Methods for Testing the Strength of Layers

for Different Optical Coatings

Ciprian Ion Rizescu, Ionela Ghita, and Dana Rizescu(B)

University POLITEHNICA of Bucharest, Splaiul Independentei 313, Bucharest, Romania

[email protected]

Abstract. The first part of the paper presents the test techniques and the equip-
ment used to make them, as well as the morphological characteristics of the tested
parts and the properties of the materials that compose them. Also, there are pre-
sented briefly the results obtained after testing the resistance of several types of
optical coatings are presented. The full description of the testing operations and
acquiring experimental results will be described in a future paper. The authors
used techniques found in the literature, but also standardized ones, comparing
the mechanical behavior of frequently used materials (for example: MgF2 , TiO2 ,
Ta2 O5 and SiO2 ), deposited on a glass substrate (BK7). The tested parts are flat sur-
faces, with a diameter of 25 mm, covered with anti-reflective layers for the visible
range. In this paper, various methods for testing the strength of thin films for three
types of optical coatings have been studied and developed. The three types of coat-
ings tested had the following morphological characteristics: AR (anti-reflective)
single layer, AR 4 layers and AR 6 layers. From the results obtained from the
tests, it was concluded that the strength of the optical coatings differs depending
on the test to which the sample is subjected. The most resistant types of optical
abrasion coatings were single-layer coating and four-layer coating, followed by
6-layer coating.

Keywords: Optical coatings · Anti-glare coatings · Layers strength

1 Introduction

Optical coatings are used for optical, microelectronic, biomedical, and decorative appli-
cations to improve elements on tribology (reduced friction), mechanics (wear / abrasion
resistance), chemical composition (barrier to aggressive gases), optical, magnetic, and
electrical properties [1].
With the development of optical technologies and for more comfort in wearing
glasses, layered lenses have become increasingly popular. Considering the variety of
these layers, we can say that they have a common feature, namely their role to replace
the deficiencies of the basic lens. Deficiencies can be the following: the gloss of glass
lenses, scratches on plastic lenses, shine and the fact that they get dirty more easily.
Anti-glare coatings are used in a wide variety of applications where light passes
through an optical surface and low reflection is desired. Examples include coatings on

© The Author(s), under exclusive license to Springer Nature Switzerland AG 2022

D. D. Cioboatǎ (Ed.): ICoRSE 2021, LNNS 305, pp. 119–128, 2022.
https://doi.org/10.1007/978-3-030-83368-8_12
120 C. I. Rizescu et al.

spectacle lenses, but also on camera lenses / cameras, as well as anti-glare coatings on
solar cells.
The simplest form of anti-glare coating was discovered by Lord Rayleigh in 1886.
The optical glass available at the time tended to develop a stain on its surface over the
years due to chemical reactions with the environment. Rayleigh tested some old, slightly
stained pieces of glass and found to his surprise that they emitted more light than the
new, clean pieces. The stains replace the air-glass interface with two interfaces: a scratch
interface and a glass interface. Because the stain formed on the glass has a refractive
index between the two glass and air interfaces, each of these interfaces has a lower degree
of reflection than the air-glass interface. In fact, the total of the two reflections is smaller
than that of the air-glass interface, as can be calculated from the Fresnel equations [2].
The simplest optical coatings are thin metal layers, such as aluminum, which is
deposited on glass supports to make mirror surfaces Fig. 1. The metal used determines
the reflection characteristics of the mirror; Aluminum is the cheapest and most common
coating and provides a reflection of about 88%–92% of the visible spectrum. More
expensive is silver, which has a reflection of 95%–99% even in far infrared but suffers
from decreased reflection (<90%) in the blue and ultraviolet spectral regions. The most
expensive is gold, which offers excellent reflection (98%–99%) on the entire infrared
surface, but at shorter wavelengths (550 nm) it is limited, resulting in the typical color
of gold (see Fig. 1) [3, 4].

Fig. 1. Spectral reflection curves for metal mirrors of aluminum (Al), silver (Ag) and gold (Au)
at normal incidence.

Another type of optical coating is dielectric coating (i.e. the use of materials with
a different refractive index than the substrate). Dielectric coatings are constructed of
thin layers of materials such as: magnesium fluoride, calcium fluoride and various metal
 Methods for Testing the Strength of Layers for Different Optical Coatings 121

oxides (i.e. tantalum pentoxide -Ta2 O5 or aluminum oxide Al2 O3 ), which are deposited
on the optical substrate. By carefully choosing the exact composition, thickness, and
number of these layers, it is possible to adapt the reflectance and transmission factors of
the optical coatings to produce almost any desired feature. Surface reflectance factors
can be reduced to less than 0.1%, producing an anti-glare coating (AR). In contrast,
the reflection can be increased to more than 99.99%, producing a high reflection (HR)
coverage [5].
Unlike UV protection, AR coating, also known as anti-glare coating, is not always
something that is stressed about when purchasing glasses. One of the problems with
prescription glasses and sunglasses, it is called back-glare. Back-glare is the light that
hits the back of the lenses and bounces right into your eyes. This can actually impair
visibility, especially at night when driving, when the headlights of cars appear to have
a halo around them. It can also produce a front glare, which is the light reflecting off
the front of our glasses. AR coating is a very thin film that is layered on the lens. If you
have polarized lenses, the AR coating is layered on the back of the lenses because the
polarized film is layered on top. Otherwise, the AR coating is usually placed on the top
and bottom. The AR film is made from multiple layers of metal oxides. These metal
oxides have an index refraction that is greater than air but less than glass. An index of
refraction is the measure of the bending of a ray of light when passing from one medium
into another. This is important because the degree of the bend of the light entering and
then exiting the surface of each film layer cancel each other out. By canceling each other
out, they eliminate the glare.

2 Methods for Testing the Strength of Different Optical Coatings

Layers
These tests are described in detail in the international standard for testing optical coatings
(ISO / FDIS 9211–4: 2014) and in the international standard for testing anti-glare coatings
deposited on finished, unobstructed spectacle lenses (SR EN ISO 8980–4: 2013) [6].

2.1 Measurement of the Reflection Coefficient

The reflection coefficient shall be determined with a double-beam spectrophotometer and
with sufficient measurement accuracy to provide the value of the reflection coefficient
at all wavelengths, between 380 nm and 780 nm with an uncertainty of less than 0.1%
(of for example, an anti-glare coating rated as having a reflectance of 0.5% can be
measured as having a reflectance of 0.4% to 0.6%). The increase in the wavelength
of the measurement shall not exceed 5 nm. The spectral bandwidth (full half-width,
FWHM) must not exceed 5 nm. [11].
The optical and photometric measurement laboratory is equipped with a spectropho-
tometer, Lambda 35 UV / VIZ produced by Perkin Elmer (see Fig. 2). Here, Fig. 2, shows
the block diagram of the Lambda 35 spectrophotometer. The essential parts are: the sta-
bilized sources by electromagnetic radiation, the monochromator (which separates the
radiation according to the wavelength), transparent cells (containing the analysis sample
and the reference sample), detector and the evaluation system (the software used with
122 C. I. Rizescu et al.

which the spectra can be recorded. [12]. The measurements regarding the reflection of the
tested samples were performed with it. Also, in Fig. 3 is presented the spectrophotometer
Lambda 35.

Fig. 2. LAMBDA 35 UV / VIS spectrophotometer block diagram [12] automatically.

Fig. 3. LAMBDA 35 UV / VIS spectrophotometer.

2.2 Abrasion Resistance Tests

The purpose of these tests is to assess the extent to which the optical and mechanical
properties of optical coatings are affected when subjected to specific abrasion conditions
in ambient atmospheric conditions. The test device must operate in a cyclic manner. A
cycle is defined as a stroke in one direction, followed by a reverse stroke. The head of
the test device must be approximately normal on the tested surface during the friction
operation. The tested samples must be firmly gripped so that they do not slip during the
test [7].
 Methods for Testing the Strength of Layers for Different Optical Coatings 123

• Moderate abrasion test

The friction head of the abrasion tester shall be covered with a cotton gauze in accor-
dance with ISO 9211–4, approximately 5 mm thick and 10 mm wide. Instructions for
preparing the gauze, lid and gauze device were considered according to standards.
• Severe abrasion test
A standard eraser shall be applied to the friction head of the abrasion tester in accor-
dance with standard. The eraser is inserted into the support so that the exposed length
does not exceed 3 mm. It is permissible for the eraser to be cleaned with a clean towel,
but no solvents should be used. The eraser can also be cleaned by rubbing it on a
clean, smooth or frozen glass surface to remove some of the rubber if foreign material
is suspected Table 1.

Table 1. The degrees of severity.

The degrees of severity 01 02 03 04

Material Gauze Gauze Eraser eraser
Stroke numbers 50 100 20 40
Force 5 ± 1 N 5 ± 1 N 10 ± 1N 10 ± 1N

• Assessment
The film on the sample must be visually examined in reflected and / or transmitted
light for physical deterioration of the coating. The examination is performed using the
method specified in the international standard ISO 8980–4. The coating must not show
any evidence of damage, such as abrasion or removal of the coating. If a slight scratch
is visible and the gauze or eraser is suspected of having foreign material embedded
in it, another area of the surface will be tested with a new gauze or eraser.
Visual examination of the optical coatings shall be performed using an adjustable light
source to set the ambient light in the inspection room to 200 lx. The inspection source
must be at least 400 lm, for example a 15 W fluorescent tube or a 40 W incandescent
lamp. The covered surface must be viewed on a matte black background. The only
lighting in the inspection area is from the light source used for the examination. This
method of examination is shown in Fig. 4.
• Materials for abrasion testing of optical coatings - Gauze
• Typhoon threads
The threads must be made of cotton, without waste and loading materials, without
lint, pulled and spun into simple threads.
Structure of the threads. The fabric structure will have 41 threads up to 47 threads
on 25 mm, and the filling will have 33 threads up to 39 threads on 25 mm. The total
number of threads in a 25 mm by 25 mm square will be 76 to 84. The mass will be
45 g / m2 to 54 g / m2 .
Types of gauze. The type of gauze must be bleached. Before use, it must be washed
to completely remove the sizing agent and then dried.
124 C. I. Rizescu et al.

Fig. 4. Recommended configuration for visual inspection [11].

• Eraser (rubber / pumice stone)

The screed must be a uniform mixture of rubber and abrasive, formed by an extrusion
process. It must be composed of at least 15% by mass of pumice. All abrasive materials
must be well ground so that they will pass 100% through a 45 µm sieve. Its composition
must not contain any ingredient that leaves a residue on the surface under test.
Eraser hardness. The eraser shall have an international rubber hardness degree (IRHD)
of 75 ± 5 on both ends, in accordance with ISO 48.
Accelerated aging. The eraser must show a hardness change of not more than 10 points
after being placed in an air oven for seven days at a temperature of 70° C ± 2° C.
Shape and sizes. The diameter of the eraser must be from 6.5 mm to 7 mm so that it
fits snugly and is held by friction in an abrasion tester, such as the one in Fig. 5. It
must be of sufficient length. to be securely attached to the abrasion tester with at least
3 mm exposed. The legend for Fig. 5 is: 1. friction tool, 2. tool holder, 3. pivot axis,
4. support for tested samples, 5. gauze / eraser.

2.3 Adhesion Tests

The purpose of these tests is to assess the extent to which the mechanical properties of
optical coatings on components and substrates are affected when subjected to specific
tensile or shear conditions under ambient atmospheric conditions [8].
 Methods for Testing the Strength of Layers for Different Optical Coatings 125

Fig. 5. Device for performing abrasion tests.

2.4 Scratch / Hatch Tests

The purpose of this test is to assess the extent to which the adhesion properties of
the optical coatings on components and substrate are affected after cutting the coating
(distorting the stress and influencing the adhesion) [9].

3 Experimental Tests

3.1 Performing Abrasion Resistance Tests

Both types of tests presented in the ISO / FDIS 9211–4 standard were performed: the
moderate abrasion test and the severe abrasion test with the help of a specialized equip-
ment [10]. Moderate abrasion tests were performed with gauze, applying a force of 5N,
performing 50 strokes (severity 01) and 100 strokes (severity 02). Severe abrasion tests
were performed with a standardized eraser, applying a force of 10 N, performing 20
strokes (severity 03) and 40 strokes (severity 04) Fig. 6.
126 C. I. Rizescu et al.

Fig. 6. a) Performing moderate abrasion tests with gauze, b) Performing severe abrasion tests
with eraser.

3.2 Performing Adhesion Tests

Adhesion tests were performed according to the steps presented in the standard (see
Fig. 7) Tests were performed for all degrees of severity, the adhesion time of the adhesive
tape being different depending on the degree of severity at which we perform the test:
≈ 2 s to 3 s (for severity 01), ≈ 1 s (for severity 02), <<1 (for severity 03).

Fig. 7. Adhesion test

 Methods for Testing the Strength of Layers for Different Optical Coatings 127

Examples of lenses that Fig. 8a and Fig. 8b pass and do not pass the visual inspection
test:
The photographs in can be used to help determine whether or not a sample passes
the test.

Fig. 8. (a) Example of a test that does not pass the abrasion resistance test

Fig. 8. (b) Example of a test that passes the abrasion resistance test

4 Conclusions

In this paper, various methods for testing the strength of thin films for three types of
optical coatings have been studied and developed. The three types of coatings tested had
the following morphological characteristics:
• AR single layer (substrate: BK7 glass, coating material: MgF2 , layer thickness:
133 nm);
128 C. I. Rizescu et al.

• AR 4 layers (substrate: BK7 glass, coating materials: Ta2 O5 = 22.7 nm, SiO2 =
24.4 nm, Ta2 O5 = 65.2 nm, SiO2 = 85.8 nm);
• AR 6 layers (substrate: BK7 glass, coating materials: TiO2 = 14.2 nm, SiO2 =
36.6 nm, TiO2 = 73.1 nm, SiO2 = 7 nm, TiO2 = 36.6 nm, MgF2 = 97.3 nm).
From the results obtained from the tests, it was concluded that the strength of the
optical coatings differs depending on the test to which the sample is subjected.
The most resistant types of optical abrasion coatings were single-layer coating and
four-layer coating, followed by 6-layer coating.
In the case of adhesion and solubility tests, it was observed that all three types of
coatings withstand these tests.
After performing the scratch tests, we can conclude that the single layer coating is
the most resistant, the multilayer ones can be scratched easily, and the scratches are
extremely visible.
Thus, three types of anti-glare coatings have been successfully tested using existing
methods in international standards for testing optical coatings.

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