JP2014126536A - Stretch test method - Google Patents
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- JP2014126536A JP2014126536A JP2012285657A JP2012285657A JP2014126536A JP 2014126536 A JP2014126536 A JP 2014126536A JP 2012285657 A JP2012285657 A JP 2012285657A JP 2012285657 A JP2012285657 A JP 2012285657A JP 2014126536 A JP2014126536 A JP 2014126536A
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- 238000010998 test method Methods 0.000 title claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 33
- 229920001971 elastomer Polymers 0.000 claims abstract description 13
- 238000001125 extrusion Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 abstract description 6
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 238000004073 vulcanization Methods 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- 229920002725 thermoplastic elastomer Polymers 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- ZZMVLMVFYMGSMY-UHFFFAOYSA-N 4-n-(4-methylpentan-2-yl)-1-n-phenylbenzene-1,4-diamine Chemical compound C1=CC(NC(C)CC(C)C)=CC=C1NC1=CC=CC=C1 ZZMVLMVFYMGSMY-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000007652 sheet-forming process Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
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- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
Description
本発明は、材料、特にゴム材料の力学試験として実施されている伸長試験方法に関する。 The present invention relates to an elongation test method implemented as a mechanical test of materials, particularly rubber materials.
耐久性などの高分子材料の製品の評価を行う際の基礎情報としては、等方性材料の応力ひずみ関係が必要となる。ゴム材料の伸長試験では、プレス加硫して得られた厚みが約１〜２ｍｍの短冊型試験片をチャックではさみ、伸長したときの伸長度に対する応力を測定する。ゴム材料自体は等方性の材料であり、本来的には評価結果に異方性は生じることはない。 As basic information for evaluating products of polymer materials such as durability, the stress-strain relationship of isotropic materials is required. In the elongation test of a rubber material, a strip-shaped test piece having a thickness of about 1 to 2 mm obtained by press vulcanization is sandwiched with a chuck, and the stress with respect to the degree of elongation is measured. The rubber material itself is an isotropic material, and there is essentially no anisotropy in the evaluation results.
しかしながら、たとえばゴム材料では、プレスをする前にシート成形工程においてロールミルでシート出しを行うため、シート出し時にゴム分子が伸長され、シート出し方向に配向し、押出し時の流動履歴がサンプルに残存する。そのため、伸長方向（ＭＤ）と幅方向（ＴＤ）で異なる応力・ひずみ挙動を示し、安定したデータが取得できないという問題がある。たとえば、このように伸長したサンプルを押出し後、緩和時間の５倍ほど放置しておくと、配向の影響がなくなるが、そのためにはシート出し後、加硫まで１日〜３日放置しておく必要がある。よって、配向しているサンプルの応力・ひずみ挙動から実際に取得したい非配向状態の応力・ひずみ挙動を短時間で推測することも困難である。これらの問題は、特にゴム材料の粘度が高い場合に顕著になる傾向がある。 However, for example, in the case of a rubber material, the sheet is unrolled by a roll mill in the sheet forming process before pressing, so that the rubber molecules are stretched during sheet unloading and oriented in the sheet unloading direction, and the flow history during extrusion remains in the sample. . Therefore, there is a problem that different stress / strain behavior is exhibited in the extension direction (MD) and the width direction (TD), and stable data cannot be acquired. For example, if the sample thus stretched is left to stand for about 5 times the relaxation time after being extruded, the influence of the orientation is eliminated, but for that purpose, it is left for 1 to 3 days until vulcanization after sheeting. There is a need. Therefore, it is also difficult to estimate in a short time the stress / strain behavior in the non-oriented state that is actually desired to be obtained from the stress / strain behavior of the oriented sample. These problems tend to be prominent especially when the viscosity of the rubber material is high.
一方、異方性材料の等方的な力学特性を測定する方法として、ねじりせん断を印加する方法が知られている（特許文献１）。しかしながら、せん断を印加する場合、破断点までの大きなひずみを印加することができないため、破断特性を評価することはできない。 On the other hand, a method of applying torsional shear is known as a method for measuring isotropic mechanical properties of anisotropic materials (Patent Document 1). However, when applying shear, a large strain up to the breaking point cannot be applied, so the breaking characteristics cannot be evaluated.
本発明は、配向した材料を用いて、配向の影響を打ち消し、無配向状態の材料の応力・ひずみ挙動を短時間で推測できる方法を提供することを目的とする。 An object of the present invention is to provide a method capable of canceling the influence of orientation and estimating the stress / strain behavior of a non-oriented material in a short time using an oriented material.
発明者は、配向した材料の試験片の伸長試験について詳細に検討したところ、押出し方向に対して、約４５°の方向に傾けてサンプルを切り出せば、配向の影響が打ち消されることを見出し、本発明を完成した。 The inventor has examined in detail the elongation test of the specimen of the oriented material, and found that if the sample is cut at an angle of about 45 ° with respect to the extrusion direction, the influence of the orientation is canceled out. Completed the invention.
すなわち、本発明は、シート押出時の伸長方向に対して３７〜５３°傾けて切り出した試験片を使用することを特徴とする材料の伸長試験方法に関する。 That is, the present invention relates to a material elongation test method characterized by using a test piece that is cut at an angle of 37 to 53 ° with respect to the elongation direction during sheet extrusion.
試験片の厚さは、０．５〜３ｍｍが好ましい。 The thickness of the test piece is preferably 0.5 to 3 mm.
本発明によれば、シート押出時の伸長方向に対して特定の角度傾けて切り出した試験片を使用するため、異方性の残った配向した材料であっても、配向の影響を打ち消し、短時間で無配向状態のゴム材料の応力・ひずみ挙動を推測することができる。 According to the present invention, a test piece cut at a specific angle with respect to the extension direction at the time of sheet extrusion is used. The stress / strain behavior of a non-oriented rubber material over time can be estimated.
本発明の材料の伸長試験方法は、シート押出時の伸長方向に対して３７〜５３°傾けて切り出した試験片を使用することを特徴とする。 The material elongation test method of the present invention is characterized by using a test piece that is cut at an angle of 37 to 53 ° with respect to the elongation direction during sheet extrusion.
試験片を切り出すため、プレス成形や射出成形で作製した材料を用いることが多い。シートの材料がゴムや熱可塑性エラストマーなど、溶融時の粘度が高い材料の場合、一旦ロールミルや押出し成形でサンプルを０．５〜５ｍｍに押出して、薄物のシートを作製してからプレス成形を行う。ロールや押出し金型でシートを作製したのちに試験片を切り出した場合には、押し出し時の流動の履歴が試験片に残るため、ゴム分子がシートの流れ方向に配向して、異方性を持つ試験片が得られる。 In order to cut out a test piece, a material produced by press molding or injection molding is often used. When the material of the sheet is a material with high viscosity at the time of melting, such as rubber or thermoplastic elastomer, the sample is once extruded to 0.5 to 5 mm by a roll mill or extrusion molding to produce a thin sheet, and then press molding is performed. . When a test piece is cut out after producing a sheet with a roll or an extrusion mold, the flow history during extrusion remains in the test piece. A test piece is obtained.
伸長試験（引張試験）は、材料の基礎物性評価として一般的に使用される方法である。短冊状に切り出した試験片を用い、伸びと力の関係（応力・ひずみ関係）を測定し、その関係から、破断点伸度、破断点応力、弾性率を評価する。 The elongation test (tensile test) is a method generally used for evaluating the basic physical properties of materials. Using a test piece cut into a strip shape, the relationship between elongation and force (stress / strain relationship) is measured, and the elongation at break, stress at break, and elastic modulus are evaluated from the relationship.
試験片の切り出しの際に、伸長方向に対して傾ける角度は、４０〜５０°が好ましい。５３°を超える、または、３７°未満では異方性が顕著になる傾向がある。図１および２に示す試験片の切り出し態様の中で、（ｂ）が本発明における試験片の切り出し態様であり、伸長方向に対して４５°傾けて切り出す。切り出される形状は特に限定されず、たとえば、長方形、正方形、ダンベル形状などが挙げられる。なお、図中の矢印は、シート作製時の伸長方向（ＭＤ）を表す。 When the test piece is cut out, the angle of inclination with respect to the extending direction is preferably 40 to 50 °. If it exceeds 53 ° or less than 37 °, anisotropy tends to be remarkable. Among the cut-out modes of the test piece shown in FIGS. 1 and 2, (b) is a cut-out mode of the test piece in the present invention, which is cut at 45 ° with respect to the extending direction. The shape to be cut out is not particularly limited, and examples thereof include a rectangle, a square, and a dumbbell shape. In addition, the arrow in a figure represents the expansion | extension direction (MD) at the time of sheet | seat preparation.
切り出した試験片の厚さは、特に限定されないが、０．５〜３ｍｍが好ましい。３ｍｍを超えると、加える応力が大きくなり、０．５ｍｍ未満では、チャックから外れやすくなる傾向がある。 Although the thickness of the cut-out test piece is not specifically limited, 0.5-3 mm is preferable. If it exceeds 3 mm, the applied stress increases, and if it is less than 0.5 mm, it tends to come off from the chuck.
切り出した試験片は、一軸伸長試験だけでなく、等二軸伸長やその他の測定にも利用する事ができる。 The cut specimen can be used not only for a uniaxial extension test but also for equibiaxial extension and other measurements.
溶融時に配向して異方性を示す材料としては、溶融時の粘度が高い材料が挙げられる。粘度が高いため、押出し伸長時の緩和時間が長くなるので、異方性の影響が発現しやすくなる。溶融時の粘度の高い材料としては、例えば、ゴムや超高分子量高分子材料だけでなく、高充填フィラー材料、熱可塑エラストマーなどが挙げられる。材料のムーニー粘度は８０以上の場合に、特に本発明の方法を好適に適用することができる。 Examples of the material that is oriented when melted and exhibits anisotropy include materials having a high viscosity when melted. Since the viscosity is high, the relaxation time at the time of extrusion elongation becomes long, so that the influence of anisotropy is easily expressed. Examples of the material having a high viscosity at the time of melting include not only rubber and ultrahigh molecular weight polymer material, but also highly filled filler material, thermoplastic elastomer, and the like. In particular, when the Mooney viscosity of the material is 80 or more, the method of the present invention can be suitably applied.
実施例に基づいて、本発明を具体的に説明するが、本発明はこれらのみに限定されるものではない。 The present invention will be specifically described based on examples, but the present invention is not limited to these examples.
（ゴム材料の作製）
以下に示す硫黄と加硫促進剤を除く各種配合材料をバンバリーミキサーで混練した後、２本ロールミルミキサーで硫黄と加硫促進剤を混練し、厚さ１．５ｍｍのシートに延伸した。１．５ｍｍのシートに延伸したサンプルを１７０℃で１２分間、プレス加硫して試験片の切り出し用シートを得た。
(Production of rubber material)
Various compounding materials excluding sulfur and vulcanization accelerator shown below were kneaded with a Banbury mixer, and then sulfur and vulcanization accelerator were kneaded with a two-roll mill mixer and stretched to a sheet having a thickness of 1.5 mm. The sample stretched to a 1.5 mm sheet was press vulcanized at 170 ° C. for 12 minutes to obtain a test piece cutting sheet.
（配合材料）
ＳＢＲ：ジェイエスアール（株）製のＳＢＲ１５０２（スチレン単位量：２３．５重量％） １００質量部
カーボンブラック：三菱化学（株）製のダイヤブラックＩ（Ｎ２２０）
４７．８７質量部
ステアリン酸：日油（株）製の椿 ２質量部
酸化亜鉛：三井金属鉱業（株）製の酸化亜鉛２種 ３質量部
老化防止剤：フレキシス社製のサントフレックス１３ １質量部
パラフィンワックス：日本精鑞（株）製のオゾエース０３５５ １質量部
硫黄：軽井沢硫黄（株）製の粉末硫黄 １．６質量部
加硫促進剤：大内新興化学工業（株）製のノクセラーＣＺ １質量部
(Blend material)
SBR: JBR Co., Ltd. SBR1502 (styrene unit amount: 23.5 wt%) 100 parts carbon black: Mitsubishi Chemical Co., Ltd. Diamond Black I (N220)
47.87 parts by mass Stearic acid: Koji made by NOF Corporation 2 parts by mass Zinc oxide: 2 types of zinc oxide made by Mitsui Mining & Smelting Co., Ltd. 3 parts by mass Anti-aging agent: Santoflex 13 made by Flexis Co. 1 mass Part paraffin wax: Ozoace 0355 manufactured by Nippon Seiki Co., Ltd. 1 part by mass Sulfur: Powdered sulfur manufactured by Karuizawa Sulfur Co., Ltd. 1.6 parts by mass Vulcanization accelerator: Noxeller CZ manufactured by Ouchi Shinsei Chemical Co., Ltd. 1 part by mass
得られたシートから、図２の（ａ）の態様で伸長方向に切り出した試験片を比較例の試験片として使用し、（ｂ）の態様で伸長方向に４５°傾けて切り出した試験片を実施例の試験片として使用した。得られた試験片を用い、二軸伸長試験機（アイエス技研株式会社製）を用いて、２３℃で伸張速度５００ｍｍ／分でサンプルの異方性を測定した。用いた試験のモードは等二軸伸長である。ここで、等二軸伸長は正方形のサンプルシートをｘ方向とｙ方向に同じ伸長速度で伸長する試験であって、ｘ方向とｙ方向の応力をそれぞれ測定し、２種類の応力を検出する。ひずみに対して応力をプロットしたものを図３に示す。 From the obtained sheet, the test piece cut out in the extending direction in the mode of (a) of FIG. 2 was used as a test piece of the comparative example, and the test piece cut out by being inclined by 45 ° in the extending direction in the mode of (b) was used. It used as a test piece of an Example. Using the obtained test piece, the anisotropy of the sample was measured at 23 ° C. and an extension rate of 500 mm / min using a biaxial extension tester (manufactured by IS Giken Co., Ltd.). The test mode used is equibiaxial stretching. Here, equibiaxial stretching is a test in which a square sample sheet is stretched in the x and y directions at the same stretching speed, and stresses in the x and y directions are measured to detect two types of stress. FIG. 3 shows a plot of stress against strain.
伸長方向に切り出した比較例のサンプルでは、ｘ方向とｙ方向で応力の値が大きく異なっていた。よって、ｘ方向とｙ方向の応力が異なり、異方性があることがわかる。 In the sample of the comparative example cut out in the extending direction, the stress values were greatly different in the x direction and the y direction. Therefore, it can be seen that the stresses in the x and y directions are different and there is anisotropy.
一方、伸長方向に対して４５°傾けて切り出した実施例の等方サンプルでは、ｘ方向とｙ方向で同じ応力の値を示した。よって、異方性がなくなったことを示す。 On the other hand, the isotropic sample of the example cut out by being inclined by 45 ° with respect to the extending direction showed the same stress value in the x direction and the y direction. Thus, the anisotropy is lost.
１ シート
２ 試験片の切り出し範囲
1
Claims (2)
The elongation test method according to claim 1, wherein the thickness of the test piece is 0.5 to 3 mm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5172487A (en) * | 1974-12-20 | 1976-06-23 | Bridgestone Tire Co Ltd | OBIJOBUTSUNOSANPURINGUSOCHI |
| JPH11211634A (en) * | 1998-01-22 | 1999-08-06 | Zeon Kasei Co Ltd | Plastic test piece punching device |
| WO2009139237A1 (en) * | 2008-05-12 | 2009-11-19 | 学校法人関西大学 | Piezoelectric element and audio equipment |
-
2012
- 2012-12-27 JP JP2012285657A patent/JP5973345B2/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5172487A (en) * | 1974-12-20 | 1976-06-23 | Bridgestone Tire Co Ltd | OBIJOBUTSUNOSANPURINGUSOCHI |
| JPH11211634A (en) * | 1998-01-22 | 1999-08-06 | Zeon Kasei Co Ltd | Plastic test piece punching device |
| WO2009139237A1 (en) * | 2008-05-12 | 2009-11-19 | 学校法人関西大学 | Piezoelectric element and audio equipment |
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