Passivation (chemistry)

Passivation, in physical chemistry and engineering, refers to a material becoming "passive," that is,
less affected or corroded by the environment of future use. Passivation involves creation of an outer layer
of shield material that is applied as a microcoating, created by chemical reaction with the base material,
or allowed to build from spontaneous oxidation in the air. As a technique, passivation is the use of a light
coat of a protective material, such as metal oxide, to create a shell against corrosion.[1] Passivation can
occur only in certain conditions, and is used in microelectronics to enhance silicon.[2] The technique of
passivation strengthens and preserves the appearance of metallics. In electrochemical treatment of
water, passivation reduces the effectiveness of the treatment by increasing the circuit resistance, and
active measures are typically used to overcome this effect, the most common being polarity reversal,
which results in limited rejection of the fouling layer. Other proprietary systems to avoid electrode
passivation, several discussed below, are the subject of ongoing research and development.

When exposed to air, many metals naturally form a hard, relatively inert surface, as in the tarnish of
silver. In the case of other metals, such as iron, a somewhat rough porous coating is formed from loosely
adherent corrosion products. In this case, a substantial amount of metal is removed, which is either
deposited or dissolved in the environment. Corrosion coating reduces the rate of corrosion by varying
degrees, depending on the kind of base metal and its environment, and is notably slower in room-
temperature air for aluminium, chromium, zinc, titanium, and silicon (a metalloid). The shell of
corrosion product inhibits deeper corrosion, and operates as one form of passivation. The inert surface
layer, termed the "native oxide layer", is usually an oxide or a nitride, with a thickness of a monolayer of
0.1-0.3 nm (1-3 Å) for a noble metal such as platinum, about 1.5 nm (15 Å) for silicon, and nearer to 5 nm
(50 Å) for aluminium after several years.[3][4][5]

Surface passivation refers to a common semiconductor device fabrication process critical to modern
electronics. It is the process by which a semiconductor surface is rendered inert, and does not change
semiconductor properties as a result of interaction with air or other materials in contact with the surface
or edge of the crystal. This is typically achieved using a form of thermal oxidation. In a silicon
semiconductor, this process allows electricity to reliably penetrate to the conducting silicon below the
surface, and to overcome the surface states that prevent electricity from reaching the semiconducting
layer.[6][7] Surface passivation by thermal oxidation is one of the key features of silicon technology, and
is dominant in microelectronics. The surface passivation process was developed by Mohamed M. Atalla
at Bell Labs in the late 1950s.[6] It is commonly used to manufacture MOSFETs (metal-oxide-
semiconductor field-effect transistors) and silicon integrated circuit chips (with the planar process), and
is critical to the semiconductor industry.[6][7] Surface passivation is also critical to solar cell and carbon
quantum dot technologies.

Contents
Mechanisms
History
Discovery
Surface passivation
Specific materials
 Aluminium
Ferrous materials
Stainless steel
Nickel
Silicon
See also
References
Further reading

Mechanisms
There has been much interest in determining the mechanisms that
govern the increase of thickness of the oxide layer over time. Some
of the important factors are the volume of oxide relative to the
volume of the parent metal, the mechanism of oxygen diffusion
through the metal oxide to the parent metal, and the relative
chemical potential of the oxide. Boundaries between micro grains, if
the oxide layer is crystalline, form an important pathway for oxygen
to reach the unoxidized metal below. For this reason, vitreous oxide
coatings – which lack grain boundaries – can retard oxidation.[9]
The conditions necessary, but not sufficient, for passivation are
recorded in Pourbaix diagrams. Some corrosion inhibitors help the
Pourbaix diagram of iron.[8]
formation of a passivation layer on the surface of the metals to which
they are applied. Some compounds, dissolved in solutions
(chromates, molybdates) form non-reactive and low solubility films
on metal surfaces.

History

Discovery

In the mid 1800s, Christian Friedrich Schönbein discovered that when a piece of iron is placed in dilute
nitric acid, it will dissolve and produce hydrogen, but if the iron is placed in concentrated nitric acid and
then returned to the dilute nitric acid, little or no reaction will take place. Schönbein named the first
state the active condition and the second the passive condition. If passive iron is touched by active iron,
it becomes active again. In 1920, Ralph S. Lillie measured the effect of an active piece of iron touching a
passive iron wire and found that "a wave of activation sweeps rapidly (at some hundred centimeters a
second) over its whole length".[10][11]

Surface passivation

The surface passivation process, also known as the Atalla passivation technique,[12] was developed by
Mohamed M. Atalla at Bell Telephone Laboratories (BTL) in the late 1950s.[6][13] In 1955, Carl Frosch
and Lincoln Derick at Bell Telephone Laboratories (BTL) accidentally discovered that silicon dioxide
(SiO2) could be grown on silicon. They showed that oxide layer prevented certain dopants into the silicon
wafer, while allowing for others, thus discovering the passivating effect of oxidation on the
semiconductor surface.[14] In the late 1950s, Atalla further discovered that the formation of a thermally
grown SiO2 layer greatly reduced the concentration of electronic states at the silicon surface,[13] and
discovered the important quality of SiO2 films to preserve the electrical characteristics of p–n junctions
and prevent these electrical characteristics from deteriorating by the gaseous ambient environment.[15]
He found that silicon oxide layers could be used to electrically stabilize silicon surfaces.[16] J.R. Ligenza
and W.G. Spitzer, who studied the mechanism of thermally grown oxides, managed to fabricate a high
quality Si/SiO2 stack, with Atalla and Kahng making use of their findings.[17][18][19] Atalla developed the
surface passivation process, a new method of semiconductor device fabrication that involves coating a
silicon wafer with an insulating layer of silicon oxide so that electricity could reliably penetrate to the
conducting silicon below. By growing a layer of silicon dioxide on top of a silicon wafer, Atalla was able
to overcome the surface states that prevented electricity from reaching the semiconducting layer.[6][7]
For the surface passivation process, he developed the method of thermal oxidation, which was a
breakthrough in silicon semiconductor technology.[20]

Before the development of integrated circuit chips, discrete diodes and transistors exhibited relatively
high reverse-bias junction leakages and low breakdown voltage, caused by the large density of traps at
the surface of single crystal silicon. Atalla's surface passivation process became the solution to this
problem. He discovered that when a thin layer of silicon dioxide was grown on the surface of silicon
where a p–n junction intercepts the surface, the leakage current of the junction was reduced by a factor
from 10 to 100. This showed that the oxide reduces and stabilizes many of the interface and oxide traps.
Oxide-passivation of silicon surfaces allowed diodes and transistors to be fabricated with significantly
improved device characteristics, while the leakage path along the surface of the silicon was also
effectively shut off. This became one of the fundamental isolation capabilities necessary for planar
technology and integrated circuit chips.[21]

Atalla first published his findings in BTL memos during 1957, before presenting his work at an
Electrochemical Society meeting in 1958.[22][23] The same year, he made further refinements to the
process with his colleagues E. Tannenbaum and E.J. Scheibner, before they published their results in
May 1959.[24][25] According to Fairchild Semiconductor engineer Chih-Tang Sah, the surface passivation
process developed by Atalla's team "blazed the trail" that led to the development of the silicon integrated
circuit.[21][24] Atalla's surface passivation method was the basis for several important inventions in 1959:
the MOSFET (MOS transistor) by Atalla and Dawon Kahng at Bell Labs, the planar process by Jean
Hoerni at Fairchild Semiconductor, and the monolithic integrated circuit chip by Robert Noyce at
Fairchild in 1959.[22][23][21][24] By the mid-1960s, Atalla's process for oxidized silicon surfaces was used
to fabricate virtually all integrated circuits and silicon devices.[26]

In solar cell technology, surface passivation is critical to solar cell efficiency.[27] In carbon quantum dot
(CQD) technology, CQDs are small carbon nanoparticles (less than 10  nm in size) with some form of
surface passivation.[28][29][30]

Specific materials

Aluminium

Aluminium naturally forms a thin surface layer of aluminium oxide on contact with oxygen in the
atmosphere through a process called oxidation, which creates a physical barrier to corrosion or further
oxidation in many environments. Some aluminium alloys, however, do not form the oxide layer well, and
thus are not protected against corrosion. There are methods to enhance the formation of the oxide layer
for certain alloys. For example, prior to storing hydrogen peroxide in an aluminium container, the
container can be passivated by rinsing it with a dilute solution of nitric acid and peroxide alternating
with deionized water. The nitric acid and peroxide mixture oxidizes and dissolves any impurities on the
inner surface of the container, and the deionized water rinses away the acid and oxidized impurities.[31]

Generally, there are two main ways to passivate aluminium alloys (not counting plating, painting, and
other barrier coatings): chromate conversion coating and anodizing. Alclading, which metallurgically
bonds thin layers of pure aluminium or alloy to different base aluminium alloy, is not strictly passivation
of the base alloy. However, the aluminium layer clad on is designed to spontaneously develop the oxide
layer and thus protect the base alloy.

Chromate conversion coating converts the surface aluminium to an aluminium chromate coating in the
range of 0.00001–0.00004 inches (250–1,000  nm) in thickness. Aluminium chromate conversion
coatings are amorphous in structure with a gel-like composition hydrated with water.[32] Chromate
conversion is a common way of passivating not only aluminium, but also zinc, cadmium, copper, silver,
magnesium, and tin alloys.

Anodizing is an electrolytic process that forms a thicker oxide layer. The anodic coating consists of
hydrated aluminium oxide and is considered resistant to corrosion and abrasion.[33] This finish is more
robust than the other processes and also provides electrical insulation, which the other two processes
may not.

Ferrous materials

Ferrous materials, including steel, may be somewhat protected by promoting oxidation ("rust") and then
converting the oxidation to a metalophosphate by using phosphoric acid and further protected by surface
coating. As the uncoated surface is water-soluble, a preferred method is to form manganese or zinc
compounds by a process commonly known as parkerizing or phosphate conversion. Older, less-effective
but chemically-similar electrochemical conversion coatings included black oxidizing, historically known
as bluing or browning. Ordinary steel forms a passivating layer in alkali environments, as reinforcing bar
does in concrete.

Stainless steel

Stainless steels are corrosion-resistant, but they are not completely

impervious to rusting. One common mode of corrosion in corrosion-
resistant steels is when small spots on the surface begin to rust
because grain boundaries or embedded bits of foreign matter (such
as grinding swarf) allow water molecules to oxidize some of the iron
in those spots despite the alloying chromium. This is called rouging.
Some grades of stainless steel are especially resistant to rouging;
The fitting on the left has not been
parts made from them may therefore forgo any passivation step,
passivated, the fitting on the right
depending on engineering decisions.[34] has been passivated.

Common among all of the different specifications and types are the
following steps: Prior to passivation, the object must be cleaned of
any contaminants and generally must undergo a validating test to prove that the surface is 'clean.' The
object is then placed in an acidic passivating bath that meets the temperature and chemical
requirements of the method and type specified between customer and vendor. While nitric acid is
commonly used as a passivating acid for stainless steel, citric acid is gaining in popularity as it is far less
dangerous to handle, less toxic, and biodegradable, making disposal less of a challenge. Passivating
temperatures can range from ambient to 60 degrees C, or 140 degrees F, while minimum passivation
times are usually 20 to 30 minutes. After passivation, the parts are neutralized using a bath of aqueous
sodium hydroxide, then rinsed with clean water and dried. The passive surface is validated using
humidity, elevated temperature, a rusting agent (salt spray), or some combination of the three.[35]The
passivation process removes exogenous iron,[36] creates/restores a passive oxide layer that prevents
further oxidation (rust), and cleans the parts of dirt, scale, or other welding-generated compounds (e.g.
oxides).[36][37]

Passivation processes are generally controlled by industry standards, the most prevalent among them
today being ASTM A 967 and AMS 2700. These industry standards generally list several passivation
processes that can be used, with the choice of specific method left to the customer and vendor. The
"method" is either a nitric acid-based passivating bath, or a citric acid-based bath, these acids remove
surface iron and rust, while sparing the chromium. The various 'types' listed under each method refer to
differences in acid bath temperature and concentration. Sodium dichromate is often required as an
additive to oxidise the chromium in certain 'types' of nitric-based acid baths, however this chemical is
highly toxic. With citric acid, simply rinsing and drying the part and allowing the air to oxidise it, or in
some cases the application of other chemicals, is used to perform the passivation of the surface.

It is not uncommon for some aerospace manufacturers to have additional guidelines and regulations
when passivating their products that exceed the national standard. Often, these requirements will be
cascaded down using Nadcap or some other accreditation system. Various testing methods are available
to determine the passivation (or passive state) of stainless steel. The most common methods for
validating the passivity of a part is some combination of high humidity and heat for a period of time,
intended to induce rusting. Electro-chemical testers can also be utilized to commercially verify
passivation.

Nickel

Nickel can be used for handling elemental fluorine, owing to the formation of a passivation layer of
nickel fluoride. This fact is useful in water treatment and sewage treatment applications.

Silicon

In the area of microelectronics and photovoltaics surface passivation is usually implemented by

oxidation to a coating of silicon dioxide. The effect of passivation on the efficiency of solar cells ranges
from 3-7%. Passivation is effected by thermal oxidation at 1000 °C. The surface resistivity is high, >100
Ωcm.[38]

See also
Cold welding
Deal-Grove model
Dental implant
Pilling–Bedworth ratio

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Further reading
ASTM (1 March 2010), ASTM A967: Standard specification for chemical passivation treatments for
stainless steel parts (http://www.astm.org/Standards/A967.htm) (Rev 05e2 ed.), doi:10.1520/A0967-
05E02 (https://doi.org/10.1520%2FA0967-05E02). The most common commercial spec for
passivation of stainless steel parts. Used in various industries; latest revision is active for new
designs; legacy designs may still require older revisions or older standards, if the engineering has
not been revisited.
SAE (8 July 2011), AMS 2700: Passivation of corrosion resistant steels. (http://standards.sae.org/am
s2700d/) (Rev D ed.). AMS specs are frequently used in the aerospace industry, and are sometimes
stricter than other standards. Latest revision is active for new designs; legacy designs may still
require older revisions or older standards, if the engineering has not been revisited.
SAE (16 February 2005), AMS QQ-P-35: Passivation treatments for corrosion-resistant steel (http://s
tandards.sae.org/amsqqp35a) (Rev A ed.). AMS-QQ-P-35 superseded U.S. federal spec QQ-P-35
on 4 April 1997. AMS-QQ-P-35 itself was canceled and superseded in February 2005 by AMS 2700.
U.S. government, QQ-P-35: Federal specification: Passivation treatments for corrosion-resistant
steel (http://www.everyspec.com/FED_SPECS/Q/QQ-P-35C_NOTICE-3_21310/) (Rev C ed.). U.S.
federal spec QQ-P-35 was superseded by AMS-QQ-P-35 on 4 April 1997 as part of the changeover
instituted by the Perry memo. Both are now outdated; they are inactive for new designs, but legacy
designs may still require their use, if the engineering has not been revisited.
Chromate conversion coating (chemical film) per MIL-DTL-5541F for aluminium and aluminium alloy
parts
A standard overview on black oxide coatings is provided in MIL-HDBK-205, Phosphate & Black
Oxide Coating of Ferrous Metals. Many of the specifics of Black Oxide coatings may be found in
MIL-DTL-13924 (formerly MIL-C-13924). This Mil-Spec document additionally identifies various
classes of Black Oxide coatings, for use in a variety of purposes for protecting ferrous metals against
rust.
Budinski, Kenneth G. (1988), Surface Engineering for Wear Resistance, Englewood Cliffs, New
Jersey: Prentice Hall, p. 48.
Brimi, Marjorie A. (1965), Electrofinishing, New York, New York: American Elsevier Publishing
Company, Inc, pp. 62–63.
Bockris, John O'M.; Reddy, Amulya K. N. (1977), Modern Electrochemistry: An Introduction to an
Interdisciplinary Area, 2, Plenum Press, ISBN 0-306-25002-0.
Passivisation : Debate over Paintability http://www.coilworld.com/5-6_12/rlw3.htm

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