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Hydrogen Embrittlement Prevention in High Strength Steels by Application of

Various Surface Coatings-A Review

Chapter · January 2021

DOI: 10.1007/978-981-15-8542-5_58

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 Hydrogen Embrittlement Prevention in High Strength
Steels by Application of Various Surface Coatings-A Re-
view

Sandeep Kumar Dwivedi1 and Manish Vishwakarma2

1,2 Department of Mechanical Engineering, Maulana Azad National Institute of Technology,
Bhopal (M.P.), India-462003
[email protected]

Abstract. The applicability of various coatings such as graphene, reduced gra-

phene, al, cu, zn, carbon, nitrogen, oxygen, niobium, boron nitride, and TiAlN,
as a protective barrier to high strength steel for hydrogen embrittlement was stud-
ied. These all coatings were applied by different coating techniques such
as(chemical vapour deposition (CVD), electroplating discharge (EPD), electrol-
ysis, gas diffusion, plasma diffusion, high velocity oxygen fuel(HVOF), mag-
netically enhanced plasma ion plating system, plasma vapour deposition, and ion
beam sputter. ) on the high strength steel substrate followed by characterization
of applied coating and mechanical testing . Reduction in life cycle due to the
hydrogen embrittlement was analysed.

Keywords: Hydrogen Embrittlement; Graphene coating; Scanning electron microscopy

1 Introduction

The phenomenon of hydrogen embrittlement (HE) will occur when metal surfaces ex-
pose to hydrogen environment which leads to catastrophic failure. It was found that HE
considered as an important problem in several application areas, such as nuclear plant
reactor vessel [1,2], high-pressure gaseous hydrogen storage tanks [3,4], petroleum and
natural gas pipelines [5,6].
Generally, when metal comes to contact with the hydrogen or working in hydrogen
atmosphere, then some common ways by metals failed are hydrogen embrittlement
(HE), hydrogen-induced-blistering, hydrogen attack, cracking due to precipitation of
internal hydrogen, and hydride-formation cracking [7]. Generally, there are two mech-
anisms which responsible for the HE in steels. First One is that at cracks or crack tip,
hydrogen atoms are accumulated, and decreases the fracture energy while inspiring
cleavage-like failure [8,9]. The second mechanism includes mobility of dislocations
increased due to effect of hydrogen at crack tip through shielding effect, reducing the
shear strength, and ultimately responsible for local plasticity enhancement [10]. In or-
der to protect the equipment from the hydrogen diffusion it is necessary to measure how
much concentration of hydrogen has been diffused into the material at the time of fail-
ure, but thrush hold concentration of hydrogen which is causing the equipment failure
2

is not found clearly. And the basic mechanism which is responsible for the HE is also
not found clearly still some discussion is going on this [11].

It was found that hydrogen diffusion causes mechanical properties broadly ten-
sile-strength and fatigue strength are reduced with and without changes in yield
strength. Temperature, source of hydrogen and surface condition are responsible for HE
[12]. Various methods which were responsible for hydrogen entrance in the material
are cathodic reaction or charging, electroplating, and during welding etc [13]. Literature
said that the cathodic charging plays a very significant role for hydrogen diffusion and
current density considered as an important factor for hydrogen absorption and propa-
gation in steel. For hydrogen diffusion and embrittlement occurrence in steel, current
density must be in range of 0.02 mA/cm2 to 40 mA/cm2 [14,15]. It was concluded that
at higher current density, hydrogen absorption and propagation is faster than the lower
current density so more hydrogen is diffused at higher current density.
In this paper, the prevention of HE in high strength steels by application of different
surface coatings such as graphene, reduced graphene, al, cu, zn, carbon, nitrogen,
oxygen, niobium, boron nitride, and TiAlN , etc. are discussed and selection of suitable
coatings are given to reduce the HE phenomena.

2 Hydrogen embrittlement in steel

High strength steels are mostly subjected to hydrogen embrittlement effect. The em-
brittlement refers to change from ductile phase to brittle phase. Due to hydrogen caused
the embrittlement is termed as “hydrogen embrittlement”. HE can be noticeable in dif-
ferent ways. HE causes reduction in the following
• Ultimate-tensile strength and Braking strain or ductility
• Fracture strength and toughness
Furthermore, there is a case where unstressed components are subjected to failure.
However, there is a case in which ductility will decrease with no change in tensile
strength [16]. Examples of internal hydrogen embrittlement is solutions used during
fabrication like acid cleaning, electroplating, pickling, and providing protective coat-
ings, phosphating, etching, and paint stripping etc. Second way of HE is external hy-
drogen embrittlement which occurs during the working condition of equipment. The
following mechanisms by which hydrogen is entering and tapped in the lattice are
• Hydrogen-enhanced decohesion mechnaism (HEDE),
• Hydrogen-enhanced local plasticity model (HELP), and
• Adsorption-induced dislocation emission (AIDE) [7,81].
After entering into the metal lattice hydrogen will be tapped in different regions.
Examples of hydrogen taps are dislocations, grain boundaries, voids, and phase bound-
aries, micro cracks, precipitates, interfaces, solutes, surface cracks, surface oxides, and
0D,1D,2D lattice defects. In last 50 years various authors focus on research related to
hydrogen diffusion and hydrogen embrittlement (HE) [17–19]. Hydrogen causes slip
localization [20–22], softening and hardening [22–30], interaction between hydrogen–
dislocation [30–33] and creep [34] have been also reported, apart from all these effects
HE has severely effect fatigue crack rate behavior as well as tensile properties.
 3

3 Hydrogen embrittlement prevention

Complete prevention of HE in high strength steels is laborious but we can prevent

some extent so that we can save the life of the equipment. To reduce the hydrogen
diffusion from metal surface, sharp and very steady variation, notches must be pre-
vented or avoided and removal of residual stresses are performed before the processing
step [35,36]. Sometime baking operation is performed to remove hydrogen which was
available in lattice or surface during the processing. In broad view, Baking is considered
as a heat-treatment-process and processing temperature is depending on the process
material [37]. Prevention from HE can also be achieved by adding specific alloying
material to the base or parent material [7].
Our main focus on prevention of HE by surface coatings, surface coatings can be
done by different ways. Very well-known methods are chemical vapor deposition,
physical vapor deposition, electroplating, plasma vapor deposition, gas diffusion etc

3.1 HE prevention by reduced graphene oxide (rGO) coating

Graphene is most suitable element to reduce the HE from high strength steel materials.
It has a thin film of carbon-atom which has some unique properties [38-40]. Its chemi-
cal inertness properties make him to use at various operating condition. It is also stable
in atmospheres condition temperature to 400˚C and reduce the oxidation of the substrate
material because of hydrophobic characteristic or property [41], and that is due to its
non-polar covalent double bonds, which is responsible for prevention of hydrogen atom
bonding with the water [42,43]. That is the reason, we are selected the graphene mate-
rial as a coating due to its light weight and halt charge transmit at the metal-electrolyte
interface. Thus, most of the researchers have studied and selected the graphene as the
coating material [44]. However, graphene coating can diminish corrosion properties of
stainless steel as it is coated by CVD. So that graphene has replaced by reduced gra-
phene oxide (rGO) because of its high-volume, low in cost and processing capabilities
at room temperature. One of the economical methods to develop rGO on stainless steel
is electrophoretic-deposition method (EPD).
Kim and Kim (2017) were explained the effect of reduced graphene oxide coating
to reduce HE in stainless steel material. They were used the electrophoretic-decompo-
sition technique to coat the rGO above the substrate material. Evaluation of mechanical
properties was done by slow strain rate test (SSRT) during hydrogen charging condition
[45].
Synthetization of purified graphene to graphene oxide (GO) was done by modi-
fied-hammers method [46]. After this synthetization, GO was spreaded out in water and
sonicated at room temperature for 4 hrs in 4mg/ml concentration solution. After prep-
aration of GO solution, electrophoretic-deposition technique was used at 10V DC cur-
rent supply to deposit rGO. For achieving required thickness of rGO above the substrate
material time required to be 8 min. After completion of deposition process, samples
were taken in vacuum for drying to prevent from oxidation [45].
A below representation showing electrophoretic-deposition process for the es-
tablishment of reduced graphene oxide on the stainless-steel substrate material is illus-
trated in Fig.1.
4

Fig. 1. rGO deposition in the stainless-steel substrate by using EPD technique.[45].

3.1.1 Characterization of sample

The investigation of the rGO in surface and cross-section of substrate material (stainless
steel) was done by Scanning-electron-microscopy (SEM).

3.1.2 Electro chemical measurements

Electro chemical behavior of rGO on stainless-steel specimen was analyzed using the
conventional three electrode cell. Cathodic-polarization experiment or examination and
electrochemical-impedance spectroscopy were conducted on rGO. Initially 0.5 M sul-
furic acid solution (H2SO4) with 250 mg/L arsenic trioxide (As2O3) (pH = 1.0) was
prepared and samples were kept in that solution for 2 hours. So that hydrogen diffusion
and penetration was taken place easily. Nitrogen gas was flows through the solution to
remove the dissolved oxygen for 2 hours and then measurement was done [45].

3.1.3 Slow strain rate tests (SSRT)

SSRT have been widely applied to environmental induced cracking like corrosion
cracking and HE. In this case, SSRT testing was performed at strain rate of 1.0×10-6/s
to evaluate the effect of rGO deposit or coating to reduce the hydrogen embrittlement
effect in stainless-steel material. Here HC was done at a negative current (-0.5 A/cm2)
for investigation of behavior or effect of HE in coated and bare samples by SSRT test-
ing.
During the testing it was found that the mechanical properties like the yield,
tensile stresses, and strain, of stainless-steel specimen in hydrogen charging condition
are reduced. After applying the rGO coating to stainless steel specimen it was found
that the mechanical properties of coated sample return back to initial value of uncharged
specimen. Elongation behavior of hydrogen charged specimen was also affected and
reduced from percentage elongation of 40.1% to the value of 23.5% for uncharged to
 5

hydrogen charged specimen. While elongation percentage of rGO coated hydrogen

charged specimen comes around 35.6%. So, effect of HE in coated sample was reduced
and these coating acts a barrier for hydrogen diffusion in stainless steel [45].

3.2 Coating of Zn, Ni, Cu, Al, PVD-Ti-DLC, carbon, nitrogen and oxygen
diffusion layers
Electroplating of Zinc (Zn), Nickel (Ni), Copper (Cu), Aluminum (Al), PVD-Ti-DLC,
various diffusion layers such as oxygen, nitrogen and carbon and electroless NiP coat-
ings are examined and evaluated to reduce the effect of HE in 304 austenitic stainless-
steel material. SSRT testing was performed for mechanical properties estimation [81].
Metastable grades like AISI 304 material rigorously experience the HE effects be-
cause of austenite to ferrite phase transformation at the time of operation [47-49].
Zn,Ti-DLC, Al, Cu, and the oxygen diffusion layers as well as amorphous Nip
coatings were examined because of their unique quality of low hydrogen diffusion co-
efficient [50-59].
Two AISI 304 stainless steel of internal heat number 40,4 were used as a substrate
material for testing various coatings and diffusion layers. The coatings properties were
illustrated by metallo-graphic cross sections, Vickers and Rockwell testing, X-ray dif-
fraction (XRD) technique was used for internal stresses and phase analysis [60]. A sim-
ple coating and some diffusion layer properties are given below in table 1.
Table- 1. Overview of various coatings [60].
Coat- Coat- Deposition Thick- Hardness Ad- Remarks
ing ing technique ness hesion
mate- type acc [HF]
rial µm
Al On top Elecrtro- 22 15-25 HB 4 Globular structure
plating
Cu On top Elecrtro- 2 50-110HB 1 Thin coating with
plating pin load
Ni On top Elecrtro- 12 510 HV 1 Ni adhesion coat-
plating ing
Zn On top Elecrtro- 11 92 HV 2 Ductile zinc coat-
plating ing

NiP On top Electro- 10 550 HV 2 Amorphous NIP

less type coating
Ti- On top PVD 3 1440HV 1 Ti adhesion coating
DLC
Car- Diffu- Gas dif- 25 1225 HV 1 Long term gas dif-
bon sion fusion fusion
Nitro- Diffu- Gas dif- 500 300HV 1 Small term gas dif-
gen sion fusion fusion
oxy- Diffu- Plasma 1 1200 HV 2 Oxidizing at -
gen sion diffusion 5500C
Calculation of HV was done by some formula HB= 0.95HV
6

Cylindrical specimen is having an outer diameter 8mm, notch diameter 6mm, radius on
notch is 0.2mm and angle of notch is 35 0. Stress concentration factor is 3.4. Fatigue
testing was performed in that specimen and operated in atmosphere of hydrogen
(10MPa) until the specimen has broken or failure occurs.

3.3 Niobium coating on API 5CT P110 steel

In gas and oil industry the components are subjected to extreme conditions and ag-
gressive environment. The corrosion phenomena in API 5CT P110 steels is very fast
[61] and HE occurs in that steel due to working in aggressive condition [62]. By appli-
cation of coating in P110 steel, they exhibit a good corrosion resistance and also work
effectively in hydrogen environment as they show resistance for, HE [63].
Thermal spray coatings have received very good attention for protection of oil and
gas industry components against HE[64-67]. These kinds of coatings have growing and
expanding application in protection against fatigue operation [68] and oxidation pro-
cess [69-71] and economical and very efficient choice to meet all requirement [72].
Recently, various authors are working in development of nanostructured coating which
have better and superior properties [73-74]. Other coating techniques such as high ve-
locity oxygen fuel (HVOF) is also very efficient in case of corrosion in API 5CT P110
steel [75].
Niobium has very good corrosion resistant in various media [76,77], and refractory
properties [78,79]. HVOF coating technique was used to deposit niobium in API 5CT
P110 steel as it acts as a protective film over the base material against the corrosion.
The parameters which are responsible for spraying process are depicted in table.3.the
surface roughness of coating substrate was measured by contact profilometer in which
by Ry values were obtained. The micro hardness of both materials was obtained by
microhardness tests and this hardness test was performed at the 3N load and 15s holding
or processing time, as specified and given in the ASTM standard [80].

Table.3 niobium coatings spraying parameter [82]

Parameters used
Flow rate of oxygen(L/min) 164
Flow of Propane (L/min) 144
Compressed air flow (L/min) 181
Nitrogen flow – carrier gas (L/min) 290
Gun to substrate distance (mm) 300
Power feed rate (g/min) 41
Speed of Gun transverse (m/s) 0.2
Number of passes 5
4 Conclusions

i. Hydrogen embrittlement resistance of rGO coating in stainless steel was ex-

amined and investigated. Experimental result showed that rGO coated speci-
men have less tendency to absorb hydrogen the uncoated sample.
ii. During hydrogen charging condition, it was found that C-H bond formation
and increase in diffusion length causes resistance properties of rGO for hydro-
gen was influenced and it was clearly found out that rGO can act as barrier for
hydrogen penetration so improving the resistance for, HE.
 7

iii. During hydrogen charging condition in coated samples, some surface irregu-
larities, defects such pores, coating and surface interface, they act as a hydro-
gen accumulator and hydrogen adsorbed sites. So, these sides inhibiting the
entry of hydrogen from coated sample APT CT P110 steel. It is concluded that
hydrogen trapping capacity of coated sample was 7.5 time more than the nor-
mal steel specimen.
iv. Thermal spraying coating of niobium using HVOF is also reduce the suscep-
tibility of hydrogen embrittlement and act as barrier for hydrogen diffusion.
v. Electroplating of Zn, Cu, Ni, Al, PVD-Ti-DLC and electrolysis NiP coatings
along with oxygen, nitrogen and carbon diffusion layers were examined for
reducing the susceptibility of HE. It was found that carbon and nitrogen diffu-
sion layer work effectively to reduce hydrogen diffusion.
vi. It was found that vary little work is carried out for tensile and ductility im-
provement when worked on hydrogen atmosphere. The Ni and C diffusion
layers reduced crack propagation in hydrogen atmosphere.

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