CN101949959B - High-temperature resistivity measuring stand - Google Patents
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Abstract
本发明提供一种高温电阻率测量台,包括:金属样品台,具有第一圆孔和第二圆孔;六方氮化硼陶瓷衬底,镶嵌在金属样品台上;第一热电偶和第二热电偶,第一热电偶的测量端位于金属样品台的第一圆孔中,第二热电偶穿过金属样品台的第二圆孔,其测量端位于六方氮化硼陶瓷衬底上方,并被压在样品表面上。其中六方氮化硼陶瓷衬底上具有4个带孔金属片,其分别通过螺丝固定,4个带孔金属片分别通过纯银焊接与4根单芯金属线相连接。测试前,将4根金属丝的一端在螺丝上缠绕压紧、另一端被粘合在样品表面。本发明所提供的高温电阻率测量台具有耐温温度高、导热性好、测温准确、容易加工成型的优点。
The invention provides a high-temperature resistivity measuring platform, comprising: a metal sample platform having a first circular hole and a second circular hole; a hexagonal boron nitride ceramic substrate embedded in the metal sample platform; a first thermocouple and a second Thermocouples, the measuring end of the first thermocouple is located in the first circular hole of the metal sample stage, the second thermocouple passes through the second circular hole of the metal sample stage, and its measuring end is located above the hexagonal boron nitride ceramic substrate, and pressed against the sample surface. Wherein the hexagonal boron nitride ceramic substrate has 4 metal sheets with holes, which are respectively fixed by screws, and the 4 metal sheets with holes are respectively connected with 4 single-core metal wires through pure silver welding. Before the test, one end of the four metal wires was wrapped and compressed on the screw, and the other end was glued to the surface of the sample. The high-temperature resistivity measuring platform provided by the invention has the advantages of high temperature resistance, good thermal conductivity, accurate temperature measurement, and easy processing and molding.
Description
技术领域 technical field
本发明涉及一种高温电阻率测量装置,特别涉及一种四引线法测量电阻率的装置,用于高温下材料的电学输运性质的测量。The invention relates to a high-temperature resistivity measuring device, in particular to a four-lead method measuring resistivity device, which is used for measuring the electrical transport properties of materials at high temperatures.
背景技术 Background technique
材料电学输运性质的测量,对研究材料的性质是十分重要的。在半导体工业中,随着样品温度的升高,样品的电阻率会发生巨大的变化,这种变化对器件的选用和安全以及仪器的精密度等有着至关重要的影响。在科研领域中,材料在高温区的相变往往伴随着电学输运性质的突变,对这种突变进行表征,会对探索和理解材料物理性能起到指导作用。The measurement of the electrical transport properties of materials is very important for the study of the properties of materials. In the semiconductor industry, as the temperature of the sample increases, the resistivity of the sample will change dramatically. This change has a crucial impact on the selection and safety of the device and the precision of the instrument. In the field of scientific research, the phase transition of materials in high-temperature regions is often accompanied by sudden changes in electrical transport properties. Characterizing this sudden change will play a guiding role in exploring and understanding the physical properties of materials.
高温电学性质测量难免受到测量台的限制,现有的测量台大致可以分为金属测量台和非金属测量台两类。The measurement of high-temperature electrical properties is inevitably limited by the measuring bench. The existing measuring bench can be roughly divided into two types: metal measuring bench and non-metallic measuring bench.
1、金属测量台。1. Metal measuring table.
金属具有良好的导电性,所以当制作成电学测量台搭载样品时,必须要考虑绝缘问题。首先样品和测量台之间要绝缘,其次样品上引出的导线和测量台上的导线连接部位要与样品台绝缘。而现有测量台一般常用到的绝缘介质,比如聚四氟乙烯等,其最高耐温温度不超过500℃,这样会大大限制测量台的温度使用区间。而若使用石英或者金刚石等可耐高温绝缘的材料,其加工工艺复杂、成本高昂,因此限制了这类测量台的开发和使用。此外,高温下通常利用热电偶测量温度,而热电偶测试顶端需要与金属测量台绝缘,故在现有设备中,热电偶往往与金属测量台不直接接触,因此存在测温不准确的问题。Metal has good electrical conductivity, so when it is made into an electrical measurement table to carry samples, insulation must be considered. Firstly, the sample and the measuring platform should be insulated, and secondly, the connecting part of the wire drawn from the sample and the wire on the measuring platform should be insulated from the sample platform. However, the insulating medium commonly used in the existing measurement platforms, such as polytetrafluoroethylene, etc., has a maximum temperature resistance of no more than 500°C, which will greatly limit the temperature range of the measurement platform. However, if a material capable of high temperature resistance and insulation such as quartz or diamond is used, the processing technology is complicated and the cost is high, which limits the development and use of this type of measuring platform. In addition, thermocouples are usually used to measure temperature at high temperatures, and the top of the thermocouple test needs to be insulated from the metal measuring platform. Therefore, in existing equipment, the thermocouple is often not in direct contact with the metal measuring platform, so there is a problem of inaccurate temperature measurement.
2、非金属测量台。2. Non-metal measuring platform.
常用的非金属测量台,往往使用到工程塑料等高分子聚合物,虽然可以解决绝缘问题,但是现有工程塑料耐温最高仅为600℃,其导热性和耐高温的性质会限制测量台的温度使用区间。Commonly used non-metallic measuring tables often use high molecular polymers such as engineering plastics. Although they can solve the insulation problem, the highest temperature resistance of existing engineering plastics is only 600°C, and their thermal conductivity and high temperature resistance will limit the performance of the measuring table. temperature range.
另外,现有的各种测量台,被测样品上引出的导线与测量台上的导线连接部位,一般均使用焊锡焊接或者弹簧压片的方式连接。但是高温下存在焊锡熔化、弹簧压片失去弹性的问题,使得连接部分松动滑落,造成测量失败。In addition, in various existing measurement platforms, the wires drawn from the sample to be tested are generally connected to the wires on the measurement platform by means of soldering or spring pressing. However, there are problems such as solder melting and spring pressing piece losing elasticity at high temperature, which makes the connection part loose and slip, resulting in measurement failure.
所以寻找合适的材料和合理的合计方案,去解决现有测量台存在的问题,得到一个在高达800℃的温度范围内依然能够良好支持电学性质的测量台具有十分重要的意义。Therefore, it is of great significance to find a suitable material and a reasonable total solution to solve the problems existing in the existing measurement platform, and to obtain a measurement platform that can still support electrical properties well in a temperature range up to 800 °C.
发明内容 Contents of the invention
本发明的目的在于解决现有测量台耐温温度低、导热性差、测温不准确、加工工艺复杂的问题。The purpose of the invention is to solve the problems of low temperature resistance, poor thermal conductivity, inaccurate temperature measurement and complicated processing technology of the existing measuring platform.
本发明提供一种高温电阻率测量台,包括:金属样品台,具有第一圆孔和第二圆孔;六方氮化硼陶瓷衬底,镶嵌在金属样品台上;第一热电偶和第二热电偶,第一热电偶的测量端位于金属样品台的第一圆孔中,第二热电偶穿过金属样品台的第二圆孔,其测量端位于六方氮化硼陶瓷衬底上方,并被压在样品表面上。The invention provides a high-temperature resistivity measuring platform, comprising: a metal sample platform having a first circular hole and a second circular hole; a hexagonal boron nitride ceramic substrate embedded in the metal sample platform; a first thermocouple and a second Thermocouples, the measuring end of the first thermocouple is located in the first circular hole of the metal sample stage, the second thermocouple passes through the second circular hole of the metal sample stage, and its measuring end is located above the hexagonal boron nitride ceramic substrate, and pressed against the sample surface.
根据本发明提供的高温电阻率测量台,其中六方氮化硼陶瓷衬底上具有4个带孔金属片,4个带孔金属片分别通过4个螺丝固定在六方氮化硼陶瓷衬底上。4个带孔金属片分别通过纯银焊接与4根单芯金属线相连接,4根单芯金属线上分别套有陶瓷管。测试前,将4根金属丝的一端在螺丝上缠绕压紧、另一端被粘合在样品表面,4根单芯铜线连接在合适的电学测量仪表(比如吉时利2400)上,以提供测试电流。According to the high-temperature resistivity measuring platform provided by the present invention, there are four metal sheets with holes on the hexagonal boron nitride ceramic substrate, and the four metal sheets with holes are respectively fixed on the hexagonal boron nitride ceramic substrate by four screws. The four metal sheets with holes are respectively connected to four single-core metal wires through pure silver welding, and the four single-core metal wires are respectively covered with ceramic tubes. Before the test, one end of the four metal wires is wrapped and pressed tightly on the screw, the other end is glued to the surface of the sample, and the four single-core copper wires are connected to a suitable electrical measuring instrument (such as Keithley 2400) to provide Test current.
根据本发明提供的高温电阻率测量台,其中金属样品台由紫铜制成。According to the high-temperature resistivity measuring platform provided by the present invention, the metal sample platform is made of red copper.
与现有技术相比,本发明所提供的高温电阻率测量台具有耐温温度高、导热性好、测温准确、容易加工成型的优点,可以满足高温(≤800℃)下电阻率测量的要求。Compared with the prior art, the high-temperature resistivity measuring platform provided by the present invention has the advantages of high temperature resistance, good thermal conductivity, accurate temperature measurement, and easy processing and molding, and can meet the requirements of resistivity measurement at high temperatures (≤800°C). Require.
附图说明 Description of drawings
以下参照附图对本发明实施例作进一步说明,其中:Embodiments of the present invention will be further described below with reference to the accompanying drawings, wherein:
图1是本发明高温电阻率测量台的俯视图。Fig. 1 is a top view of the high temperature resistivity measuring platform of the present invention.
图2是图1中的高温电阻率测量台沿A-A线的剖面示意图。Fig. 2 is a schematic cross-sectional view of the high-temperature resistivity measuring platform in Fig. 1 along line A-A.
图3是图1中的高温电阻率测量台的背面示意图。Fig. 3 is a schematic diagram of the back of the high temperature resistivity measuring platform in Fig. 1 .
图中各数字所代表的内容为:401、衬底;402、样品台;4021、样品台第一部分;4022、样品台第二部分;101、单芯铜线;102、陶瓷管;103、带孔铜片;104、铜螺丝;105、铜丝;201、圆孔;202、热电偶;203、圆孔;204、热电偶;301、螺丝;302、铜片;303、六方氮化硼陶瓷压片;304、螺丝。The contents represented by each number in the figure are: 401, substrate; 402, sample stage; 4021, the first part of sample stage; 4022, the second part of sample stage; 101, single-core copper wire; 102, ceramic tube; 103, belt Hole copper sheet; 104, copper screw; 105, copper wire; 201, round hole; 202, thermocouple; 203, round hole; 204, thermocouple; 301, screw; 302, copper sheet; 303, hexagonal boron nitride ceramics Pressing tablet; 304, screw.
具体实施方式 Detailed ways
实施例1Example 1
如图1、2、3所示,本实施例的高温电阻率测量台包括具有凹槽的紫铜样品台402,凹槽中镶嵌有六方氮化硼陶瓷衬底401。紫铜样品台与六方氮化硼陶瓷衬底用套有铜片302的螺丝301固定。其中紫铜样品台具有平行于六方氮化硼陶瓷衬底的第一部分4021以及垂直于六方氮化硼陶瓷衬底的第二部分4022。上述紫铜样品台的第一部分4021上具有圆孔203,圆孔203的延伸方向基本垂直于六方氮化硼陶瓷衬底。上述紫铜样品台的第二部分4022具有圆孔201,圆孔201的延伸方向基本平行于六方氮化硼陶瓷衬底。圆孔201中填充有氮化硼粉末,两端用高温水泥封堵,用以使热电偶202的测量端固定于圆孔201中,以读出样品台的温度。圆孔203用于穿过热电偶204,热电偶204的测量端位于六方氮化硼陶瓷衬底上方,并被六方氮化硼陶瓷压片303轻压在样品表面上,以读出样品表面的实际温度。六方氮化硼陶瓷压片通过螺丝304固定在六方氮化硼陶瓷衬底表面。热电偶202和热电偶204的非测量端被铜片302和螺丝301固定于紫铜样品台上。As shown in FIGS. 1 , 2 and 3 , the high-temperature resistivity measuring platform of this embodiment includes a red
六方氮化硼陶瓷衬底上具有4个带孔铜片103,4个带孔铜片分别通过4个铜螺丝104固定于六方氮化硼陶瓷衬底上。4个带孔铜片通过纯银焊接分别与4根单芯铜线101相连接。4根单芯铜线上分别套有陶瓷管102。4根单芯铜线连接在合适的电学测量仪表(比如吉时利2400)上,以提供测试电流。There are four
测试前,用高温银浆分别将4根铜丝105的一端粘合在样品表面,4根铜丝的另一端分别在4个铜螺丝上缠绕压紧。测量时,将样品台整体放入可变温的高温炉中(≤800℃)。4根铜丝105、4个铜螺丝104、4个带孔铜片103和4根单芯铜线101组成导电通路,将电学测量仪表(比如吉时利2400)的电流引入到样品上,热电偶202和热电偶204分别测量样品台的温度和样品表面的实际温度,从而可以用四引线法精确得到样品在不同温度下的电阻。Before the test, one end of four
根据本发明提供的高温电阻率测量台,其衬底由六方氮化硼陶瓷构成。六方氮化硼具有良好的绝缘性,且在高温下具有近似于金属的导热性,六方氮化硼的工作温度上限为1000℃,可以满足高温(≤800℃)下电阻率测量的要求,另外六方氮化硼莫氏硬度为2,因此容易加工成型。六方氮化硼陶瓷衬底镶嵌在紫铜样品台上,从而使测量台的结构更坚固。此外,紫铜和六方氮化硼优良的导热性,又进一步保证了在高温环境中温度测量的准确性。因此,本实施例的测量台既具有非金属测量台的绝缘性好、样品可直接接触的优点,又具有金属测试台导热率高、耐高温的优点。According to the high-temperature resistivity measuring platform provided by the present invention, its substrate is made of hexagonal boron nitride ceramics. Hexagonal boron nitride has good insulation, and has a thermal conductivity similar to that of metal at high temperatures. The upper limit of the working temperature of hexagonal boron nitride is 1000°C, which can meet the requirements of resistivity measurement at high temperatures (≤800°C). In addition, Hexagonal boron nitride has a Mohs hardness of 2, so it is easy to process and shape. The hexagonal boron nitride ceramic substrate is inlaid on the copper sample stage, so that the structure of the measuring stage is stronger. In addition, the excellent thermal conductivity of copper and hexagonal boron nitride further ensures the accuracy of temperature measurement in high temperature environments. Therefore, the measuring platform of this embodiment not only has the advantages of good insulation of the non-metallic measuring platform and direct contact with samples, but also has the advantages of high thermal conductivity and high temperature resistance of the metal testing platform.
根据本实施例的测量台,两只热电偶分别监控样品表面温度和样品台温度,从而减小了样品台和样品之间的温度误差,保证了高温电阻率测量中温度的准确性。According to the measuring platform of this embodiment, two thermocouples monitor the surface temperature of the sample and the temperature of the sample stage respectively, thereby reducing the temperature error between the sample stage and the sample, and ensuring the accuracy of temperature in high temperature resistivity measurement.
根据本实施例的测量台,铜丝与铜螺丝的机械结合代替了焊锡焊接,方便了样品的取换,具有良好的导电性,同时避免了高温下焊锡熔化、弹簧压片失去弹性的问题。纯银焊接保证了连接的耐高温性和良好的导电性。4根陶瓷管102分别套于4根单芯铜线上,保证了单芯铜线的耐高温性和绝缘性。According to the measuring platform of this embodiment, the mechanical combination of copper wire and copper screw replaces soldering, which facilitates the replacement of samples, has good electrical conductivity, and avoids the problems of solder melting at high temperature and spring pressing piece losing elasticity. Pure silver soldering ensures high temperature resistance and good electrical conductivity of the connection. The four
根据本实施例的测量台,其中样品台也可以采用其他的形状,如H形、圆盘形等,只要该样品台能够将六方氮化硼陶瓷衬底镶嵌于其中即可。样品台的形状可以依据高温炉的环境而改变,以达到方便样品台放置的目的。热电偶的布置也可以根据样品台形状的改变而改变,只要一个热电偶的测量端位于样品台的圆孔中、另一热电偶的测量端穿过样品台的圆孔即可。According to the measuring stage of this embodiment, the sample stage can also adopt other shapes, such as H shape, disk shape, etc., as long as the sample stage can be embedded with a hexagonal boron nitride ceramic substrate. The shape of the sample stage can be changed according to the environment of the high-temperature furnace to facilitate the placement of the sample stage. The arrangement of thermocouples can also be changed according to the shape of the sample stage, as long as the measuring end of one thermocouple is located in the round hole of the sample stage, and the measuring end of the other thermocouple passes through the round hole of the sample stage.
样品台优选为导热率好且造价低的紫铜,但可由铁、不锈钢、金、银、铂等导热率好的其它金属制成。The sample stage is preferably copper with good thermal conductivity and low cost, but it can be made of other metals with good thermal conductivity such as iron, stainless steel, gold, silver, platinum, etc.
铜片302、带孔铜片103、铜螺丝104、铜丝105和单芯铜线101也可由铁、不锈钢、金、银、铂等导热率好的其它金属制成。The
实施例2Example 2
本实施例提供的测量台与实施例1中提供的测量台的区别在于,六方氮化硼陶瓷衬底不是镶嵌在金属样品台上,而是单独使用。一个热电偶穿过六方氮化硼陶瓷衬底,其测量端被压在样品表面,用于测量样品的温度。另一个热电偶的测量端位于六方氮化硼陶瓷衬底的通孔中,用于测量衬底的温度。The difference between the measuring platform provided in this embodiment and the measuring platform provided in Example 1 is that the hexagonal boron nitride ceramic substrate is not embedded on the metal sample platform, but used alone. A thermocouple passes through the hexagonal boron nitride ceramic substrate, and its measuring end is pressed against the sample surface to measure the temperature of the sample. The measuring end of another thermocouple is located in the through-hole of the hexagonal boron nitride ceramic substrate for measuring the temperature of the substrate.
因为六方氮化硼具有良好的绝缘性,且在高温下具有近似于金属的导热性,因此热电偶可与衬底直接接触(例如热电偶的测量端位于衬底的通孔中),从而避免温度测量不准确的问题。Because hexagonal boron nitride has good insulation and has thermal conductivity close to that of metal at high temperature, the thermocouple can be in direct contact with the substrate (for example, the measuring end of the thermocouple is located in the through hole of the substrate), thereby avoiding Problem with inaccurate temperature measurement.
最后所应说明的是,以上实施例仅用以说明本发明的技术方案而非限制。尽管参照实施例对本发明进行了详细说明,本领域的普通技术人员应当理解,对本发明的技术方案进行修改或者等同替换,都不脱离本发明技术方案的精神和范围,其均应涵盖在本发明的权利要求范围当中。Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than limit them. Although the present invention has been described in detail with reference to the embodiments, those skilled in the art should understand that modifications or equivalent replacements to the technical solutions of the present invention do not depart from the spirit and scope of the technical solutions of the present invention, and all of them should be included in the scope of the present invention. within the scope of the claims.
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