JPS6162853A - Inspection for degree of curing in process of hardening thermosetting resin - Google Patents

Inspection for degree of curing in process of hardening thermosetting resin

Info

Publication number
JPS6162853A
JPS6162853A JP18373284A JP18373284A JPS6162853A JP S6162853 A JPS6162853 A JP S6162853A JP 18373284 A JP18373284 A JP 18373284A JP 18373284 A JP18373284 A JP 18373284A JP S6162853 A JPS6162853 A JP S6162853A
Authority
JP
Japan
Prior art keywords
degree
curing
molding
resin
hardening
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP18373284A
Other languages
Japanese (ja)
Other versions
JPH0365865B2 (en
Inventor
Yasuhiro Ito
康宏 伊藤
Yoshiji Ito
好二 伊藤
Katsuji Sakamoto
坂元 勝治
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Institute of Advanced Industrial Science and Technology AIST
Original Assignee
Agency of Industrial Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Agency of Industrial Science and Technology filed Critical Agency of Industrial Science and Technology
Priority to JP18373284A priority Critical patent/JPS6162853A/en
Publication of JPS6162853A publication Critical patent/JPS6162853A/en
Publication of JPH0365865B2 publication Critical patent/JPH0365865B2/ja
Granted legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/44Resins; Plastics; Rubber; Leather
    • G01N33/442Resins; Plastics
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/041Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)

Abstract

PURPOSE:To evaluate the degree of hardening of a molding quickly a non- destructive manner during the hardening thereof, by measuring the electric resistance value of a resin secularly during the molding/heating process thereof to determine the curing level CL of the resin from the increment rate of the measured value. CONSTITUTION:Electrodes 2 are stuck in pairs separately at proper points of a molding 1. These electrodes are connected to a high electric resistance measuring device 3. A thermosensitive element 4 like a thermocouple is brought into contact with the molding 1 to monitor the surface temperature thereof and is connected to a temperature converter 5. Outputs of the measuring device 3 and the converter 5 are connected to a processor 6 like a microcomputer and the results of the computation are outputted to a display 7. The molding 1 is placed into a heater/pressurizer, the surface temperature T is measured secularly with the temperature converter 5 and the value thereof is applied to the display 7 via the processor 6. Likewise, measured resistance values are applied to the display 7 via the processor 6 to obtain the curing level CL from changes in the resistance R.

Description

【発明の詳細な説明】 産業上の利用分野 本発明は、熱硬化性樹脂の硬化工程における硬化程度の
検査方法に関する。
DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for inspecting the degree of curing in the curing process of thermosetting resin.

(先行技術) エポキシ樹脂系複合材料のような熱硬化性樹脂を含む材
料からなる成形体では、加熱成形によって樹脂が十分に
硬化したかどうかを判定する必要がある。
(Prior Art) In a molded article made of a material containing a thermosetting resin, such as an epoxy resin-based composite material, it is necessary to determine whether the resin has been sufficiently cured by thermoforming.

この判定のために従来採用されている方法としては、成
形体と同一材料、同一工程、同一治具で小形の試験板を
製作し、この試験板から強度評価試験片を切り出して、
所要の強度試験を行ない、その結果により、同時に成形
した成形体の強度を推定する方法がある。しかし、この
従来の方法は、試験片が成形体から切り出されたもので
はないため間接的評価となり、大型、厚肉あるいは形状
の複雑な成形体のばあいには、判定の信頼性の問題が生
じる。さらに、試験板製作のために、成形治具に余分の
加工が必要になり、かつこの試験を行なうためには、試
験板の成形、試験片の切り出し、本発明は、従来技術の
上記の問題に71目して111ら゛れたもので、熱硬化
性樹脂を含む成形体の成形加熱工程中に、樹脂の硬化程
度を迅速かつ精度よく評価し、判定できる検査方法を提
供することを目1白とする。
The conventional method for making this determination is to manufacture a small test plate using the same material, same process, and same jig as the molded body, and cut out a strength evaluation test piece from this test plate.
There is a method of conducting required strength tests and estimating the strength of the molded product simultaneously molded based on the results. However, this conventional method is an indirect evaluation because the test piece is not cut out from the molded product, and there is a problem with the reliability of the judgment in the case of large, thick-walled, or complex-shaped molded products. arise. Furthermore, in order to manufacture the test plate, extra processing is required on the forming jig, and in order to conduct this test, the test plate must be formed and the test piece cut out. The purpose of this invention is to provide an inspection method that can quickly and accurately evaluate and determine the degree of hardening of a resin during the molding and heating process of a molded article containing a thermosetting resin. 1 white.

(発明の構成) 本発明による熱硬化性樹脂の硬化程度の検査方法は、熱
硬化性樹脂を含む成形体に高電気抵抗測定用電極を貼り
付けて、該成形体の成形硬化過程を通して経時的に成形
体中の樹脂の電気抵抗Rを測定し、電気抵抗R対時間デ
ータから、電気抵抗Rの立ち上がり開始時点t。を求め
、ついでこの時点t。における電気抵抗Rの増加速さく
dR/dt)。を求める。その後は任意時点で、最確の
増加速さくdR/dt)、を求め、式 による計りを行って、硬化度CLを求めることに断する
(Structure of the Invention) The method for inspecting the degree of curing of a thermosetting resin according to the present invention involves attaching a high electrical resistance measuring electrode to a molded article containing a thermosetting resin, and measuring the temperature over time during the molding and curing process of the molded article. The electrical resistance R of the resin in the molded body was measured at , and from the electrical resistance R vs. time data, the rise start point t of the electrical resistance R was determined. , and then at this point t. The rate of increase in electrical resistance R at dR/dt). seek. Thereafter, at an arbitrary point in time, the most probable rate of increase (dR/dt) is determined, and measurement is performed using the formula to determine the degree of hardening CL.

(発すの効果) 本発明は、上述のとおり、樹脂の成形加熱工程中に該樹
脂の電気抵抗値を経時的に測定し、その測定値の増加率
から樹脂の硬化度CLを求めるため、演算が容易で高速
化でき、成形体の硬化中に、非破壊で迅速に硬化程度を
検査することができる。
(Effect of emitting light) As described above, the present invention measures the electrical resistance value of the resin over time during the molding and heating process of the resin, and calculates the degree of curing CL of the resin from the increase rate of the measured value. This method is easy and can be performed at high speed, and the degree of curing can be quickly and non-destructively inspected while the molded product is being cured.

又、電気抵抗の任意時点における増加率で硬化程度を評
価するため、長時間の加熱を行っても電気抵抗Rの増加
傾向が残るような反応速度の遅い樹脂の硬化程度の判断
が可能である。
In addition, since the degree of curing is evaluated based on the rate of increase in electrical resistance at any point in time, it is possible to judge the degree of curing of resins with a slow reaction rate in which the tendency of increase in electrical resistance R remains even after long-term heating. .

〈実施例の説明) 第1図を参照すると、成形体1には適当な個処にそれぞ
れ対になった電極2が貼付けられており、これら電極は
高電気抵抗計測器3に接続される。
<Description of Embodiments> Referring to FIG. 1, pairs of electrodes 2 are pasted at appropriate locations on a molded body 1, and these electrodes are connected to a high electrical resistance measuring device 3.

高電気抵抗計測器としては、数ギガオームの抵抗値の測
定が必要であるため、米国ケイスレイ インコーホレー
テッド(K旧七旧ey Inc、  )により製造販売
されているモデル619などの計測器を用ピニータのよ
うな処理装置6に接続され、処理装置6はその演算結果
を表示装置7に出力する。成1形体1は、オートクレー
ブなどの加熱加圧装置内に入れられて、公知の方法で成
形圧力を与えられながら加熱されるのであるが、その間
の表面温度Tは温度変換器5により経時的に計測されて
、その値が処理装置6を経て表示装置7に与えられ、表
示画面に表示される。
As a high electrical resistance measuring instrument, it is necessary to measure a resistance value of several gigaohms, so we use a measuring instrument such as Model 619 manufactured and sold by Keithley Inc. It is connected to a processing device 6 such as a pinita, and the processing device 6 outputs the calculation results to a display device 7. The molded body 1 is placed in a heating and pressurizing device such as an autoclave and heated while applying molding pressure using a known method. During this time, the surface temperature T is changed over time by a temperature converter 5. The measured value is given to the display device 7 via the processing device 6 and displayed on the display screen.

高抵抗剖測器3は、成形体1の表面抵抗値を連続的に測
定し、その値を処理装置6に出力する。
The high-resistance autopsy instrument 3 continuously measures the surface resistance value of the molded body 1 and outputs the value to the processing device 6 .

処理装置6は、訓測器3からの計測値を経時的にとり込
んで表示装置7に出力し、その変化の様子を表示させる
。また、処理装置6は、樹脂の硬化程度の評価のため、
第2図のフローチャートに従った演算処理を行なう。す
なわち、成形体1の加熱が始まると、成形体1の表面温
度Tの計測値が人力され、その計測値の変化は前述のよ
うに表示装置7に表示されるのであるが、温度Tが所定
値Tcに達したとき計測器3からの抵抗計測値Rの第3
図にRで示すようになり、この変化は表示装置7に表示
される。計測値R(t)の記憶点数が所定の数層上にな
ったとき、最小自乗法により、はじめにRの立ち上がり
開始時点t。の最確値を求め、ついでt。におけるRの
増加速さくdR/di)。
The processing device 6 takes in the measured values from the training measuring device 3 over time and outputs them to the display device 7 to display the changes thereof. In addition, the processing device 6 is configured to evaluate the degree of curing of the resin.
Arithmetic processing is performed according to the flowchart in FIG. That is, when heating of the molded body 1 starts, the measured value of the surface temperature T of the molded body 1 is manually input, and the change in the measured value is displayed on the display device 7 as described above. The third of the resistance measurement value R from the measuring instrument 3 when the value Tc is reached.
This change is indicated by R in the figure, and this change is displayed on the display device 7. When the number of storage points of the measured value R(t) reaches a predetermined number of layers, the rise start point t of R is first determined by the least squares method. Find the most probable value of t. The rate of increase in R at dR/di).

を求める。seek.

その後、計測値R(t)から適時、Rの増加速さくcl
 R/、、d t ) 、を求め、式に基づく演算を行
なって、硬化度CLを碍る。この硬化度CLは、あらか
じめ設定された値と仕較され、演算値が設定値以上であ
れば加熱成形工程を終了させる。演算値が設定値より小
さいばあいには、加熱成形工程を続行し、抵抗計測値R
(t)のとり込みを続け、各とり込み毎に(1)式およ
び(2)式による演算を行なって同様な判定をくり返ず
After that, from the measured value R(t), calculate the increase rate of R at a suitable time by cl
R/, d t ), and perform calculations based on the formula to improve the degree of hardening CL. This degree of hardening CL is compared with a preset value, and if the calculated value is equal to or greater than the set value, the thermoforming process is terminated. If the calculated value is smaller than the set value, the heat forming process is continued and the measured resistance value R
Continuing to import (t), perform calculations using equations (1) and (2) for each import, and repeat the same judgment.

【図面の簡単な説明】[Brief explanation of drawings]

第1図は本発明の樹脂硬化程度検査方法に用いられる装
置の一例を示すブロック図、第2図は本1・・・成形体
、2・・・電極、 3・・・高電気抵抗計測器、6・・・処理装置、7・・
表示装置
Fig. 1 is a block diagram showing an example of an apparatus used in the resin curing degree inspection method of the present invention, and Fig. 2 shows the following: 1... molded body, 2... electrode, 3... high electrical resistance measuring device , 6... processing device, 7...
display device

Claims (2)

【特許請求の範囲】[Claims] (1)熱硬化性樹脂を含む成形体に高電気抵抗測定用電
極を貼り付けて、該成形体の成形硬化過程を通して経時
的に成形体中の樹脂の電気抵抗Rを測定し、電気抵抗R
の増加速さ(dR/dt)を求め、該電気抵抗Rの立ち
上がり開始時点の増加速さ(dR/dt)_oと、それ
以後の任意時点の増加速さ(dR/dt)_xから式 CL={1−(dR/dt)_o/(dR/dt)_x
}×100(%)ただし、t:時間 に基づく計算を行って硬化度CLを求めることにより、
成形体中の樹脂の抵抗測定部位における硬化程度を評価
することを特徴とする熱硬化性樹脂の硬化工程における
硬化程度の検査方法。
(1) A high electrical resistance measuring electrode is attached to a molded body containing a thermosetting resin, and the electrical resistance R of the resin in the molded body is measured over time through the molding and curing process of the molded body.
Find the rate of increase (dR/dt) of the electric resistance R, and use the rate of increase (dR/dt)_o at the time when the electrical resistance R starts to rise and the rate of increase (dR/dt)_x at any point thereafter to the formula CL. ={1-(dR/dt)_o/(dR/dt)_x
}×100(%) However, by calculating the degree of curing CL by calculating based on t: time,
1. A method for inspecting the degree of hardening in a thermosetting resin curing process, which comprises evaluating the degree of hardening at a resistance measurement site of a resin in a molded article.
(2)前記第(1)項の方法において、硬化度CLにつ
いて所定の値を予め定めておき、前記計算によって得ら
れるCLの値が、前記所定値に達したとき、樹脂の硬化
終了と判定する硬化程度の検査方法。
(2) In the method of item (1) above, a predetermined value is determined in advance for the degree of curing CL, and when the value of CL obtained by the calculation reaches the predetermined value, it is determined that the curing of the resin is completed. A method of inspecting the degree of hardening.
JP18373284A 1984-09-04 1984-09-04 Inspection for degree of curing in process of hardening thermosetting resin Granted JPS6162853A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP18373284A JPS6162853A (en) 1984-09-04 1984-09-04 Inspection for degree of curing in process of hardening thermosetting resin

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP18373284A JPS6162853A (en) 1984-09-04 1984-09-04 Inspection for degree of curing in process of hardening thermosetting resin

Publications (2)

Publication Number Publication Date
JPS6162853A true JPS6162853A (en) 1986-03-31
JPH0365865B2 JPH0365865B2 (en) 1991-10-15

Family

ID=16140999

Family Applications (1)

Application Number Title Priority Date Filing Date
JP18373284A Granted JPS6162853A (en) 1984-09-04 1984-09-04 Inspection for degree of curing in process of hardening thermosetting resin

Country Status (1)

Country Link
JP (1) JPS6162853A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0730148A3 (en) * 1995-02-28 1998-05-27 Orc Manufacturing Co., Ltd. Apparatus and method to measure the hardening of a UV-curable agent containing pigment
JP2009300275A (en) * 2008-06-13 2009-12-24 Jfe Steel Corp Diagnosis method of power cable when power cable is repaired
GR20080100768A (en) * 2008-07-30 2010-02-24 Νικολαος Γρηγοριου Παντελελης System for monitoring a forming process of reactant mixtures.

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57190257A (en) * 1981-04-27 1982-11-22 Le Goruni I Im Jii Bui Purehan Method and device for measuring structure forming motion in binder

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57190257A (en) * 1981-04-27 1982-11-22 Le Goruni I Im Jii Bui Purehan Method and device for measuring structure forming motion in binder

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0730148A3 (en) * 1995-02-28 1998-05-27 Orc Manufacturing Co., Ltd. Apparatus and method to measure the hardening of a UV-curable agent containing pigment
JP2009300275A (en) * 2008-06-13 2009-12-24 Jfe Steel Corp Diagnosis method of power cable when power cable is repaired
GR20080100768A (en) * 2008-07-30 2010-02-24 Νικολαος Γρηγοριου Παντελελης System for monitoring a forming process of reactant mixtures.

Also Published As

Publication number Publication date
JPH0365865B2 (en) 1991-10-15

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