boron nitride Mohs value is 2 in addition, therefore machine-shaping easily.The hexagonal boron nitride ceramic substrate is embedded on the red copper sample stage, thereby makes the structure of test desk firmer.In addition, the thermal conductivity that red copper and hexagonal boron nitride are good has further guaranteed thermometric accuracy in hot environment again.Therefore, the test desk of present embodiment had both had the good insulating of nonmetal test desk, the advantage that sample can directly contact, and had metallic test platform temperature conductivity height, resistant to elevated temperatures advantage again.
According to the test desk of present embodiment, two thermopairs are monitored sample surfaces temperature and sample stage temperature respectively, thereby have reduced the temperature error between sample stage and the sample, have guaranteed the accuracy of temperature in the high-temperature resistivity measurement.
According to the test desk of present embodiment, the mechanical bond of copper wire and brass screws has replaced the scolding tin welding, has made things convenient for getting of sample to change, and has good electrical conductivity, has avoided the problem that melts soldering tin, spring pressuring plate follow the string under the high temperature simultaneously.The fine silver welding has guaranteed the heat-resisting quantity and the good electrical conductivity that connect.4 ceramic pipes 102 are placed in respectively on 4 single core copper cash, have guaranteed the heat-resisting quantity and the insulativity of single core copper cash.
According to the test desk of present embodiment, wherein sample stage also can adopt other shape, like H shape, disc etc., as long as this sample stage can be embedded in the hexagonal boron nitride ceramic substrate wherein.The shape of sample stage can change according to the environment of high temperature furnace, to reach the purpose that makes things convenient for sample stage to place.The layout of thermopair is the change of platform shape and changing per sample also, as long as the measuring junction of a thermopair is arranged in the circular hole of sample stage, the measuring junction of another thermopair passes the circular hole of sample stage.
Sample stage is preferably the red copper that temperature conductivity is good and cost is low, but can be processed by other good metals of temperature conductivity such as iron, stainless steel, gold, silver, platinum.
Embodiment 2
The difference of the test desk that provides among test desk that present embodiment provides and the embodiment 1 is that the hexagonal boron nitride ceramic substrate is not to be embedded on the metal sample platform, but uses separately.A thermopair passes the hexagonal boron nitride ceramic substrate, and its measuring junction is crushed on sample surfaces, is used for the temperature of measuring samples.The measuring junction of another thermopair is arranged in the through hole of hexagonal boron nitride ceramic substrate, is used to measure substrate temperature.
Because hexagonal boron nitride has good insulation performance property, and at high temperature have the thermal conductivity that is similar to metal, so thermopair can directly contact (for example the measuring junction of thermopair be arranged in substrate through hole) with substrate, thereby avoid the inaccurate problem of temperature survey.
It should be noted last that above embodiment is only unrestricted in order to technical scheme of the present invention to be described.Although the present invention is specified with reference to embodiment; Those of ordinary skill in the art is to be understood that; Technical scheme of the present invention is made amendment or is equal to replacement, do not break away from the spirit and the scope of technical scheme of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (9)
1. high-temperature resistivity test desk is characterized in that this test desk comprises:
The metal sample platform has first circular hole and second circular hole;
The hexagonal boron nitride ceramic substrate is embedded on the metal sample platform;
First thermopair and second thermopair; The measuring junction of first thermopair is arranged in first circular hole of metal sample platform; Second thermopair passes second circular hole of metal sample platform, and the measuring junction of second thermopair is positioned at hexagonal boron nitride ceramic substrate top, and is crushed on the sample surfaces.
2. high-temperature resistivity test desk according to claim 1 is characterized in that, metal sample platform and hexagonal boron nitride ceramic substrate are fixed with the screw that is with sheet metal.
3. high-temperature resistivity test desk according to claim 1 is characterized in that, the non-measuring junction of first thermopair and second thermopair is fixed by sheet metal.
4. high-temperature resistivity test desk according to claim 1 is characterized in that, is filled with boron nitride powder in above-mentioned first circular hole, and the high-temperature cement shutoff is used at the first circular hole two ends.
5. high-temperature resistivity test desk according to claim 1 is characterized in that, the measuring junction of above-mentioned second thermopair is pressed on the sample surfaces by hexagonal boron nitride pottery compressing tablet, and hexagonal boron nitride pottery compressing tablet is fixed on hexagonal boron nitride ceramic substrate surface.
6. according to any described high-temperature resistivity test desk in the claim 1 to 5, it is characterized in that the metal sample platform is processed by red copper.
7. according to any described high-temperature resistivity test desk in the claim 1 to 5; It is characterized in that; 4 perforated metal sheets are fixed on the hexagonal boron nitride ceramic substrate through 4 screws respectively, and an end of 4 one metal wires twines on 4 screws respectively and compresses, the other end is bonded to sample surfaces.
8. high-temperature resistivity test desk according to claim 7 is characterized in that, 4 single core metal lines are connected with 4 perforated metal sheets through the fine silver welding respectively, are with ceramic pipe respectively on 4 single core metal lines.
9. high-temperature resistivity test desk according to claim 7 is characterized in that, perforated metal sheet, screw, material wiry are copper.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102809421A CN101949959B (en) | 2010-09-13 | 2010-09-13 | High-temperature resistivity measuring stand |
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| CN2010102809421A CN101949959B (en) | 2010-09-13 | 2010-09-13 | High-temperature resistivity measuring stand |
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| CN101949959A CN101949959A (en) | 2011-01-19 |
| CN101949959B true CN101949959B (en) | 2012-09-05 |
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| CN2010102809421A Active CN101949959B (en) | 2010-09-13 | 2010-09-13 | High-temperature resistivity measuring stand |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104062318B (en) * | 2013-03-19 | 2016-08-10 | 国家纳米科学中心 | The specimen holder of thermoelectricity capability and measuring method for measuring samples |
| CN104267004B (en) * | 2014-10-24 | 2018-04-24 | 合肥市再德高分子材料有限公司 | A kind of sample stimulation system of photoelectric direct-reading spectrograph |
| CN108362743A (en) * | 2018-04-03 | 2018-08-03 | 中国工程物理研究院激光聚变研究中心 | Low-temperature resistivity measuring device and its installation method |
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|---|---|---|---|---|
| US5656940A (en) * | 1994-01-28 | 1997-08-12 | Commissariat A L'energie Atomique | Apparatus for measuring the surface resistance and electrical resistivity of a homogeneous resistive material at high temperature |
| CN1250874A (en) * | 1999-11-10 | 2000-04-19 | 冶金工业部钢铁研究总院 | Method and device for measuring resistivity of carbon-contained refractory material |
| CN1851485A (en) * | 2006-05-26 | 2006-10-25 | 中国科学院上海硅酸盐研究所 | High temperature resistivity measuring device and its measuring method |
| CN101038265A (en) * | 2007-04-23 | 2007-09-19 | 华中科技大学 | Device for measuring Seebeck coefficient and resistivity of semi-conductor film material |
| CN101782544A (en) * | 2010-03-02 | 2010-07-21 | 济南大学 | Device for testing metal melt electrical resistivity and testing method therefor |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348958C (en) * | 2005-07-20 | 2007-11-14 | 哈尔滨工业大学 | Real time measuring method of heat proof material ablation temperature field and its special measuring device |
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- 2010-09-13 CN CN2010102809421A patent/CN101949959B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5656940A (en) * | 1994-01-28 | 1997-08-12 | Commissariat A L'energie Atomique | Apparatus for measuring the surface resistance and electrical resistivity of a homogeneous resistive material at high temperature |
| CN1250874A (en) * | 1999-11-10 | 2000-04-19 | 冶金工业部钢铁研究总院 | Method and device for measuring resistivity of carbon-contained refractory material |
| CN1851485A (en) * | 2006-05-26 | 2006-10-25 | 中国科学院上海硅酸盐研究所 | High temperature resistivity measuring device and its measuring method |
| CN101038265A (en) * | 2007-04-23 | 2007-09-19 | 华中科技大学 | Device for measuring Seebeck coefficient and resistivity of semi-conductor film material |
| CN101782544A (en) * | 2010-03-02 | 2010-07-21 | 济南大学 | Device for testing metal melt electrical resistivity and testing method therefor |
Non-Patent Citations (1)
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| 字正华等.自制低温电阻测量系统的分析研究.《思茅师范高等专科学校学报》.1999,第15卷(第4期), * |
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