JPH0365865B2 - - Google Patents

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Publication number
JPH0365865B2
JPH0365865B2 JP59183732A JP18373284A JPH0365865B2 JP H0365865 B2 JPH0365865 B2 JP H0365865B2 JP 59183732 A JP59183732 A JP 59183732A JP 18373284 A JP18373284 A JP 18373284A JP H0365865 B2 JPH0365865 B2 JP H0365865B2
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Prior art keywords
degree
resin
curing
value
electrical resistance
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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.)
Expired - Lifetime
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JPS6162853A (en
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Priority to JP18373284A priority Critical patent/JPS6162853A/en
Publication of JPS6162853A publication Critical patent/JPS6162853A/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/44—Resins; Plastics; Rubber; Leather
    • G01N33/442—Resins; Plastics
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/041—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body

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  • 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)

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 Industrial Application) 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、加熱成形によつ
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、試験片の成形、試験片の切り
出し、試験用の特別な材料、治具などが必要にな
り、製品価格上昇の原因になる。また、成形終了
後、評価試験の完了までに時間を要し、製造能率
の低下を招く。 The conventional method used for this determination is to manufacture a small test plate using the same material, same process, and same jig as the molded object, cut out a strength evaluation test piece from this test plate, and measure the required strength. conduct a test,
There is a method of estimating the strength of a molded article formed at the same time 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 molding jig, and in order to conduct this test, it is necessary to mold the test piece, cut out the test piece, use special materials for the test, use a jig, etc. will be required, which will cause an increase in product prices. Furthermore, it takes time to complete the evaluation test after the molding is completed, which leads to a decrease in manufacturing efficiency.

（発明の目的） 本発明は、従来技術の上記の問題に着目して得
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
目的とする。(Objective of the Invention) The present invention was achieved by focusing on the above-mentioned problems of the prior art, and quickly and accurately evaluates the degree of curing of the resin during the molding and heating process of a molded article containing a thermosetting resin. The purpose is to provide an inspection method that can make a determination.

（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tpを求め、ついでこの時
点tpにおける電気抵抗Ｒの増加速さ（dR／dt）pを
求める。その後は任意時点で、最確の増加速さ
（dR／dt）xを求め、式 CL＝｛１−（dR／dt）x／（dR／dt）p｝×100（％） による計算を行つて、硬化度CLを求めることに
より成形体中の熱硬化性樹脂の抵抗測定部位にお
ける硬化程度を評化する。(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 is measured, the time point t p at which the electrical resistance R starts to rise is determined from the electrical resistance R vs. time data, and the rate of increase in the electrical resistance R at this point t p is then calculated (dR/ dt) Find p . After that, at any point in time, find the most probable rate of increase (dR/dt) x and calculate using the formula CL = {1-(dR/dt) x / (dR/dt) p } x 100 (%). Then, by determining the degree of cure CL, the degree of cure at the resistance measurement site of the thermosetting resin in the molded article is evaluated.

又、樹脂の硬下終了は、硬化度CLによつて所
定の値を予め定めておき、前記計算によつて得ら
れる値がこの所定値に達した時に、硬化終了と判
断する。 Further, the end of hardening of the resin is determined by predetermining a predetermined value based on the degree of hardening CL, and when the value obtained by the above calculation reaches this predetermined value, it is determined that hardening has ended.

（発明の効果） 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。(Effects of the Invention) 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. The process can be easily and quickly performed, 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、長時間の加熱を行つても電
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 where 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
にそれぞれ対になつた電極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。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
インコーポレーテツド（Keithley Inc.）によ
り製造販売されているモデル619などの計測器を
用いることが望ましい。また、成形体１には表面
温度をモニターするための熱電対のような感温素
子４が接触させられ、この感温素子４は、温度変
換器５に接続されている。(Description of Examples) 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. Since it is necessary to measure a resistance value of several gigaohms as a high electrical resistance measuring instrument, it is preferable to use a measuring instrument such as model 619 manufactured and sold by Keithley Inc. in the United States. Further, a temperature sensing element 4 such as a thermocouple for monitoring the surface temperature is brought into contact with the molded body 1, and this temperature sensing element 4 is connected to a temperature converter 5.

計測器３および変換器５の出力はマイクロコン
ピユ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
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。 The outputs of the measuring device 3 and the converter 5 are connected to a processing device 6 such as a microcomputer, 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 measured over time by a temperature converter 5. and the value is given to the display device 7 via the processing device 6,
displayed on the display screen.

高抵抗計測器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。
処理装置６は、計測器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図のフローチヤートに従
つ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
入力され、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
入力が開始され、抵抗計測値Ｒが立ち上がり始め
たかどうかが判定される。抵抗計測値Ｒが立ち上
がり始めた、と判定されたとき、抵抗計測値Ｒの
経時的なとり込みが行なわれ、とり込まれた各時
点での計測値Ｒ（ｔ）が記憶される。ここで抵抗
Ｒを経時的に測定する理由は、絶縁抵抗Ｒの値が
室温では数百ギガオームという大きな値であるた
め測定条件のバラツキの影響が大きく、測定精度
が落ちることによる。抵抗値の変化は第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以
上になつたとき、最小自乗法により、はじめにＲ
の立ち上がり開始時点tpの最確値を求め、ついで
tpにおけるＲの増加速さ（dR／dt）pを求める。 The high resistance measuring device 3 continuously measures the surface resistance value of the molded body 1 and outputs the value to the processing device 6.
The processing device 6 takes in the measured values from the measuring device 3 over time and outputs them to the display device 7 to display the changes thereof. Further, the processing device 6 performs arithmetic processing according to the flowchart of FIG. 2 in order to evaluate the degree of hardening of the resin. That is, when heating of the molded body 1 begins, the measured value of the surface temperature T of the molded body 1 is input, and changes in the measured value are displayed on the display device 7 as described above. value
When Tc is reached, input of the resistance measurement value R from the measuring device 3 is started, and it is determined whether the resistance measurement value R has started to rise. When it is determined that the resistance measurement value R has started to rise, the resistance measurement value R is captured over time, and the measurement value R(t) at each time of capture is stored. The reason why the resistance R is measured over time is that the value of the insulation resistance R is a large value of several hundred gigaohms at room temperature, so the influence of variations in measurement conditions is large and the measurement accuracy decreases. The change in resistance value is shown in Figure 3.
This change is displayed on the display device 7. When the number of memorized points of the measured value R(t) exceeds a predetermined number, first R
Find the most probable value of the rising start point t p , and then
Find the rate of increase of R (dR/dt) p at t p .

その後、計測値Ｒ（ｔ）から適時、Ｒの増加速
さ（dR／dt）xを求め、式 CL＝｛１−（dR／dt）x／（dR／dt）p｝×100（％） に基づく演算を行なつて、硬化度CLを特る。こ
の硬化度CLは、あらかじめ設定された値と比較
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。硬化度CLの設定値は本来成形材
料の性質によつて決まるものであるが成形する部
品の用途、所定性能を考慮に入れ通常95〜98％の
値に設定する。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つて同様な判定をくり返す。 After that, calculate the rate of increase in R (dR/dt) x from the measured value R(t) and use the formula CL = {1-(dR/dt) x / (dR/dt) p } x 100 (%) Perform calculations based on , and determine the degree of hardening CL. This degree of hardening CL is compared with a preset value, and if the calculated value is greater than or equal to the set value, the heating molding process is terminated. The set value of the degree of hardening CL is originally determined by the properties of the molding material, but it is usually set at a value of 95 to 98%, taking into consideration the intended use and specified performance of the part to be molded. If the calculated value is smaller than the set value, the heat forming process is continued and the measured resistance value R(t)
Continue to import, and for each import, formula (1) and (2)
Perform calculations using formulas and repeat similar judgments.

第４図に加熱硬化型エポキシ樹脂の温度一定条
件での絶縁抵抗Ｒと時間ｔとの実験データを示
す。各測定データを整理して回帰分析した結果、
絶縁抵抗Ｒは図中の実線で示されるように Ｒ（ｔ）／Ａ＝１−e-kt の形で表されることがわかつた。 FIG. 4 shows experimental data regarding the insulation resistance R and time t of a thermosetting epoxy resin under constant temperature conditions. As a result of organizing each measurement data and performing regression analysis,
It was found that the insulation resistance R is expressed in the form R(t)/A=1-e -kt , as shown by the solid line in the figure.

いま、加熱硬化性樹脂の反応物の初期量をａと
し、反応量をｘとし、反応が未反応量の単純な一
次反応とするならば、反応速度Ｖは次式の通りと
なる。 Now, if the initial amount of the reactant of the thermosetting resin is a, the reaction amount is x, and the reaction is a simple first-order reaction of the unreacted amount, the reaction rate V is as shown in the following equation.

Ｖ＝dx／dt＝ａ−ｘ これを解けば、 ｘ／ａ＝１−e-kt となる。すなわち、樹脂の硬化反応が一次反応と
するならば、上記のＲ（ｔ）／Ａは、反応率ｘ／
ａに相当することとなる。 V=dx/dt=a-x If you solve this, x/a=1-e -kt . That is, if the curing reaction of the resin is a first-order reaction, the above R(t)/A is the reaction rate x/
This corresponds to a.

さらに、反応率が単純に樹脂の硬化度CLに比
例するとするならば、CLは次式で求まることと
なる。 Furthermore, if the reaction rate is simply proportional to the degree of curing CL of the resin, then CL can be found by the following equation.

CL＝Ｒ（ｔ）／Ａ x100（％） ＝（１−e-kt） 100（％） ＝１−（dR／dt）x／（dR／dt）p X100(%) 次に、これまでの推定の妥当性を判断するた
め、すなわちCLが実際の硬化度とどの程度一致
するかを確認するため、硬化度CLと樹脂の熱的
安定性をあらわすガラス移転温度Tgとの関係
（第５図）、さらに複合材料マトリツクス樹脂のひ
とつの強度を表す層間剪断強度ILSSとの関係
（第６図）を実験的に求めた。第５図、第６図か
らわかるように、硬化度CLとガラス移転温度Tg
と層間剪断強度ILSSは直線で回帰される強い相
関関係を有している。したがつて、前述のCLを
算出することにより樹脂の硬化程度、言い換えれ
ば所定の強度を有するか否かを判定することが可
能であることが判明した。 CL=R(t)/A x100(%) =(1-e -kt ) 100(%) =1-(dR/dt) x /(dR/dt) p X100(%) Next, In order to judge the validity of the estimation, that is, to confirm the extent to which CL matches the actual degree of hardening, we investigated the relationship between the degree of hardening CL and the glass transition temperature Tg, which represents the thermal stability of the resin (Fig. 5). ) and the interlaminar shear strength ILSS (Figure 6), which represents one strength of the composite matrix resin, was experimentally determined. As can be seen from Figures 5 and 6, the degree of hardening CL and the glass transition temperature Tg
and interlaminar shear strength ILSS have a strong correlation that is linearly regressed. Therefore, it has been found that by calculating the above-mentioned CL, it is possible to determine the degree of hardening of the resin, in other words, whether or not it has a predetermined strength.

以上の実験結果は熱効果性樹脂の一つであるエ
ポキシ樹脂に関してのものではあるが、他の熱硬
化性樹脂であるポリイミド樹脂での実験データを
第７図に示す。この樹脂についても絶縁抵抗はＲ
＝Ａ（１−e-kt）の形に回帰される。これらの結
果は樹脂の硬化反応が一種のイオン反応であり反
応が未反応分の濃度に依存する化学反応であるこ
とを示しており、本反応は基本的に架橋反応タイ
プであるところの熱硬化性樹脂一般に適用しうる
ものである。 Although the above experimental results are related to epoxy resin, which is one of the thermosetting resins, experimental data on polyimide resin, which is another thermosetting resin, is shown in FIG. The insulation resistance of this resin is R
=A(1-e -kt ). These results indicate that the resin curing reaction is a type of ionic reaction, and that the reaction is a chemical reaction that depends on the concentration of unreacted components.This reaction is basically a crosslinking reaction type, but thermosetting. It can be applied to general resins.

【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ツク図、第２図は本
発明の方法を実行するためのプログラムフローの
一例を示すフローチヤート、第３図は成形体の温
度および電気抵抗の変化を示す図表である。第４
図は実験データであつて抵抗値と時間との関係を
示す図、第５図は硬化度とガラス移転温度との関
係を示す図、第６図はガラス移転温度と層間剪断
強度との関係を示す図である。第７図は他の樹脂
での実験データであつて抵抗値と時間との関係を
示す図である。 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, Fig. 2 is a flowchart showing an example of a program flow for executing the method of the present invention, and Fig. 3 is a molding It is a chart showing changes in body temperature and electrical resistance. Fourth
The figure shows experimental data and shows the relationship between resistance value and time, Figure 5 shows the relationship between degree of hardening and glass transition temperature, and Figure 6 shows the relationship between glass transition temperature and interlaminar shear strength. FIG. FIG. 7 is a diagram showing experimental data using other resins, showing the relationship between resistance value and time. DESCRIPTION OF SYMBOLS 1... Molded object, 2... Electrode, 3... High electrical resistance measuring device, 6... Processing device, 7... Display device.

Claims (1)

【特許請求の範囲】 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）p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）x／（dR／dt）p｝×100（％） ただし、ｔ：時間 に基づく計算を行つて硬化度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。 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、前記計算によつ
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。[Claims] 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 during the molding and curing process of the molded body. , find the rate of increase in electrical resistance R (dR/dt),
From the rate of increase (dR/dt) p at the start of the rise of the electrical resistance R and the rate of increase (dR/dt) x at any point thereafter, the formula CL = {1-(dR/dt) x /( dR/dt) p } × 100 (%) where t: Calculations based on time are performed to obtain the degree of cure CL, thereby evaluating the degree of cure at the resistance measurement site of the resin in the molded article. A method for inspecting the degree of curing in the curing process of thermosetting resin. 2. In the method of item 1 above, a predetermined value for the degree of curing CL is determined in advance, and when the value of CL obtained by the calculation reaches the predetermined value,
A method of testing the degree of curing to determine when the resin has finished curing.
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 JPS6162853A (en) 1986-03-31
JPH0365865B2 true JPH0365865B2 (en) 1991-10-15

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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)

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Publication number Priority date Publication date Assignee Title
JP3282064B2 (en) * 1995-02-28 2002-05-13 株式会社オーク製作所 Apparatus and method for measuring degree of cure of ultraviolet-curable transfer coating material containing colorant
JP5309706B2 (en) * 2008-06-13 2013-10-09 Ｊｆｅスチール株式会社 Diagnostic method of power cable at the time of power cable repair
GR20080100768A (en) * 2008-07-30 2010-02-24 Νικολαος Γρηγοριου Παντελελης System for monitoring a forming process of reactant mixtures.

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1049791A1 (en) * 1981-04-27 1983-10-23 Ленинградский Ордена Ленина,Ордена Октябрьской Революции И Ордена Трудового Красного Знамени Горный Институт Им.Г.В.Плеханова Process for determining adhesion of binding agent to solid surface

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