JP4185028B2 - Differential scanning calorimeter with cooling mechanism - Google Patents
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本発明は、冷却機構を有した、示差走査差熱量計に関する。 The present invention relates to a differential scanning differential calorimeter having a cooling mechanism.
示差走査熱量計などの熱分析装置は、温度制御されたヒートシンク、前記ヒートシンク内にある試料、基準物質ホルダー、ヒートシンクを加熱するためのヒーター、ヒートシンクを冷却するための冷却装置を備えている。この冷却装置としては、従来液化窒素などを気化させた冷却ガスにより冷却を行なうガス冷却装置（例えば特許文献１）がある。又、コンプレッサーを内蔵しそれにより冷却された冷媒により冷却される金属製の冷却部材を介して、冷却を行なう電気冷却装置がある。そして従来においては、上記ガス冷却装置か電気冷却装置のいずれかの冷却部材を必要に応じて取り替えて熱分析装置の加熱炉に装着して冷却を行っていた。
従来の示差走査熱量計においては、１種類の冷却装置しか取り付けることができないため、測定温度に応じて２種類の冷却装置の付け替えをするわずらわしさがあった。 In the conventional differential scanning calorimeter, since only one type of cooling device can be attached, there is a hassle of replacing two types of cooling devices according to the measured temperature.
また、液化窒素を用いた冷却装置と電気冷却装置の２つの冷却装置が同時に装着できる機構にすると、それぞれ独立した冷却装置を冷却機構へ接続する機構を設けているため、冷却装置を取り替えるわずらわしさを取り除くことができるが、以下の問題点もある。 In addition, if a mechanism that can mount two cooling devices, that is, a cooling device using liquefied nitrogen and an electric cooling device, is provided, a mechanism that connects each independent cooling device to the cooling mechanism is provided. Can be removed, but there are also the following problems.
上記２つの冷却装置をヒートシンクに固定されている冷却機構に接続した熱分析装置において、高温測定する場合は、ヒートシンクの昇温能力を高めるため、２つの冷却装置の動作を止めるのが望ましい。しかしながら、電気冷却装置を動作させず、液化窒素を用いた冷却装置の液化窒素の供給を止めた時、ヒートシンクに固定された冷却機構はヒートシンクの熱により加熱され、冷却機構に接続されている電気冷却ヘッドの耐熱限界に達し、電気冷却装置を損傷させてしまう。一方、電気冷却装置を動作させた場合は、冷却ヘッドの耐熱限界は問題ないが、ヒートシンクから冷却機構へ熱流が生じ、高温測定ができなくなるという問題点もある。従って、液化窒素の供給を止めるときは、電気冷却ヘッドを取り外しておかねばならないという制約が生じる。 In a thermal analysis apparatus in which the above two cooling devices are connected to a cooling mechanism fixed to a heat sink, it is desirable to stop the operations of the two cooling devices in order to increase the temperature raising capability of the heat sink when measuring at a high temperature. However, when the supply of liquefied nitrogen to the cooling device using liquefied nitrogen is stopped without operating the electric cooling device, the cooling mechanism fixed to the heat sink is heated by the heat of the heat sink and is connected to the cooling mechanism. The heat limit of the cooling head is reached and the electric cooling device is damaged. On the other hand, when the electric cooling device is operated, there is no problem with the heat resistance limit of the cooling head, but there is also a problem that heat flow is generated from the heat sink to the cooling mechanism and high temperature measurement cannot be performed. Therefore, when the supply of liquefied nitrogen is stopped, the electric cooling head must be removed.
そこで、本願発明は上記問題点を解決し、液化窒素を用いた冷却装置の冷却ヘッドと電気冷却装置の冷却ヘッドの接続機構を共有化し、冷却装置の切替えを簡便化し、温度範囲を容易に切り替えられる示差走査熱量計を提供することを課題とする。 Therefore, the present invention solves the above problems, shares the connection mechanism between the cooling head of the cooling device using liquefied nitrogen and the cooling head of the electric cooling device, simplifies switching of the cooling device, and easily switches the temperature range. It is an object of the present invention to provide a differential scanning calorimeter.
上記課題を解決するために、本願発明においては、測定試料と基準物質を収納するヒートシンクと、前記ヒートシンクを加熱するヒーターと、前記ヒートシンクの底板に固定されている示差熱流検出器を有する示差走査熱量計において、前記ヒートシンクの下端に固定された冷却機構を有し、前記冷却機構には、冷却ガス導入用の冷却ヘッドあるいは電気冷却ヘッドを装着するための挿入穴と、前記挿入穴と導通する冷却ガスのガス流路が設けられている。前記ガス流路は、液化窒素を気化させた冷却ガスと冷却機構間の熱交換を行い、前記ガス流路は、冷却ガスを導入、排気するための導入口、排気口を有し、その側壁に複数の突起物を有する。冷却ガス導入口は前記挿入穴の側壁に設けられている。冷却ガス導入用の冷却ヘッドにはガス送出穴が設けられており、挿入穴に差し込んだ時、このガス送出穴が前記挿入穴に設けられたガス導入口の位置にくるように調整されている。前記冷却ガス導入口から導入され、ガス流路で冷却機構を冷却し、熱交換後の冷却ガスは、前記冷却ガス排気口から排気される。前記挿入穴は、電気冷却装置の円柱型の冷却ヘッドの接続機構にもなる。すなわち、前記挿入穴と同形状の前記電気冷却ヘッドを固定することができる。 In order to solve the above problems, in the present invention, a differential scanning calorie having a heat sink for storing a measurement sample and a reference material, a heater for heating the heat sink, and a differential heat flow detector fixed to a bottom plate of the heat sink. A cooling mechanism fixed to the lower end of the heat sink, and the cooling mechanism has an insertion hole for mounting a cooling head for introducing a cooling gas or an electric cooling head, and cooling conducted to the insertion hole. A gas flow path for gas is provided. The gas flow path performs heat exchange between a cooling gas obtained by vaporizing liquefied nitrogen and a cooling mechanism, and the gas flow path has an inlet and an exhaust outlet for introducing and exhausting the cooling gas, and the side wall thereof. Have a plurality of protrusions. The cooling gas inlet is provided on the side wall of the insertion hole. The cooling head for introducing the cooling gas is provided with a gas delivery hole, and when inserted into the insertion hole, the gas delivery hole is adjusted so as to come to the position of the gas introduction port provided in the insertion hole. . The cooling gas is introduced from the cooling gas introduction port, the cooling mechanism is cooled by the gas flow path, and the cooling gas after heat exchange is exhausted from the cooling gas exhaust port. The insertion hole also serves as a connection mechanism for a cylindrical cooling head of the electric cooling device. That is, the electric cooling head having the same shape as the insertion hole can be fixed.
以上のように本発明による示差走査熱量計においては、ヒートシンクに固定された冷却機構は、液化窒素を用いた冷却装置の冷却ヘッドと電気冷却装置の冷却ヘッドの接続機構を共通化することで、冷却装置の切替えをそれぞれの冷却ヘッドを抜き差しするだけで行うことができ、温度範囲も容易に切り替えることが可能である。また、液化窒素を用いた冷却装置と電気冷却装置の２つの冷却装置が同時に装着できる機構におけるような、冷却ガスの供給を止めた時に、電気冷却ヘッド差し込んだままにしておいたことで、電気冷却ヘッドを損傷させたり、また、ヒートシンクの昇温効率を低下させることもない。 As described above, in the differential scanning calorimeter according to the present invention, the cooling mechanism fixed to the heat sink has a common connection mechanism between the cooling head of the cooling device using liquefied nitrogen and the cooling head of the electric cooling device. Switching of the cooling device can be performed simply by inserting / removing each cooling head, and the temperature range can also be switched easily. In addition, when the supply of the cooling gas is stopped, as in the mechanism in which the cooling device using liquefied nitrogen and the two cooling devices of the electric cooling device can be installed at the same time, the electric cooling head is left inserted. The cooling head is not damaged, and the heating efficiency of the heat sink is not reduced.
図１より本発明の示差走査熱量計と冷却機構５１について説明する。試料、基準物質を収納するヒートシンク１内に試料ホルダー２と基準物質ホルダー３がある。ヒートシンク１側面にはヒートシンク１を加熱するための絶縁皮膜付きヒーター４とヒートシンク温度を検知して温度制御のフィードバックに用いる制御熱電対５が設けられている。前記ヒートシンク１底面と前記試料及び基準物質ホルダー間には示差熱流検出器６があり、試料温度と、試料と基準物質の温度差を検出し、熱流差信号として出力される。
次に液化窒素を用いた冷却装置と電気冷却装置の接続機構の共通化を行った冷却機構５１を図２に示す。冷却機構は、ヒートシンク１下面に固定され、冷却ヘッド挿入穴７と冷却ガスを外部に排気するための冷却ガス排気口８を有している。また、冷却機構の上部に存在する示差熱流検出器６からの信号線を通すための貫通穴９が設けられている。
The differential scanning calorimeter and
Next, FIG. 2 shows a
次に液化窒素を用いた冷却装置の使用方法を冷却機構５１の上面に平行な、図２におけるＡ−Ａ‘線に沿った面で切断した断面図である図３と、冷却ガス導入ヘッド５２の図４を用いて説明する。液化窒素を用いた冷却装置使用時の場合、まず初めに冷却機構５１に冷却ガスを導入するための冷却ガス導入ヘッド５２を冷却ヘッド挿入穴７へ挿入する。液化窒素をヒーターによって気化された冷却ガスは、冷却ガス導入パイプ１１から導入され、冷却機構への導入口１２から冷却機構へ流れる。冷却機構５１へ流入した冷却ガスは、ガス流路１０を通り、冷却ガス排気口８から排気される。このとき、ガス流路１０によって冷却ガスと冷却機構５１間で熱交換が行われ、冷却機構５１全体が冷却される。また、冷却効率を高めるためにガス流路の表面を増やすための突起物１３を設けている。液化窒素を用いた冷却装置の場合、ヒートシンク１及び試料は約−１５０℃まで冷却される。
Next, FIG. 3 which is a cross-sectional view of the method of using the cooling device using liquefied nitrogen cut along a plane along the line AA ′ in FIG. 2 parallel to the upper surface of the
一方、電気冷却装置の場合であるが、電気冷却装置は、コンプレッサー式の冷媒循環による冷却装置である。金属製のパイプの中で冷媒が循環され、パイプ先端の金属製冷却ヘッドが冷却される。冷却ヘッドの装着は、冷却ヘッド挿入穴７の形状に適合した円柱型の冷却ヘッドを冷却ヘッド挿入穴７に挿入する。電気冷却装置が稼動すると初めに冷却ヘッドが、−９０℃前後にその後冷却機構全体が冷却される。電気冷却装置使用時の場合、ヒートシンク１及び試料は約−７５℃まで冷却される。
On the other hand, although it is a case of an electric cooling device, an electric cooling device is a cooling device by compressor type refrigerant circulation. The refrigerant is circulated in the metal pipe, and the metal cooling head at the tip of the pipe is cooled. The cooling head is mounted by inserting a cylindrical cooling head adapted to the shape of the cooling
各種冷却装置によって冷却された冷却機構とヒートシンクには温度差が生じ、ヒートシンクから冷却機構への熱流が生まれ、ヒートシンクは冷却される。 A temperature difference occurs between the cooling mechanism and the heat sink cooled by the various cooling devices, a heat flow from the heat sink to the cooling mechanism is generated, and the heat sink is cooled.
液化窒素を用いた冷却装置の場合、冷却を行う時、冷却ガスを供給する。ヒーターパワーを必要とする高速昇温や高温域の測定時にはヒートシンクから冷却機構への熱流の移動を抑え、昇温能力を維持するために、冷却ガスの供給を止めることができるので、−１５０から７２５℃までの広範囲な温度域で測定が可能となる。しかしながら、液化窒素を消費するので、液化窒素の補給の作業やランニングコストがかかる。 In the case of a cooling device using liquefied nitrogen, cooling gas is supplied when cooling is performed. In order to suppress the heat flow from the heat sink to the cooling mechanism and maintain the temperature rising capability at the time of high-temperature temperature rise or high temperature measurement requiring heater power, the supply of cooling gas can be stopped. Measurement is possible in a wide temperature range up to 725 ° C. However, since liquefied nitrogen is consumed, liquefied nitrogen replenishment work and running costs are required.
一方電気冷却装置は、電源の再投入は装置の特性上、電源を切ってから３０分程度時間を取らなければいけない点、電源が切れたままヒートシンクの昇温を行うとヒートシンクの熱により冷却機構が加熱され、冷却ヘッドの耐熱限界に達する点から、測定時は、常に電源を投入し、稼動する必要がある。そのため、電気冷却装置は、冷媒の補給のわずらわしさはないが、昇温時は、常にヒートシンクから冷却機構への熱流移動があるため、液化窒素を用いた冷却装置よりは、高温域の温度範囲が限定される。 On the other hand, in the electric cooling device, it is necessary to take about 30 minutes after the power is turned off due to the characteristics of the device. When the temperature of the heat sink is raised while the power is turned off, the cooling mechanism is caused by the heat of the heat sink. From the point that reaches the heat resistance limit of the cooling head, it is necessary to always turn on the power and operate during measurement. Therefore, the electric cooling device does not have the trouble of replenishing the refrigerant, but when the temperature is raised, there is always a heat flow from the heat sink to the cooling mechanism, so the temperature range is higher than the cooling device using liquefied nitrogen. Is limited.
このように各冷却装置には、それぞれ長所、短所があるため、測定用途に応じて冷却装置を切りかえることが理想である。例えば、通常は電気冷却装置を装着して測定し、６００℃を超える高温域や−１００℃以下の測定時は、液化窒素を用いた冷却装置に切り換える。これにより、液化窒素の補充も少なく、冷却装置の接続機構を共通化し、冷却装置の切り替えを冷却ヘッドの抜き差しのみで行えるため測定温度範囲も容易に切り替えが可能となる。 Thus, since each cooling device has advantages and disadvantages, it is ideal to switch the cooling device according to the measurement application. For example, the measurement is usually performed with an electric cooling device attached, and when measuring at a high temperature range exceeding 600 ° C. or at a temperature of −100 ° C. or lower, switching to a cooling device using liquefied nitrogen is performed. As a result, replenishment of liquefied nitrogen is small, the connection mechanism of the cooling device is made common, and switching of the cooling device can be performed only by inserting and removing the cooling head, so that the measurement temperature range can be easily switched.
Claims (2)
前記ヒートシンクの底板上に固定されている示差熱流検出器とを有する示差走査熱量計において、
冷却ガスを送出する送出穴を設けた冷却ガス導入用のガス冷却ヘッドまたは電気冷却ヘッドのいずれをも装着可能な挿入穴を有する前記ヒートシンクの底板下に固定した冷却機構と、
前記ガス冷却ヘッドの挿入時に該冷却ヘッドの前記ガス送出穴と一致する前記挿入穴の側壁に設けたガス導入口と、
該ガス導入口と連結し、その反対側にガス排気口を有したガス流路とを有し、
前記ガス冷却ヘッド又は前記電気冷却ヘッドの相互の脱着交換のみでガス冷却又は電気冷却の相互の冷却手段の切替えを可能としたことを特徴とする示差走査熱量計。 A heat sink containing a measurement sample and a reference material, a heater for heating the heat sink,
A differential scanning calorimeter having a differential heat flow detector fixed on the bottom plate of the heat sink;
A cooling mechanism fixed below the bottom plate of the heat sink having an insertion hole into which either a gas cooling head for introducing a cooling gas or an electric cooling head provided with a delivery hole for delivering a cooling gas can be mounted ;
A gas inlet provided in a side wall of the insertion hole that coincides with the gas delivery hole of the cooling head when the gas cooling head is inserted;
A gas flow path connected to the gas inlet and having a gas outlet on the opposite side;
A differential scanning calorimeter capable of switching between cooling means for gas cooling or electric cooling only by detaching and replacing the gas cooling head or the electric cooling head .
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| JP5283535B2 (en) * | 2009-02-20 | 2013-09-04 | 株式会社日立ハイテクサイエンス | Differential scanning calorimeter |
| JP5551811B2 (en) * | 2013-05-24 | 2014-07-16 | 株式会社日立ハイテクサイエンス | Differential scanning calorimeter |
| CN109164128B (en) * | 2018-10-29 | 2020-11-10 | 中国科学院上海硅酸盐研究所 | Furnace body for thermal analyzer |
| CN109164127B (en) * | 2018-10-29 | 2020-12-11 | 中国科学院上海硅酸盐研究所 | Cooler for thermal analyzer |
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| CN101938861A (en) * | 2010-08-17 | 2011-01-05 | 上海交通大学 | Linear heat source type heater for protecting and heating plate devices |
| CN101938861B (en) * | 2010-08-17 | 2013-01-02 | 上海交通大学 | Linear heat source type heater for protecting and heating plate devices |
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