JP4264935B2 - Corrosion resistance Long life High precision pressure gauge - Google Patents

Corrosion resistance Long life High precision pressure gauge Download PDF

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JP4264935B2
JP4264935B2 JP2003148706A JP2003148706A JP4264935B2 JP 4264935 B2 JP4264935 B2 JP 4264935B2 JP 2003148706 A JP2003148706 A JP 2003148706A JP 2003148706 A JP2003148706 A JP 2003148706A JP 4264935 B2 JP4264935 B2 JP 4264935B2
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Prior art keywords
pressure gauge
pressure
corrosion
corrosion resistance
diaphragm
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JP2003148706A
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JP2004354062A (en
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新太郎 石山
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独立行政法人 日本原子力研究開発機構
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Description

【0001】
【発明の属する技術分野】
本発明は、原子力分野及び一般産業分野における、高温強酸環境下で使用される圧力計の耐酸性、計測精度及びその寿命の向上を計るものである。
【0002】
【従来の技術】
従来の圧力計では、誤差出力が0.5%F.S(表示圧力のゼロから最高計測圧力値を示す)程度であり、更にその寿命も1×105サイクルが保証限界であった。
【0003】
【発明が解決しようとする課題】
従来の圧力計を高温且つ強酸環境下で使用した場合には、その耐酸性において十分なものでないために、その測定精度及びその寿命においても問題が生じていた。そこで、本発明では、かかる問題点を解決することにより、高温強酸環境下における圧力計の耐酸性、計測精度及びその寿命の向上を計るものである。
【0004】
【課題を解決するための手段】
本発明においては、圧力制御されるハロゲン化水素循環系のハロゲンに対する圧力計の耐食性並びに計測感度を向上させるために、圧力計のダイヤフラムのハロゲン化水素溶液接液側を耐食性の高いタンタル薄板の波板とし、その波板を接液側と反対側の圧力計構造材のステンレス材(SUS316)と接合した。この接合の際に施したアーク溶接により、タンタル/SUS316溶融部に弾性変形におけるヒステリシスが少なく、且つヒステリシスの繰り返しにおいて疲労強度の高いTa−Fe−Cr−Ni−Mo化合物を生成させたことにより、高温強酸環境下で使用される圧力計の耐酸性、計測精度及びその寿命の向上を計るものである。この圧力計により、核熱化学ISプロセス(水を原料とした硫酸とヨウ素化水素の分解合成混合サイクルで水素と酸素を生産できる)のヨウ化水素循環系の圧力制御が可能となる。
【0005】
即ち、本発明は、ハロゲン化水素溶液のハロゲン化水素雰囲気で使用される圧力計であって、その接液部側/機器側ケーシングでタンタル/ステンレス製のダイヤフラム構造を有することにより、2,500℃までの圧力計測が行え、誤差圧力が0.1%F.S(フルスケール)であり、且つ最高出力90%以上の繰り返し使用でも1×107サイクル以上の寿命を有する耐酸性且つ耐熱性の高温下で測定精度の高い圧力計である。
【0006】
【発明の実施の形態】
図1のヨウ化水素(HIx)循環試験用圧力センサーの高温耐食性圧力計の断面図に示されるように、圧力導入方向に対して垂直にタンタル製のダイヤフラムが設置される。このダイヤフラムは、圧力制御されるヨウ化水素循環試験装置内のヨウ化水素蒸気又は溶液(循環溶液の量によっては、溶液界面下に圧力計ダイヤフラム部も水没し、接液部が生ずる)に接しており、この溶液の圧力変動がダイヤフラムを介して測定されるように構成されている。
【0007】
このタンタル製のダイヤフラムは、図5(a)に示されるように、高温耐食性圧力計のステンレス(SUS313)製のケーシング基板材に溶接され、その溶接によりダイヤフラムのタンタル基板の外周辺が圧力計のケーシング基板材に結合される。この溶接部断面構造が図5(b)に示されている。ダイヤフラムのタンタル(Ta)基板とSUS316製のケーシング基板との間に形成された溶接部の内部構造は、図2及び図5(a)に示されるように、タンタル(Ta)基板端部を囲んで、溶融部▲2▼(Ta近傍)及び溶融部▲3▼(熱影響部)から構成されていている。
【0008】
図1のヨウ化水素循環試験用センサーは、高温耐食性圧力計及び高温耐食性温度計から構成されており、この圧力計及び温度計は、図6に示されるように、ヨウ化水素循環試験装置内に配置される。この装置内において、ヨウ化水素溶液は、SiC製プランジャーポンプによりTa製継手を経て、矢印方向に腐食サンプルに向けて送られ、ヨウ化水素溶液による腐食試験が行われる。その際ヨウ化水素蒸気又は溶液の圧力が、本発明の高温耐食性圧力計により測定され、その溶液の温度が高温耐食性温度計により測定される。圧力及び温度が測定されたヨウ化水素溶液は、超音波流量計においてその流速が測定された後、ガラスライニングエルボー配管を経て再びポンプへと環流される。
【0009】
本発明においては、タンタル製のダイヤフラムを溶接して得られた圧力計をヨウ化水素循環試験装置内のヨウ化水素溶液の循環系に設置し、その溶液の圧力、温度及び流速を測定しながら腐食サンプルの腐食状態を計測用観測ボードを透して観測するものである。特に、本発明においては、圧力計にタンタル製のダイヤフラムを溶接して使用しているので、その耐食性が飛躍的に向上し、その結果として圧力計の寿命を長引かせることにより高精度で圧力の測定ができるものである
【0010】
【実施例】
(ア)試作試験(タンタル製ダイヤフラムを溶接した腐食サンプルの試作)
図1に示す圧力計ダイヤフラム部にタンタル波板(板厚0.1mm)をアーク溶接した圧力計用の腐食サンプルを制作した。その際のアーク溶接条件は、溶接電流×速度、50A×7mm/sで、2回転溶接を行い、溶接棒はSUS316YL(JISG316)、線径(溶接棒直径)1mmで実施した。
【0011】
(イ)腐食試験(上記腐食サンプルの腐食試験)
ダイヤフラム溶接部用の腐食サンプルのヨウ化水素溶液中の腐食試験を実施した結果、図2に示すようにタンタル部及び溶融部がヨウ化水素の腐食に耐性を示すことが分かった。即ち、図2において、SUS316基板、熱影響部、Ta近傍、及びタンタル(Ta)基板からなる腐食サンプルに関するヨウ化水素(HI)溶液腐食速度をみると、Ta基板とSUS316基板との溶融部のTa近傍がTa基板以外では耐腐食性に最も富んでいることが分かった。したがって、ヨウ化水素溶液に接しているTa基板及び溶接部の耐腐食性が高いので、圧力計のダイヤフラムにタンタル材を使用すれば、耐腐食性能等を向上させることは明らかである。
【0012】
(ウ)高温試験
長時間ヨウ化水素溶液循環試験に用いたタンタル製のダイヤフラムを備えた圧力計について圧力計測時の誤差出力を313Kまで計測した。その結果、図3に示すように、温度の上昇とともに出力誤差は高くなるが、再現性(高温において圧力が上下したり、減圧、加圧したときの示指値のヒステリシス効果による誤差値が少ない)が良いので温度補正すれば高温での利用が可能であることが分かった。
【0013】
(エ)疲労試験
長時間ヨウ化水素溶液循環試験に用いたタンタル製のダイヤフラムを備えた圧力計について、繰り返し使用試験を行った。その結果、図4に示すように、最高出力の90%以上の繰り返し使用でも1×107サイクル以上で破壊せず、疲労初期で0.44%F.S(フルスケール)の誤差出力を生ずるものの、それ以降0.1%F.S以下であった。このことから、使用前に予め3×106サイクルの疲労を加えておけば、高精度化できることが分かる。
【0014】
【発明の効果】
本発明の圧力計は、強酸に対する耐食性能が高いので、原子力分野の外に、強酸を扱う化学プラント等への転用が有効である。
【図面の簡単な説明】
【図1】 タンタル製のダイヤフラムを使用した圧力計の構造を示す図である。
【図2】 タンタル/SUS316接合ダイヤフラム部のヨウ化水素溶液中の腐食試験結果を示す図である。
【図3】 タンタル製のダイヤフラムを使用した圧力計の高温試験の高温試験の結果を示す図である。
【図4】 タンタル製のダイヤフラムを使用した圧力計の疲労試験の高温試験の結果を示す図である。
【図5】 (a)Ta−SUS製ダイヤフラム及び(b)Ta−SUS316溶接部の断面構造を示す図である。
【図6】 ヨウ化水素循環試験装置の概要を示す図である。
[0001]
BACKGROUND OF THE INVENTION
The present invention is intended to improve the acid resistance, measurement accuracy and life of a pressure gauge used in a high temperature and strong acid environment in the nuclear field and general industrial field.
[0002]
[Prior art]
In the conventional pressure gauge, the error output is 0.5% F.S. It was about S (indicating the maximum measured pressure value from zero of the displayed pressure), and the lifetime was also a guaranteed limit of 1 × 10 5 cycles.
[0003]
[Problems to be solved by the invention]
When a conventional pressure gauge is used in a high temperature and strong acid environment, the acid resistance is not sufficient, and thus there is a problem in the measurement accuracy and the life. Therefore, in the present invention, by solving such problems, the acid resistance, measurement accuracy, and life of the pressure gauge in a high temperature and strong acid environment are improved.
[0004]
[Means for Solving the Problems]
In the present invention, in order to improve the corrosion resistance and measurement sensitivity of the pressure gauge against halogen in the hydrogen halide circulation system under pressure control, the wave of the tantalum thin plate having high corrosion resistance is placed on the wetted liquid solution side of the pressure gauge diaphragm. A corrugated plate was joined to a stainless steel (SUS316) of a pressure gauge structure material on the side opposite to the liquid contact side. By arc welding performed at the time of joining, a Ta-Fe-Cr-Ni-Mo compound having less hysteresis in elastic deformation in the tantalum / SUS316 melted portion and high fatigue strength in repeated hysteresis is obtained. It is intended to improve the acid resistance, measurement accuracy and life of pressure gauges used in high temperature and strong acid environments. This pressure gauge makes it possible to control the pressure of the hydrogen iodide circulation system in the nuclear thermochemical IS process (hydrogen and oxygen can be produced in a sulfuric acid and hydrogen iodide decomposition and synthesis cycle using water as a raw material).
[0005]
That is, the present invention is a pressure gauge used in a hydrogen halide atmosphere of a hydrogen halide solution, and has a diaphragm structure made of tantalum / stainless steel at the wetted part side / equipment side casing, thereby obtaining 2500 Can measure pressure up to ℃, error pressure is 0.1% F. The pressure gauge is S (full scale) and has a life of 1 × 10 7 cycles or more even when it is repeatedly used at a maximum output of 90% or more, and is a pressure gauge with high measurement accuracy under a high temperature and acid resistance.
[0006]
DETAILED DESCRIPTION OF THE INVENTION
As shown in the cross-sectional view of the high-temperature corrosion-resistant pressure gauge of the hydrogen iodide (HIx) circulation test pressure sensor in FIG. 1, a tantalum diaphragm is installed perpendicular to the pressure introduction direction. This diaphragm is in contact with hydrogen iodide vapor or a solution in the hydrogen iodide circulation test apparatus under pressure control (depending on the amount of the circulating solution, the pressure gauge diaphragm part is also submerged under the solution interface, resulting in a wetted part). The pressure fluctuation of the solution is measured through a diaphragm.
[0007]
As shown in FIG. 5A, the tantalum diaphragm is welded to a stainless steel (SUS313) casing substrate material of a high temperature corrosion resistance pressure gauge, and the outer periphery of the tantalum substrate of the diaphragm is welded to the pressure gauge. Bonded to the casing substrate material. This weld cross-sectional structure is shown in FIG. The internal structure of the weld formed between the tantalum (Ta) substrate of the diaphragm and the casing substrate made of SUS316 surrounds the end of the tantalum (Ta) substrate, as shown in FIG. 2 and FIG. Thus, it is composed of a melting part (2) (in the vicinity of Ta) and a melting part (3) (heat-affected zone).
[0008]
The hydrogen iodide circulation test sensor shown in FIG. 1 is composed of a high temperature corrosion resistance pressure gauge and a high temperature corrosion resistance thermometer. The pressure gauge and thermometer are located in the hydrogen iodide circulation test apparatus as shown in FIG. Placed in. In this apparatus, the hydrogen iodide solution is sent to the corrosion sample in the direction of the arrow through a Ta joint by a SiC plunger pump, and a corrosion test with the hydrogen iodide solution is performed. At that time, the hydrogen iodide vapor or the pressure of the solution is measured by the high-temperature corrosion-resistant pressure gauge of the present invention, and the temperature of the solution is measured by the high-temperature corrosion-resistant thermometer. The hydrogen iodide solution whose pressure and temperature have been measured is recirculated to the pump through the glass lining elbow pipe after its flow rate is measured by an ultrasonic flowmeter.
[0009]
In the present invention, a pressure gauge obtained by welding a diaphragm made of tantalum is installed in a hydrogen iodide solution circulation system in a hydrogen iodide circulation test apparatus, and while measuring the pressure, temperature and flow rate of the solution, The corrosion state of the corrosion sample is observed through the measurement observation board. In particular, in the present invention, a tantalum diaphragm is welded to the pressure gauge, so that the corrosion resistance is drastically improved, and as a result, the pressure gauge is highly accurate by prolonging the life of the pressure gauge. It can be measured. [0010]
【Example】
(A) Prototype test (Prototype of corrosion sample welded with tantalum diaphragm)
A corrosion sample for a pressure gauge was produced by arc-welding a tantalum corrugated sheet (plate thickness: 0.1 mm) to the pressure gauge diaphragm shown in FIG. The arc welding conditions at that time were welding current × speed, 50 A × 7 mm / s, two-turn welding was performed, and the welding rod was SUS316YL (JISG316) and the wire diameter (welding rod diameter) was 1 mm.
[0011]
(B) Corrosion test (corrosion test of the above corrosion sample)
As a result of conducting a corrosion test in a hydrogen iodide solution of a corrosion sample for a diaphragm welded portion, it was found that the tantalum portion and the melted portion are resistant to corrosion of hydrogen iodide as shown in FIG. That is, in FIG. 2, the hydrogen iodide (HI) solution corrosion rate for the corrosion sample composed of the SUS316 substrate, the heat affected zone, the vicinity of Ta, and the tantalum (Ta) substrate, the melting portion of the Ta substrate and the SUS316 substrate is shown. It was found that the vicinity of Ta has the most corrosion resistance except for the Ta substrate. Therefore, since the Ta substrate in contact with the hydrogen iodide solution and the welded portion have high corrosion resistance, it is clear that the use of a tantalum material for the pressure gauge diaphragm improves the corrosion resistance performance.
[0012]
(C) High temperature test The error output at the time of pressure measurement was measured up to 313K for a pressure gauge equipped with a tantalum diaphragm used for the hydrogen iodide solution circulation test for a long time. As a result, as shown in FIG. 3, the output error increases as the temperature rises, but reproducibility (the error value due to the hysteresis effect of the indicated value when the pressure rises and falls, or the pressure is reduced or increased at high temperature) is small. However, it was found that it can be used at high temperatures if the temperature is corrected.
[0013]
(D) Fatigue test A repeated use test was conducted on a pressure gauge equipped with a tantalum diaphragm used in a long-term hydrogen iodide solution circulation test. As a result, as shown in FIG. 4, even after repeated use of 90% or more of the maximum output, it did not break at 1 × 10 7 cycles or more, and 0.44% F.F. S (full scale) error output is generated, but 0.1% F.V. S or less. From this, it can be seen that high accuracy can be achieved if fatigue of 3 × 10 6 cycles is added in advance before use.
[0014]
【The invention's effect】
Since the pressure gauge of the present invention has high corrosion resistance against strong acids, it can be effectively used for chemical plants that handle strong acids in addition to the field of nuclear power.
[Brief description of the drawings]
FIG. 1 is a diagram showing the structure of a pressure gauge using a tantalum diaphragm.
FIG. 2 is a diagram showing a corrosion test result in a hydrogen iodide solution of a tantalum / SUS316 bonded diaphragm portion.
FIG. 3 is a diagram showing a result of a high temperature test of a high pressure test of a pressure gauge using a tantalum diaphragm.
FIG. 4 is a diagram showing the results of a high temperature test of a fatigue test of a pressure gauge using a tantalum diaphragm.
FIG. 5 is a view showing a cross-sectional structure of a (a) Ta-SUS diaphragm and (b) Ta-SUS316 welded portion.
FIG. 6 is a diagram showing an outline of a hydrogen iodide circulation test apparatus.

Claims (1)

耐食性長寿命高精度の圧力計において、前記圧力計が、循環ポンプによりハロゲン化水素溶液を循環用配管中で循環させ、前記配管に圧力計、温度計及び流量計を設置して前記溶液の圧力、温度及び流速を測定しながら腐食サンプルの腐食状態を前記配管に設けられた観測ボードを透して観測するハロゲン化水素溶液循環試験装置用の圧力計であり、前記圧力計がダイヤフラム型圧力計であって、そのダイヤフラムのハロゲン化水素溶液接液側を耐食性の高いタンタル薄板の波板とし、その波板を接液側と反対側の圧力計構造材のステンレスと溶接接合したことにより、2500℃までの圧力計測が行え、誤差圧力が0.1%F.S(フルスケール)であり、且つ最高出力90%以上の繰り返し使用でも1×10サイクル以上の寿命を有することを特徴とする、前記圧力計。Corrosion resistance Long life High-precision pressure gauge In the pressure gauge, the pressure gauge circulates a hydrogen halide solution in a circulation pipe by a circulation pump, and a pressure gauge, a thermometer and a flow meter are installed in the pipe, and the pressure of the solution A pressure gauge for a hydrogen halide solution circulation test apparatus for observing a corrosion state of a corrosion sample through an observation board provided in the pipe while measuring a temperature and a flow velocity, and the pressure gauge is a diaphragm type pressure gauge a is, by the hydrogen halide solution wetted side of the diaphragm and the corrugated sheet of high corrosion resistance of tantalum sheet, and stainless steel with welded opposite pressure gauge structural members of the corrugated plate and the liquid contact side, 2500 Can measure pressure up to , error pressure is 0.1% F. The pressure gauge is characterized by being S (full scale) and having a life of 1 × 10 7 cycles or more even after repeated use with a maximum output of 90% or more.
JP2003148706A 2003-05-27 2003-05-27 Corrosion resistance Long life High precision pressure gauge Expired - Fee Related JP4264935B2 (en)

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