(19)
(11)EP 2 905 602 B1

(12)EUROPEAN PATENT SPECIFICATION

(45)Mention of the grant of the patent:
22.05.2019 Bulletin 2019/21

(21)Application number: 15153892.3

(22)Date of filing:  05.02.2015
(51)International Patent Classification (IPC): 
G01N 19/04(2006.01)

(54)

Method for determining the tack of a material

Verfahren zur Bestimmung der Klebrigkeit eines Materials

Procédé permettant de déterminer l'adhérence d'un matériau


(84)Designated Contracting States:
AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

(30)Priority: 07.02.2014 IT TO20140101

(43)Date of publication of application:
12.08.2015 Bulletin 2015/33

(73)Proprietor: LEONARDO S.P.A.
00195 Roma (IT)

(72)Inventor:
  • Corvaglia, Stefano Giuseppe
    73100 Lecce (IT)

(74)Representative: Vanzini, Christian et al
Jacobacci & Partners S.p.A. Corso Emilia 8
10152 Torino
10152 Torino (IT)


(56)References cited: : 
WO-A1-2012/157686
JP-A- S56 111 439
FR-A- 1 580 947
US-A- 3 303 697
  
  • ROTHMAN L B: "PROPERTIES OF THIN POLYIMIDE FILMS", JOURNAL OF THE ELECTROCHEMICAL SOCIETY, ELECTROCHEMICAL SOCIETY, vol. 127, no. 10, 1 October 1980 (1980-10-01), pages 2216-2220, XP000839961, ISSN: 0013-4651
  
Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention).


Description


[0001] This invention relates in general to methods for determining the tack of materials, in particular composite materials of the type comprising a resin matrix reinforced with fibre material.

[0002] Methods for determining the tack of adhesives are known. In these materials the forces responsible for tack are in general various orders of magnitude larger than the composite materials in question. In addition to this, the phenomena underlying attachment of the materials are significantly different. It is therefore felt that the tests developed for adhesives are unsuitable for determining the tack of composite materials.

[0003] On the other hand, in the industrial environment there is a need to develop a method of test which can be used to evaluate and compare materials used for the forming of components or for application to a mould or mandrel for the manufacture of particular pieces.

[0004] US 3 303 697 A discloses a method for determining the tack of a material placed in contact with a surface is therefore provided and comprises the following stages:
  • providing a sample of the said material, the sample comprising a sheet with a first end and a second end;
  • applying the sample to the an upward facing supporting surface of a plate;
  • compacting the sample against the surface of the supporting plate;
  • attaching a weight to the first end of the sample;
  • turning the plate over in such a way that the supporting surface faces downwards; and
  • measuring detachment of the sample from the supporting surface from the first end of the sample in terms of distance detached as a function of time.


[0005] According to the present invention, a method of the above mentioned type is provided for determining the tack of a material, wherein the width of the sheet increases from a narrow first end of the sample to a wide second end of the sample.

[0006] Although the process according to the invention has been envisaged in relation to determination of the tack of composite materials, it may also find application for other materials which exhibit tack.

[0007] Particular embodiments of the invention form the subject matter of the dependent claims, whose content is to be understood to constitute an integral part of this description.

[0008] Further features and advantages of the invention will be described in greater detail in the following detailed description of an embodiment provided by way of a non-limiting example with reference to the appended drawings in which:
  • Figure 1 is a plan view of an example of a sample used in the method according to the invention;
  • Figure 2 is a plan view of a plate supporting the sample in Figure 1; and
  • Figures 3 to 6 are diagrammatical views showing different operating stages in the method according to this invention.


[0009] With reference to Figure 1, this shows a sample 10 for use in a process for determining tack according to the invention. This sample 10 comprises a sheet having a width w which increases from a first narrow end 10a to a second wide end 10b. In particular sample 10 has a longitudinal section 10c having a width w that increases linearly towards second end 10b of the sample. Sample 10 also has a tab portion 10d at its first end 10a, the function of which will be clarified below.

[0010] Sample 10 is made of a material whose tack with regard to the surface of another material is to be tested. This tack may be the intrinsic tack of the material or the tack imparted to the material by the interposition of an adhesive agent or tackifier between the material under test and the surface (or other material where it is desired to test tack between two similar or different materials; in this case the substrate material will be anchored to the plate by two-sided adhesive tape applied over the entire surface area).

[0011] In particular, sample 10 may be made of a composite material comprising a resin matrix reinforced with fibre material.

[0012] Sample 10 may be obtained by cutting the material under test into the desired shape, for example using masks.

[0013] With reference to Figure 2, this shows a plate 20 for use in the method according to the invention.

[0014] Plate 20 comprises a supporting surface 21 to which it is intended that sample 10 should be applied. This plate may for example be of metal material, such as aluminium. A mask 23 of non-adhering material delimiting an area of application 25 suitable for receiving sample 10 is preferably located on supporting surface 21 of plate 20. As will be seen, the shape of application area 25 approximately matches the shape of sample 10. In addition to this, a graduated scale 27 for measuring length, arranged parallel to the longitudinal direction of application area 25, which when in use corresponds to the longitudinal direction of sample 10, is located on supporting surface 21 of plate 20.

[0015] Preferably, plate 20 is attached to a base 30 by means of a hinge 29, as may be seen in Figure 3. Through this arrangement, plate 20 may rotate with respect to base 30 about an axis of rotation y located perpendicularly to the longitudinal direction of area 25 to which sample 10 is applied. Plate 20 can therefore rotate between a starting position (shown in Figures 3 and 4) in which supporting surface 21 faces upwards, and an overturned position (shown in Figures 5 and 6) in which supporting surface 21 faces downwards.

[0016] An embodiment of a method for determining tack according to the invention will now be described with references to Figures 3 to 6.

[0017] Initially, plate 20 is in the starting position on base 30. Supporting surface 21 may be first cleaned with specific solvents to remove any substances which might have an adverse effect on the measurements. Plate 20 may also be placed in a climatised chamber (not illustrated) to condition the plate to a particular temperature and relative humidity, depending upon the specific conditions which it is desired to test. Sheet 10 of the material under test, which has not yet been applied to plate 20, is also placed within the climatised chamber.

[0018] Subsequently, an adhesive agent or tackifier may or may not be applied to previously conditioned plate 20 in the area of application 25 (or another material may be placed in between if it is desired to test tack between two similar or different materials; in this case the substrate material will be anchored to the plate with two-sided adhesive tape applied over the entire surface area).

[0019] When the tackifier has been applied, plate 20 may undergo a second conditioning in the climatised chamber, again together with sample 10, for the necessary time determined by means of individual tests ("tackifier flash time").

[0020] Sample 10 will then be applied to supporting surface 21 of plate 20, as illustrated in Figure 3, in application area 25 which may have been treated with tackifier.

[0021] As illustrated in Figure 4, a vacuum bag 40 is then fitted over sample 10 and sample 10 is compacted against supporting surface 21 of plate 20 under vacuum. The vacuum pressure applied and the vacuum application time will depend on the test conditions. In accordance with alternative embodiments (not illustrated) compaction may be performed by means of a roller, or manually, according to the conditions which it is desired to simulate.

[0022] Once the vacuum bag has been removed, plate 20, together with applied and compacted sample 10, is again subjected to conditioning in a climatised chamber at a controlled temperature and humidity for a desired length of time.

[0023] A weight 50 (shown in Figures 5 and 6) is then attached to first end 10a of the sample, more specifically to tab portion 10d. This may be done, for example, by applying a clip or spring to which weight 50 is attached to the tab portion 10d. In order to allow the clip to be attached to tab portion 10d the latter must be dimensioned to have a length which partly overlaps mask 23. This prevents the portion of tab 10d from adhering completely to supporting surface 21 during compaction under vacuum, thus leaving a free portion which will allow the clip with weight 50 to be inserted. The area of overlap between mask 23 and tab portion 10d is shown by a dashed line in Figure 2 and is designated by reference 23a.

[0024] As illustrated in Figure 5, plate 20 is then turned upside down by causing it to rotate about hinge 29.

[0025] As a result of the effect of plate 50 attached to first end 10a, sheet 10 becomes progressively detached from supporting surface 21 of plate 20, starting from first end 10a (Figure 6). Thanks to graduated scale 27 located on supporting surface 21 the distance d through which sheet 10 becomes detached at a particular time following the application of weight 50 can be measured.

[0026] By reading off detachment distance d at intervals of time defined according to the circumstances it is possible to draw a graph of the increase in detachment distance d of sheet 10 as a function of time.

[0027] By making measurements on the same material, but varying different parameters such as tackifier flash time, temperature, relative humidity, aging of the material and application time of the vacuum, it is possible to draw graphs to evaluate the correlation between these parameters and tack.

[0028] One method of assessing tack is to consider the graphs obtained for detachment distance d as a function of time, by determining the area subtended by each curve starting from a particular time after application of the weight (for example 30 seconds after application of the weight) in order to rule out any initial errors due to the different speeds at which the weight is allowed to fall, up to a maximum predetermined time (for example 10 minutes). Bearing in mind that this subtended area is proportional to the detachment of sheet 10 from plate 20, tack can be considered to be directly proportional to the reciprocal of the calculated area.

[0029] By then drawing the graph of the reciprocal of the area as a function of a variable parameter (for example temperature or another of the parameters indicated above) it is possible to observe the change in tack as a given characteristic varies.


Claims

1. A method for assessing tack of a material contacting a surface, comprising the following steps:

- providing a sample (10) of said material, the sample consisting of a sheet with a first end (10a) and a second end (10b);

- laying the sample (10) on a support surface (21) of a plate (20) facing upwards;

- compacting the sample (10) against the support surface (21) of the plate (20);

- attaching a weight (50) to the first end (10a) of the sample (10);

- reversing the plate (20) to cause the support surface (21) to face downwards; and

- measuring detachment of the sample (10) from the support surface (21), in terms of detachment distance (d) from the first end (10a) of the sample (10), as a function of time,

said method being characterized in that the width (w) of the sheet increases from a narrow first end (10a) of the sample to a wide second end (10b) of the sample.
 
2. A method according to claim 1, wherein the sample (10) comprises a longitudinal section (10c) whose width (w) linearly increases from the first end (10a) toward the second end (10b) of the sample (10).
 
3. A method according to claim 1 or 2, wherein the sample (10) comprises a tab portion (10d) at its first end (10a) which is provided for attachment of the weight (50).
 
4. A method according to any of the preceding claims, wherein a mask (23) of adhesion-preventing material is disposed on the support surface (21) of the plate (20), said mask limiting a laying area (25) for receiving the sample (10).
 
5. A method according to any of the preceding claims, wherein a graduated scale (27) is disposed on the support surface (21) of the plate (20), said scale being provided for measuring detachment of the sample (10) from the support surface (21).
 
6. A method according to any of the preceding claims, wherein the plate (20) is hinged to a base (30), said plate being rotatable between a start position wherein the support surface (21) is facing upwards, and a reversed position wherein the support surface (21) is facing downwards.
 
7. A method according to any of the preceding claims, wherein said material is a composite material comprising a resin matrix reinforced with fibre material.
 
8. A method according to any of the preceding claims, wherein before laying the sample (10) on the support surface (21) of the plate (20) the sample (10) and the plate (20) are subjected to conditioning at predetermined humidity and temperature.
 
9. A method according to any of the preceding claims, wherein after compacting the sample (10) and the plate (20) are subjected to conditioning at predetermined humidity and temperature.
 


Ansprüche

1. Verfahren zum Beurteilen einer Klebrigkeit eines Materials, das eine Oberfläche berührt, mit den nachfolgenden Schritten:

- Bereitstellen einer Probe (10) des Materials, wobei die Probe aus einem Bogen mit einem ersten Ende (10a) und einem zweiten Ende (10b) besteht;

- Legen der Probe (10) auf eine Auflagefläche (21) einer Platte (20), die nach oben gerichtet ist;

- Pressen der Probe (10) gegen die Auflagefläche (21) der Platte (20);

- Anbringen eines Gewichts (50) an dem ersten Ende (10a) der Probe (10);

- Umdrehen der Platte (20) zum Bewirken, dass die Auflagefläche (21) nach unten gerichtet ist; und

- Messen eines Ablösens der Probe (10) von der Auflagefläche (21) in Form einer Ablösedistanz (d) von dem ersten Ende (10a) der Probe (10) als eine Funktion der Zeit,

wobei das Verfahren dadurch gekennzeichnet ist, dass die Breite (w) des Bogens sich von einem engen ersten Ende (10a) der Probe zu einem weiten zweiten Ende (10b) der Probe vergrößert.
 
2. Verfahren nach Anspruch 1, bei dem die Probe (10) einen Längsabschnitt (10c) aufweist, dessen Breite (w) sich linear von dem ersten Ende (10a) in Richtung zu dem zweiten Ende (10b) der Probe (10) vergrößert.
 
3. Verfahren nach Anspruch 1 oder 2, bei dem die Probe (10) einen Streifenbereich (10d) an ihrem ersten Ende (10a) aufweist, der zur Befestigung des Gewichts (50) vorgesehen ist.
 
4. Verfahren nach einem der vorhergehenden Ansprüche, bei dem eine Maske (23) aus einem anhaftungsverhindernden Materials auf der Auflagefläche (21) der Platte (20) angeordnet ist, wobei die Maske ein Auflagegebiet (25) zum Aufnehmen der Probe (10) einschränkt.
 
5. Verfahren nach einem der vorhergehenden Ansprüche, bei dem eine Stufenskala (27) auf der Auflagefläche (21) der Platte (20) angeordnet ist, wobei die Skala zum Messen einer Ablösung der Probe (10) von der Auflagefläche (21) vorgesehen ist.
 
6. Verfahren nach einem der vorhergehenden Ansprüche, bei dem die Platte (20) an einer Basis (30) drehbar angebracht ist, wobei die Platte drehbar ist zwischen einer Startposition, bei der die Auflagefläche (21) nach oben gerichtet ist, und einer Wendeposition, bei der die Auflagefläche (21) nach unten gerichtet ist.
 
7. Verfahren nach einem der vorhergehenden Ansprüche, bei dem das Material ein Verbundmaterial ist, das eine Harzmatrix aufweist, die mit einem Fasermaterial verstärkt ist.
 
8. Verfahren nach einem der vorhergehenden Ansprüche, bei dem vor dem Legen der Probe (10) auf die Auflagefläche (21) der Platte (20), die Probe (10) und die Platte (20) einer Behandlung bei einer vorgegebenen Feuchtigkeit und Temperatur unterzogen werden.
 
9. Verfahren nach einem der vorhergehenden Ansprüche, bei dem nach dem Pressen die Probe (10) und die Platte (20) einer Behandlung bei einer vorgegebenen Feuchtigkeit und Temperatur unterzogen werden.
 


Revendications

1. Procédé permettant de déterminer l'adhérence d'un matériau en contact avec une surface, comprenant les étapes suivantes :

- fournir un échantillon (10) dudit matériau, l'échantillon consistant en une feuille avec une première extrémité (10a) et une seconde extrémité (10b) ;

- poser l'échantillon (10) sur une surface de support (21) d'une plaque (20) tournée vers le haut ;

- compacter l'échantillon (10) contre la surface de support (21) de la plaque (20) ;

- fixer un poids (50) à la première extrémité (10a) de l'échantillon (10) ;

- renverser la plaque (20) de façon à faire en sorte que la surface de support (21) soit tournée vers le bas ; et

- mesurer le détachement de l'échantillon (10) de la surface de support (21), en termes de distance de détachement (d) depuis la première extrémité (10a) de l'échantillon (10), en fonction du temps,

ledit procédé étant caractérisé en ce que la largeur (w) de la feuille augmente depuis une première extrémité étroite (10a) de l'échantillon jusqu'à une seconde extrémité large (10b) de l'échantillon.
 
2. Procédé selon la revendication 1, dans lequel l'échantillon (10) comprend une section longitudinale (10c) dont la largeur (w) augmente de manière linéaire depuis la première extrémité (10a) vers la seconde extrémité (10b) de l'échantillon (10).
 
3. Procédé selon la revendication 1 ou 2, dans lequel l'échantillon (10) comprend une partie de patte (10d) au niveau de sa première extrémité (10a) qui est fournie pour la fixation du poids (50).
 
4. Procédé selon l'une quelconque des revendications précédentes, dans lequel un masque (23) de matériau anti-adhérence est disposé sur la surface de support (21) de la plaque (20), ledit masque limitant une zone de pose (25) pour recevoir l'échantillon (10).
 
5. Procédé selon l'une quelconque des revendications précédentes, dans lequel une échelle graduée (27) est disposée sur la surface de support (21) de la plaque (20), ladite échelle étant fournie pour mesurer le détachement de l'échantillon (10) de la surface de support (21).
 
6. Procédé selon l'une quelconque des revendications précédentes, dans lequel la plaque (20) est articulée par rapport à une base (30), ladite plaque pouvant tourner entre une position de départ dans laquelle la surface de support (21) est tournée vers le haut, et une position renversée dans laquelle la surface de support (21) est tournée vers le bas.
 
7. Procédé selon l'une quelconque des revendications précédentes, dans lequel ledit matériau est un matériau composite comprenant une matrice en résine renforcée par un matériau fibreux.
 
8. Procédé selon l'une quelconque des revendications précédentes, dans lequel, avant la pose de l'échantillon (10) sur la surface de support (21) de la plaque (20), l'échantillon (10) et la plaque (20) font l'objet d'un conditionnement à une humidité et une température prédéterminées.
 
9. Procédé selon l'une quelconque des revendications précédentes, dans lequel, après le compactage, l'échantillon (10) et la plaque (20) font l'objet d'un conditionnement à une humidité et une température prédéterminées.
 




Drawing











Cited references

REFERENCES CITED IN THE DESCRIPTION



This list of references cited by the applicant is for the reader's convenience only. It does not form part of the European patent document. Even though great care has been taken in compiling the references, errors or omissions cannot be excluded and the EPO disclaims all liability in this regard.

Patent documents cited in the description