# Recatest—A Technique for Qualitative and Quantitative Assessment of Deferment and Degraded PVD Coatings and CVD Layers in the Deformed Area in the Scratch Test

^{1}

^{2}

^{*}

## Abstract

**:**

_{s}), coating thickness (h

_{1}), flash height (h

_{oc}, h

_{os}), depth of intended material (h

_{d}), material depth under scratch (h

_{cp}), and material depth under coating (h

_{db}). The paper also includes a description of the Recalo test device designed by the authors, which is used to make a series of spherical abrasion traces on the scratch surface. Recalo is dedicated to the Recatest technique. The analysed material was the CrN/CrCN/HS6-5-2, AlCrN -Alcrona-Balinit/D2 coatings deposited on tool steels.

## 1. Introduction

## 2. Methods and Materials

#### 2.1. Spherical Microsections of PVD Coatings-Recalo

- thickness measurement of the coating and of the coating layers,
- evaluation of the coating and layer structure in metallographic examinations,
- microhardness examination on the developed coating cross section,
- distribution of chemical elements on the developed coating cross section,
- quality evaluation of mutual adhesion of the coating layers,
- quality evaluation of adhesion of the coating to the substrate,
- quantitative surface roughness measurement,
- preliminary evaluation of local friction wear,
- density of coating materials (defined abrasion cap geometry),
- point marking of surface with microabrasion, and
- formation of reactive environment diffusion channels to the coating and substrate zones.

- a new specialized optical system integrated with Recalo for using digital cameras,
- a bench (micro-vice) integrated with the x-y cross table for specimen positioning,
- a rotary body ensuring better access,
- an optical system precisely positioned in x–y or x–y–z axes,
- a microprocessor controller with a display of set and current operating parameters,
- a digital camera with a dedicated lens, magnifying software for analysing images, including spherical microsections.

- fastening the specimen in the micro-vice clamps with x-y positioning relative to the microscope and image recorder optical axis,
- surface visual inspection through the microscope or at the computer screen (optical system with a CCD camera)(Delta Optical, Mińsk Mazowiecki, Poland) and choosing the test location Figure 1,
- optical calibration of the image (sharpness, magnification) along with determination of the observation optical axis which changes during the test. The optical calibration involves the first, blind abrasion test with a ball of minimum depth outside the test area. The resultant micro-abrasion is a point at which the optical axis of the image recording system is trained,
- making of a spherical microsection of a determined diameter in the determined place requires that this place be located in the optical axis. To this purpose, the test place is moved in x–y positions along the optical axis.

_{b}—radius of the measured ball (µm), T—depth of the spherical microsection (µm), t—depth penetration in the base material, h

_{1}—vcoating thickness (µm), d, x, y, D measurement data defined on the spherical microsection (µm).

#### 2.2. Recatest Technique—Qualitative and Quantitative Analysis of the Revealed Structures of Coating Materials

- precise revealing of the microstructure of the deformed coating,
- a quantitative analysis of changes of the microstructure geometry parameters in the deformed coating under the bottom of the scratch,
- a graphical illustration of microstructure geometry changes within the scratch in correlation with scratch test parameters–critical forces Lc1, Lc2, Lc3,

#### 2.3. The Analysis of the Coating Structure on the Spherical Microsection within the Area of Scratches

- Deeper than the scratched bottom: type I.
- At the border of the scratching: type II.
- Less deep than the scratched bottom: type III.

- Case A represents a situation when a continuous uniform coating microstructure is maintained under the scratch bottom and on the scratch rim within the local deformation force Fn (N). The system quality is high. The basic quantitative parameter characterising this case is the maximum coating indentation depth under the scratch bottom h
_{cp}[µm] and the resulting depth of indented coating h_{d}(µm), - Case B shows a coating microstructure under the scratch bottom when the local deformation force Fn (N) is exceeded. The coating undergoes deformation in the form of cracking, chipping and delamination. The coating microstructure partially loses its continuity. The system quality is still satisfactory,
- Case C corresponds to the total coating removal from the plastic strain area when the local deformation force Fn (N) is exceeded. The microstructure observation on the spherical microsection does not indicate the presence of the coating material under the scratch bottom and on the scratch rim. The system quality is poor.

#### Recatest Analysis of Case A Coating Structures

_{s}determines the scratch bottom point, r

_{d}determines the distance to the coating end point under the scratch, r

_{oc}determines the radius of the outflow coating material, r

_{os}determines the radius of the outflow base material, r

_{1}determines the radius of the bowl boundary, and r

_{2}indicates the radius on the coating end boundary under the surface. Based on measurement data from Figure 14 and Figure 15 and mathematical relationships between geometrical points on the spherical surface, the following values can be determined: coating thickness, scratch bottom depth, and thickness of the coating underneath the scratch bottom. The geometrical relationships and exemplary calculations conducted on the basis of data from Figure 8 and Figure 9 are shown in Table 2 below.

_{1}—coating thickness, h

_{d}—scratch depth, h

_{oc}—flash height, h

_{db}—coating indentation depth, h

_{s}—scratch bottom depth, h

_{cp}—thickness coating pressing under the scratch bottom, h

_{os}—height of the outflow of the base material, R—ball radius; D—diameter of the spherical rubbed out area; x, y, d—measurement data (Table 1).

#### 2.4. Experimental Part

- Testing techniques used

^{®}coating (Oerlikon Balzers Coatings, Polkowice, Poland) the following tests: metallographic, scratch test, spherical metallographic section in the area of scratches (Recatest).

- Metallographic tests

- Scratch tests

^{®}Scratch (CSEM Instruments, Neuchatel, Switzerland) installation, with an increasing load force of 0–100N, 0–150 N and an indenter speed of 10 mm/min. The scratch was made using a Rockwell indenter of a 200 µm vertex radius.

- Recatest

_{d}= 0.2 N–0.7 N range.

#### 2.5. Tests of the CrAlN–Alcrona Balinit Coating

_{s}, h

_{oc}, h

_{os}. Being able to make several spherical microsections in the scratch area, it is possible to assess the change dynamics of the aforementioned parameters as a function of the indenter pressing force. The determined parameters included: scratch bottom depth, substrate and coating material flash height, substrate material flash height, depth T of coating visual inspection under the scratch bottom.

_{oc}, at which the Lc3-148 N coating fragmentation occurs is 6 µm, and the scratch depth is h

_{s}= 10 µm. The coating material fragments are pressed under the scratch bottom to the depth of T = h

_{d}= 11 µm.

_{2}steel have shown the high mechanical cohesion of the coating in the scratch area up to Fn = 148 N. The coating does not delaminate in the entire load range, and the coating material is pressed under the scratch bottom and subjected to fragmentation and flow along with the substrate. This phenomenon is observed to the depth of h

_{d}= 11 µm Figure 24 and Figure 25. The statistical measurement error in this method with microsections of diameter up to 2 mm does not exceed 10%.

## 3. Research Results and Discussion

#### Tests of the (CrN/CrCN)×16/ HS6-5-2 Coating

_{s}(Fn), system flash height h

_{oc}(Fn), coating indentation depth into the surface h

_{cp}(Fn). With the analysis of curves h

_{s}(Fn) and h

_{cp}(Fn) it is possible to determine the range of penetrator forces which define the microstructural durability of the tested areological system (Figure 19 and Figure 27). In the 16× CrCN/CrN coating system tested, the critical value for the destruction of the coating at the bottom of the crack is plastic deformation, force Fn 55 N. The coating loses its structural continuity under the bottom of the crack at a depth of 8 µm. The approximated scratch depth on the basis of the analysed geometric data at the force point F 55 N is 4 µm.

## 4. Conclusions

_{s}= 8 ± 0.5 µm, flash size h

_{oc}= 4 ± 0.5 µm and trace amounts of the coating material pressed into the coating down to the depth of h

_{d}= 11 µm. The CrN/CrCN undergoes destruction at Lc3 = 98 N, and the estimated material pressing depth is h

_{d}= 11 µm.

## Author Contributions

## Funding

## Institutional Review Board Statement

## Informed Consent Statement

## Data Availability Statement

## Conflicts of Interest

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**Figure 1.**Recalo; (

**a**)—a ball in a tribological node, (

**b**)—a scheme of the geometry of the spherical microsection with an indication of measurement parameters for determining thickness of the coating, (

**c**)—a image of multi-layer PVD CrN (Nikon), (

**d**)—an image of multi-layer PVD coating spherical microsections CrN/CrCN ×4 /HS6-5-2 (Nikon). All units appearing in drawings are measurement in (µm).

**Figure 2.**A new type of Recalo (

**a**)—an assembly drawing structure; 1—a optical head with sight, y-x axis sample; 2—a head with micro vice; 3—a ball drive roller; 4—a belt transmission; 5—a x-y axis electric motor, rotation speed 100 ÷ 350 n/min; 6—a angular head with movement lock, (

**b**)—a version dedicated to the Recatest research technology with precise location of the spherical microsection.

**Figure 3.**Recalo stand layout, friction node positioning (

**a**)—measurement head position at low friction node load; (

**b**)—measurement head position at high friction node load.

**Figure 4.**The structure of the multilayer coatings TiN/TiAlN/TiCN/ HS6-5-2 on the flat surface, (

**a**)—a polished surface, (

**b**)—a structure of the multilayer coatings TiN/TiAlN/ HS6-5-2 on the cylindrical cutter, (

**c**)—a precise spherical polished surface in the center axis of the Rockwell test, the coating adhesion (

**d**)—a multilayer coatings TiN/TiAlN/TiCN/ HS6-5-2 of the Rockwell test, the coating adhesion.

**Figure 5.**A scheme of the geometry of the spherical microsection with an indication of measurement parameters for determining thickness of the mono-coating, (

**a**)—a flat surface, (

**b**)—a convex cylindrical surface, (

**c**)—a concave cylindrical surface, (

**d**)—a spherical surface. A—major axis of the ellipse, B—minor axis of the ellipse, R—ball radius, D—diameter spherical cap of the coating and substrate, d—diameter spherical cap of the substrate, dimensions x and y the thickness of the coating h is calculated by h = xy/2R, h—thickness coatings, Db—diameter of the ball with the coating, Rb—radius of the ball before coating.

**Figure 6.**The structure of the multilayer coatings 4× (CrCN/CrN)/HS6-5-2 on the cylindrical cutter, (

**a**)—a deformed coating in the scratch area, cohesive chipping, (

**b**)—a deformed coating on the spherical microsection.

**Figure 7.**The structure of the multilayer coatings 32×(CrCN/CrN)/HS6-5-2 on the cylindrical cutter, (

**a**)—multilayer coatings 32×(CrCN/CrN), (

**b**)—a deformed coating in the scratch area, cohesive chipping, (

**c**,

**d**)—a cohesive chipping in the area of the upper layers of the coating.

**Figure 8.**The spherical microsection in area scratches, (

**a**)—a three tracks spherical micros section in area scratches, (

**b**)—a map of surface microgeometry changes (Keyence VR-5000).

**Figure 9.**Diagrams and a microstructure image (spherical microsection) of the coating areological system in the scratch area: (

**a**)—a spherical microsection diagram, (

**b**)—microstructure of the CrN coating revealed on the spherical microsection with a description (30 mm ball).

**Figure 10.**Diagrams and a microstructure image (perpendicular microsection ) of the coating areological system in the scratch area: (

**a**)—a spherical microsection diagram, (

**b**)—a microstructure of the TiN coating a perpendicular microsection diagram, letters are assigned to the measured structure: h

_{1}—coating thickness, h

_{d}—scratch depth, h

_{oc}—flash height, h

_{d}—coating indentation depth, h

_{s}—scratch bottom depth, h

_{cp}—thickness coating pressing under the scratch bottom, h

_{os}—height of the outflow of the base material, (

**c**)—a microstructure of the TiN coating a perpendicular microsection diagram, h

_{oc}—height of the outflow of the coating material parameter.

**Figure 11.**Diagrams and a microstructure image of the coating areological system in the scratch area: (

**a**)—a spherical microsection diagram the microstructure CrN type I, (

**b**)—a spherical microsection diagram the microstructure CrN type II, (

**c**)—a spherical microsection diagram the microstructure CrN type III.

**Figure 12.**Diagrams and a microstructure image of the coating areological system in the scratch area: (

**a**)—a spherical microsection diagram, (

**b**)—a microstructure of the CrN coating revealed on the spherical microsection with a description (30 mm ball).

**Figure 13.**This is a figure. Schemes follow the same formatting; (

**a**) a type A microstructure, the coating microstructure with structural continuity under the scratch bottom; (

**b**) a type B microstructure, the coating microstructure with partial loss of structural continuity under the scratch bottom; (

**c**) a type C microstructure, the coating microstructure with total loss of structural continuity under the scratch.

**Figure 14.**A surface structure in Recatest. Microstructure images; (

**a**)—a deformed coating in the scratch area, (

**b**)—a deformed coating on the spherical microsection.

**Figure 15.**The PVD coatings and A type traces of the scratch revealed on the surface of the spherical cut on steel; (

**a**)—a deformed coating without flashing on the edge of the crack, (

**b**)—a deformed coating with a flash on the edge of the crack, the outflow of the coating material, the base material. Explanation of the markings; rd—radius of the depth of pressing the deposited coating, rs—radius to the apex of the scratch bottom, r1—radius of the base of de cap, r2—radius of the lower limit of coating, ros—radius of the upper edge of the outflow substrate material, roc—radius of the upper edge of the outflow coating material.

**Figure 16.**Microstructure images; (

**a**)—a metallographic section transverse metallographic, (

**b**)—a spherical microsection, yellow arrows, coating thickness measuring radii r1, r2.

**Figure 17.**The scratch test, structure of the scratch bottom surface; (

**a**)—a load force range for 16–27 N, (

**b**)—a load force range for 39–50 N, (

**c**)—a load force range for 64–78 N, Fn = 64 N (Lc1).

**Figure 18.**The scratch test, structure of the scratch bottom surface (

**a**)—a load force range for 83–99 N Fn = 83 N (Lc2), (

**b**)—a load force range for 106–124 N, (

**c**)—a load force range for 129–148 N, Fn = 148 N (Lc3).

**Figure 19.**A surface structure in Recatest. Microstructure images; (

**a**)—a spherical microsection of the CrCN/CrN/HS6-5-2 coating for 40–46 N (Lc1), (

**b**)—a spherical microsection of the CrCN/CrN/HS6-5-2 coating for Fn = 61 N (Lc2).

**Figure 20.**A surface structure in Recatest, a microstructure images spherical microsection of the AlCrN- Balinit Arcrona in six areas of the scratch the spherical microsection, load force range for 1⟶16–27 N; 2⟶39–50 N; 3⟶64–78; 4⟶83–99; 5⟶106–124; 6⟶129–148; No 1–6—Spherical microsection number.

**Figure 21.**A surface structure in Recatest. Microstructure images spherical microsection of the AlCrN-Alcrona Balinit coating; (

**a**)—a load force range for 16–27 N, (

**b**)—a load force range for 39–50 N Fn = 50 N (Lc1), (

**c**)—a load force range for 64–78 N.

**Figure 22.**A surface structure in Recatest. Microstructure images spherical microsection of the AlCrN- Balinit Arcrona coating; (

**a**)—a load force range for 83–99 N (Lc2), (

**b**)—a load force range for 106–24 N, (

**c**)—a load force range for 129–148 N (Lc3).

**Figure 23.**A change of scratch depth, indentation depth and flash height in the scratch area on the AlCrN—Alcrona Balinit coating as a function: h

_{s}(Fn), h

_{oc}(Fn), h

_{os}(Fn) of a normal penetrator loading force Fn in the range from 0 to 150 N, and the structure of the deformed areological system, h

_{s}—scratch bottom depth, h

_{cp}—thickness coating pressing under the scratch bottom, h

_{os}—height of the outflow of the base material.

**Figure 24.**A surface structure in Recatest. Microstructure images; (

**a**)—a spherical microsection of the AlCrN-Alcrona Balinit coating for 39–50 N, (

**b**)—a spherical microsection of the AlCrN—Alcrona Balinit coating for 50–53 N, Fn = 50 N (Lc1).

**Figure 25.**A surface structure in Recatest. Microstructure images; (

**a**)—a spherical microsection of the AlCrN-Balinit Arcrona coating for 116–124 N, (

**b**)—a spherical microsection of the AlCrN-Balinit Arcrona coating for 140–150 N (Lc3).

**Figure 26.**Spherical microsections in the scratch area on the 16× CrCN/CrN coating. A scratch made with a 0–100 N rising load: (

**a**)—a spherical microsection of the 16× CrCN/CrN coating; (

**b**)—a diagram of the herical microsection location on the scratch area.

**Figure 27.**A change of scratch depth, indentation depth and flash height in the scratch area on the PVD coating as a function of a normal penetrator loading force Fn in the range from 0 to 150 N, and the structure of the deformed areological system, h

_{s}—scratch bottom depth, h

_{cp}—thickness coating pressing under the scratch bottom, h

_{os}—height of the outflow of the base material.

Geometry of Coated Surface | Coatings Thickness (µm) | Depth Penetration (µm) |
---|---|---|

Planar (Figure a)—The total penetration depth of the ball in the layer and into the substrate is: | - | $T=R-\sqrt{{R}^{2}-{r}_{1}^{2}}$ |

Planar (Figure a)—The depth penetration in the base material is: | - | $t=R-\sqrt{R-\frac{{d}^{2}}{4}}$ |

Planar (Figure a)—The thickness of the layer, coatings is: | ${h}_{1}=\frac{1}{2}\left(\sqrt{4{R}^{2}-{d}^{2}}-\sqrt{4{R}^{2}-{D}^{2}}\right)$ ${h}_{1}=\frac{x\ast y}{2R}$ | - |

Cylindrical convex (Figure b) The thickness of the layer is: | - | |

Cylindrical concave (Figure c) The thickness of the layer is | - | |

Conical (Figure b) The thickness of the layer is | - | |

Spherical (Figure d) The thickness of the layer is: | ${h}_{1}=\frac{x\times y}{2}\left(\frac{1}{{R}_{b}}+\frac{1}{R}\right)$ | - |

**Table 2.**Methods of parametrical measurement of the coating on the spherical cut. All units appearing in the patterns and drawings are measurement in (µm).

Trigonometric Relationship Measured Parameter | Diagram of the Deformed Areological System | Spherical Cut | |
---|---|---|---|

1 | Total penetration depth of the ball $T=R-\sqrt{{R}^{2}-{r}_{1}^{2}}$ | ||

2 | Coating thickness ${h}_{1}=\sqrt{{R}^{2}-{r}_{2}{}^{2}}-\sqrt{{R}^{2}-{r}_{1}{}^{2}}$ | ||

3 | Scratch bottom depth ${h}_{s}=\sqrt{{R}^{2}-{r}_{s}{}^{2}}-\sqrt{{R}^{2}-{r}_{1}{}^{2}}$ | ||

4 | The depth of pressing the coating as measured from the surface ${h}_{d}=\sqrt{{R}^{2}-{r}_{d}{}^{2}}-\sqrt{{R}^{2}-{r}_{1}{}^{2}}$ | ||

5 | The depth of the coating pressing in measured from the surface of the base material ${h}_{db}=\sqrt{{R}^{2}-{r}_{d}{}^{2}}-\sqrt{{R}^{2}-{r}_{2}{}^{2}}$ | ||

6 | Thickness of the coating pressing under the scratch bottom ${h}_{cp}=\sqrt{{R}^{2}-{r}_{d}{}^{2}}-\sqrt{{R}^{2}-{r}_{s}{}^{2}}$ | ||

7 | The height of the outflow of the coating material ${h}_{oc}=\sqrt{{R}^{2}-{r}_{1}{}^{2}}-\sqrt{{R}^{2}-{r}_{oc}{}^{2}}$ | ||

8 | The height of the outflow of the base material ${h}_{os}=\sqrt{{R}^{2}-{r}_{2}{}^{2}}-\sqrt{{R}^{2}-{r}_{os}{}^{2}}$ |

**Table 3.**Quantitative parameters T, h

_{s}, h

_{oc}, h

_{os}of the deformed coating structure geometry on spherical microsection obtained with the Racatest technique, Fn (N)-penetrator force range. Measurement of the scratch trace parameters on the left side (’) and right side (’’) of the spherical microsection.

Values | |||||||

Parametr | T (µm) | h_{s}’(µm) | h_{s}’’(µm) | h_{oc}’(µm) | h_{oc}’’(µm) | h_{os}’(µm) | h_{os}’’(µm) |

1 | 4.0 | −1.3 | −1.9 | - | - | - | - |

2 | 5.0 | −4.1 | −4.1 | 1.1 | 0.9 | 1.3 | 0.9 |

3 | 6.5 | −4.1 | −4.7 | 2.2 | 1.9 | 1.9 | 1.9 |

4 | 7.9 | −6.0 | −6.2 | 2.2 | 2.5 | 2.4 | 3.4 |

5 | 9.0 | −6.7 | −6.7 | 3.6 | 4.1 | 3.5 | 3.8 |

5 | 10.9 | −9.4 | −10 | 4.2 | - | 4.8 | - |

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**MDPI and ACS Style**

Domanowski, P.; Betiuk, M.
Recatest—A Technique for Qualitative and Quantitative Assessment of Deferment and Degraded PVD Coatings and CVD Layers in the Deformed Area in the Scratch Test. *Materials* **2021**, *14*, 2625.
https://doi.org/10.3390/ma14102625

**AMA Style**

Domanowski P, Betiuk M.
Recatest—A Technique for Qualitative and Quantitative Assessment of Deferment and Degraded PVD Coatings and CVD Layers in the Deformed Area in the Scratch Test. *Materials*. 2021; 14(10):2625.
https://doi.org/10.3390/ma14102625

**Chicago/Turabian Style**

Domanowski, Piotr, and Marek Betiuk.
2021. "Recatest—A Technique for Qualitative and Quantitative Assessment of Deferment and Degraded PVD Coatings and CVD Layers in the Deformed Area in the Scratch Test" *Materials* 14, no. 10: 2625.
https://doi.org/10.3390/ma14102625