METRIC

MIL-STD-3021
4 August 2008
_______________________________

DEPARTMENT OF DEFENSE
MANUFACTURING PROCESS
STANDARD

MATERIALS DEPOSITION, COLD SPRAY

AMSC N/A AREA MFFP

DISTRIBUTION STATEMENT A. Approved for public release; distribution is unlimited.

 MIL-STD-3021

FOREWORD

1. This standard is approved for use by all Departments and Agencies of the Department of
Defense.

2. The purpose of this standard is to develop the manufacturing process controls for a cold
spray operation utilizing a high-velocity jet of solid-phase particles. The jet temperatures are
below the melting thresholds of many engineering materials. This allows the process to be used
to apply deposits on a wide variety of substrates, such as, alloys, ceramics, and plastics.
Moreover, the deleterious effects of deposit oxidation, evaporation, and residual stresses are
avoided.

3. This standard is required because the cold spray deposition process has significant
differences from thermal spray coating technologies such as high velocity oxy-fuel (HVOF),
detonation gun, plasma spray, flame spray, and arc spray. These process differences result in
application criteria, process equipment, and operating parameters that are considerably different
than previously documented processes. The objective is to enable the application of Cold Spray
Deposition with the success of the aforementioned processes when properly applied.

4. Comments, suggestions, or questions on this document should be addressed to:

Director, U.S. Army Research Laboratory, Weapons and Materials Research Directorate,
Materials Applications Branch, Specifications and Standards Office, Attn: AMSRD-ARL-WM-
MC, Aberdeen Proving Ground, MD 21005-5069 or emailed to [email protected]. Since
contact information can change, you may want to verify the currency of this address information
using the ASSIST Online database at http://assist.daps.dla.mil/.

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CONTENTS

PARAGRAPH PAGE

FOREWORD……………………………………………………………… ii

1. SCOPE
1.1 Purpose…………………………………………………………… .. 1
1.2 Process…….……………………………………………………….. 1
1.2.1 Types. ……………………………………………………………… 1
1.3 Applications. …………………………………………….………… 1

2. APPLICABLE DOCUMENTS
2.1 General……………………………………………………………. 2
2.2 Government documents. …………………………………………. 2
2.2.1 Specifications, standards, and handbooks. ……………………….. 2
2.3 Non-Government publications……………………......................... 3
2.4 Order of precedence…………………………………..................... 3

3. DEFINITIONS
3.1 Cold spray. …………………………………................................... 3
3.2 Nozzle. …………………………………......................................... 4
3.3 Powder lot. …………………………………................................... 4
3.4 Powder meter wheel ………………………………………………. 4
3.5 Simulated part…………………………………………………….. 4
3.6 Substrate............................................................................................ 4
3.7 Lot………………………………………………………………….. 4
3.8 Pass. ………………………………………………………………... 4
3.9 Increment …………………………………………………………... 4
3.10 Layer. ……………………………………………………………..... 4
3.11 Thermal spraying. ……………………….………………………..... 4

4. GENERAL REQUIREMENTS
4.1 Application......................................................................................... 4
4.2 Process. .............................................................................................. 5
4.2.1 Cold spray equipment……………………………………….............. 5
4.2.2 Material. ............................................................................................. 5
4.2.2.1 Gas. .................................................................................................... 5
4.2.2.1.1 Gas specifications …………………………………………………… 5
4.2.2.2 Coating powder. ................................................................................. 5
4.3 Required procedures and operations. ................................................. 6
4.3.1 Process control. .................................................................................. 6
4.3.1.1 Gauges, meters, and sensors ………………………………………… 6
4.3.1.2 Checks................................................................................................. 6
4.3.2 Surface preparation. ........................................................................... 6
4.3.2.1 Cleaning. ............................................................................................ 6

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CONTENTS

PARAGRAPH PAGE

4.3.2.2 Handling and storage. ........................................................................ 6

4.3.2.2.1 Handling. ........................................................................................... 7
4.3.2.2.2 Storage. .............................................................................................. 7
4.3.2.3 Overspray protection. ........................................................................ 7
4.3.3 Abrasive blast. ................................................................................... 7
4.3.3.1 Blast contamination………………………………………………… 7
4.3.4 Preheating. ......................................................................................... 7
4.3.5 Coating deposition. ............................................................................ 7
4.3.6 Identification. ..................................................................................... 9
4.4 Operator certification. ........................................................................ 9
4.4.1 Cold spray operator. ........................................................................... 9
4.4.1.1 Continuance of certification ............................................................. 9

5. DETAILED REQUIREMENTS
5.1 General................................................................................................ 9
5.1.1 Certification........................................................................................ 9
5.1.1.1 Certification samples. ........................................................................ 9
5.1.1.2 Re-certification ................................................................................. 10
5.1.2 Test samples. ....................................................................................... 10
5.1.2.1 Metallographic test specimens. ........................................................... 10
5.1.2.1.1 Specimen configuration. ..................................................................... 10
5.1.2.2 Bond strength specimens. ................................................................... 10
5.1.2.2.1 Size...................................................................................................... 10
5.1.2.2.2 Material. ............................................................................................. 10
5.1.2.2.3 Deposit. .............................................................................................. 10
5.1.2.2.4 Deposition thickness. .......................................................................... 10
5.1.3 Process approvals. .............................................................................. 10
5.1.3.1 Processing data. .................................................................................. 10
5.1.3.2 Sample part. ........................................................................................ 11
5.1.3.3 Rework. .............................................................................................. 11
5.1.3.3.1 Stripping. ............................................................................................ 11
5.1.3.4 Metallographic test sample. ................................................................ 11
5.1.4 Process certification. ........................................................................... 11
5.2 Test methods. ...................................................................................... 11
5.2.1 Visual. ................................................................................................. 11
5.2.2 Micro examination. ............................................................................. 11
5.2.3 Oxides and porosity. ........................................................................... 12
5.2.4 Bond strength test. ............................................................................. 12

6. NOTES
6.1 Intended use......................................................................................... 12
6.2 Acquisition requirements. ................................................................... 12

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CONTENTS

PARAGRAPH PAGE

6.3 Issue of DoDISS. ................................................................................ 13

6.4 Safety. ................................................................................................. 13
6.4.1 Material safety data sheets (MSDS). .................................................. 13
6.5 English units ………………………………………………………… 13
6.6 Subject term (key word) listing. ......................................................... 14

TABLE

I. Operating parameters.......................................................................... 6

FIGURE

1. High-pressure system.......................................................................... 2
2. Low-pressure system……….………………………………….……. 2
3. Typical cold spray control sheet…………..………….……….…….. 8

CONCLUDING MATERIAL..................................................................................... 14

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1. SCOPE

1.1 Purpose. The procedures covered by this standard are intended to ensure that cold
spray coating operations, either manual or automated, meet prescribed requirements. This
process can be used to restore dimensionally discrepant parts, or parts requiring protection from
corrosion and wear (e.g. abrasion, cavitations, and erosion) but not limited to these applications.

1.2 Process. This standard describes the process requirements for surfacing by means of
cold spray deposition. The term “cold spray” has been used to describe this process because both
the temperature of the powder-laden gas jet and the temperature of the powder material are low
enough to prevent a phase change or stress in the deposit or substrate. Cold spray is a process
whereby metal powder particles are utilized to form a deposit by means of ballistic impingement
upon a substrate. The metal powders range in particle size from 5 to 100 micrometers (µm) and
are accelerated by injection into a high-velocity stream of gas. The high velocity gas stream is
generated through the expansion of a pressurized, preheated, gas through a nozzle. The
pressurized gas is expanded in order to achieve high velocity, with an accompanying decrease in
pressure and temperature. The powder particles, initially carried by a separate gas stream, are
injected into the nozzle either at the nozzle entrance or at a lower pressure point downstream of
the entrance. The particles are then accelerated by the main nozzle gas flow and are impacted
onto a substrate after exiting the nozzle. The solid particles that impact the substrate above a
threshold (critical) velocity for the powder and substrate combination will deform and bond in a
dense layer. As the process continues, particles continue to impact the substrate and form bonds
with the previously deposited material resulting in a uniform deposition with very little porosity
and high bond strength.

1.2.1 Types. The two principal cold spray system configurations are depicted by
Figures 1 and 2. The two configurations differ in the carrier gas, gas pressure, and powder
injection location. Figure 1 shows a high-pressure system in which the main gas stream and the
powder stream are both introduced into the inlet chamber of the nozzle. This configuration
requires that the powder feeder be capable of high gas pressure and is most often used in
stationary cold spray systems. High-pressure systems utilize higher pressure gases and often
have a dedicated gas compressor. A low molecular weight gas, such as helium, is sometimes
used as the accelerating gas when particles must be brought to very high velocity. Figure 2
shows a system in which the powder stream is injected into the nozzle at a point where the gas
has expanded to low pressure. Atmospheric pressure air, drawn by the lower pressure nozzle
injection point, is used for powder transport from the feeder. Since this system does not require
a pressurized feeder, it is often used in portable cold spray systems. The low-pressure system
generally utilizes readily available compressed air, but can utilize nitrogen as well.

1.3 Applications. The superior qualities of cold sprayed deposits are often required by
the application. For example, the high heat transfer coefficient and electrical conductivity of cold
sprayed deposits favor its use in electronic applications. Applications for cold spray technology
often occur in situations where conventional thermal metal spray technology cannot be
successfully used and where cold spray will result in an improved deposit. These situations often
occur when high temperatures cannot be tolerated by the substrate. Good corrosion protection is

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achieved by dense, impermeable cold sprayed deposits. Wear resistant, hard surfaces, such as
MCrAlYs, can be deposited by cold spray when operated at its high-temperature end.

Gas heater

Pressured gas
2.5 – 4.5 MPa Nozzle

Powder
feeder Substrate

FIGURE 1. High-pressure system.

Pressured gas
Gas heater Nozzle
0.5 – 1 MPa

Low pressure Substrate

Powder
gas, 1 atm
feeder

FIGURE 2. Low-pressure system.

2. APPLICABLE DOCUMENTS

2.1 General. The documents listed in this section are specified in sections 3, 4, or 5 of this
standard. This section does not include documents cited in other sections of this standard or
recommended for additional information or as examples. While every effort has been made to
ensure the completeness of this list, document users are cautioned that they must meet all
specified requirements of documents cited in sections 3, 4, or 5 of this standard, whether or not
they are listed.

2.2 Government documents.

2.2.1 Specifications, standards, and handbooks. The following specifications, standards,

and handbooks form a part of this document to the extent specified herein. Unless otherwise
specified, the issues of these documents are those cited in the solicitation or contract.

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 MIL-STD-3021

DEPARTMENT OF DEFENSE SPECIFICATIONS

MIL-S-5002 - Surface Treatments and Inorganic Coatings for

Metal Surfaces of Weapons Systems

(Copies of these documents are available online at http://assist.daps.dla.mil/quicksearch/ or

http://assist.daps.dla.mil/ or from the Standardization Document Order Desk, 700 Robbins
Avenue, Building 4D, Philadelphia, PA 19111-5094.)

2.3 Non-Government publications. The following documents form a part of this

document to the extent specified herein. Unless otherwise specified, the issues of these
documents are those cited in the solicitation or contract.

SAE INTERNATIONAL

SAE-AMS 2750 - Pyrometry (DoD Adopted).

(Copies of this document are available from www.sae.org or SAE International, 400
Commonwealth Drive, Warrendale, PA 15096-0001)

ASTM INTERNATIONAL

ASTM C633 - Standard Test Method for Adhesion or Cohesion

Strength of Thermal Spray Coatings (DoD Adopted)
ASTM E3 - Standard Guide for Preparation of Metallographic
Specimens (DoD Adopted).
ASTM E407 - Standard Practice for Micro-Etching Metals and
Alloys (DoD Adopted).

(Copies of these documents are available from www.astm.org or ASTM International, 100 Barr
Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959.)

2.4 Order of precedence. In the event of a conflict between the text of this document
and the references cited herein, the text of this document takes precedence. Nothing in this
document, however, supersedes applicable laws and regulations unless a specific exemption has
been obtained.

3. DEFINITIONS

3.1 Cold spray. Cold spray is a materials deposition process in which relatively small
particles (ranging in size from approximately 5 to 100 micrometers (µm) in diameter) in the solid
state are accelerated to high velocities (typically 300 to 1200 meters/second), and subsequently
develop a coating or deposit by impacting an appropriate substrate. Various terms—including
“kinetic energy metallization,” “kinetic metallization,” “kinetic spraying,” “high-velocity powder
deposition,” and “cold gas-dynamic spray method”—have been used to refer to this technique.
In most instances, deformable powder particles in a gas carrier are brought to high velocities

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through introduction into a nozzle, designed to accelerate the gas. The subsequent high-velocity
impact of the particles onto the substrate disrupts the oxide films on the particle and substrate
surfaces, pressing their atomic structures into intimate contact with one another under
momentarily high interfacial pressures and temperatures.

3.2 Nozzle. A gas manifold designed to accelerate a gas to high velocity.

3.3 Powder lot. A powder lot is all the powder of a specified type manufactured at the
same time.

3.4 Powder meter wheel. A perforated wheel which meters powder feed rate through
rotation speed.

3.5 Simulated part. A simulated part is a test piece or section with a similar surface
configuration to the part it represents. The simulated part will be approved by the acquisition
authority.

3.6 Substrate. The material, work piece or substance on which a coating is deposited.

3.7 Lot. A lot is all the parts of a similar configuration, coated sequentially on the same
machine setup using the same batch of coating material and process parameters, within a shift or
eight hours of operation, and presented for processor’s inspection at one time.

3.8 Pass. A single traverse by the nozzle over the work piece.

3.9 Increment. The distance between adjacent passes.

3.10 Layer. Multiple passes over the work piece that result in complete coverage.

3.11 Thermal spraying. A group of processes wherein metallic or nonmetallic materials

are deposited in a molten or semi-molten condition to form a deposit. The feed material may
initially be in the form of powder, ceramic rod, or wire.

4. GENERAL REQUIREMENTS

4.1 Application. The cold spray process has been used to produce dense, pure, thick and
well bonded deposits of many metals and alloys, such as aluminum (Al), copper (Cu), nickel
(Ni), tantalum (Ta), commercially pure titanium (Ti), silver (Ag), and zinc (Zn), as well as
stainless steel, nickel-base alloys (Inconels, Hastalloys), and bondcoats, such as MCrAlYs. Cold
spray can produce composites, such as metal-metal like copper-tungsten (Cu-W) or copper-
chromium, metal-carbides like aluminum-silicon carbide (Al-SiC), and metal-oxides like
aluminum-alumina. Cold spray has been used to produce protective coatings and performance
enhancing layers, ultra thick coatings, freeform and near net shape substrates. Typical protective
coatings produced by cold spray include MCrAlY coatings for high temperature protection and
bond coats for thermal barriers, copper-chrome layers for oxidation protection, and corrosion
resistant aluminum and zinc coatings for oil and auto industries and others.

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4.2 Process. The process utilizes nitrogen, which has been compressed to propel metal
powder onto the surface of a substrate. Alternatively, compressed air or helium may be used.
The deposition thickness produced by a moving nozzle can vary from 0.01 to 1.0 millimeter
(mm), depending on powder feed rate, nozzle traverse speed, and deposition efficiency. The
cold spray nozzle is frequently handled by a robot. Multiple coating layers can result in deposits
several centimeters thick. The width of a single pass can be between 2 and 12 mm, depending on
nozzle design, and large surfaces can be coated through multiple, slightly overlapping, parallel
passes. Large sizes and shapes can be spray fabricated and geometrical features can be easily
incorporated during spray preparation and subsequent machine finishing. Moreover, by
controlling the feedstock composition, one could vary the deposit microstructure and
composition to produce functionally graded materials and other special structures.

4.2.1 Cold spray equipment. The process gas is introduced to a manifold system
containing a gas heater and powder-metering device. The pressurized gas is heated to a preset
temperature, often using a coil of an electrical resistance-heated tube. The gas is heated not to
heat or soften spray particles, but instead to achieve higher flow velocities, which ultimately
result in higher particle impact velocities. The high-pressure gas is introduced into the entrance
of a nozzle (converging/diverging or converging only), where the gas accelerates to high velocity
(Mach numbers ranging from 1 to 4) as it expands in the nozzle. The gas cools as it expands in
the spray nozzle, sometimes exiting the spray gun at below ambient temperature. The powder to
be deposited is introduced by a separate gas stream either at the nozzle entrance or at a lower
pressure location on the nozzle, where the powder mixes with the main gas stream and is
accelerated by the gas stream.

4.2.2 Material.

4.2.2.1 Gas. The gas may be (but not restricted by) any of the following:

a. Nitrogen (N2).
b. Helium (He).
c. Mixture of nitrogen and helium (N2 + He).
d. Air.

4.2.2.1.1 Gas specifications. Gas specifications, if used by the processor for

procurement, shall be acceptable to the cognizant engineering organization.

4.2.2.2 Coating powder. The powder for coating shall be dry, free flowing, and
thoroughly blended. Mixtures of powder stock with varying density and/or size particulates shall
be kept from settling or stratifying in the feeder as long as that powder charge is utilized. The
mass median particle size shall be between 5 and 100 micrometers in diameter. The user should
be cautioned to the importance of paying attention to the manufacturer’s instructions pertaining
to the storage and handling of finely divided metal powders. If the powder to be used by the
manufacturer requires that it is controlled by a specification, it shall be specified in the contract
or purchase order (see (6.2).

4.3 Required procedures and operations.

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4.3.1 Process control. The cold spray process is optimized through the adjustment of
control parameters. These parameters include the gas preheat temperature, gas pressure, nozzle
geometry, throat size, powder feed rate, and spray distance. A critical process parameter is the
feedstock powder material itself—primarily particle size distribution and particle attributes such
as oxide layer and mechanical properties, which influence the ability to form a compacted
deposit. Operational parameters are typically selected to achieve the most suitable deposit for
its intended application at the lowest operational temperatures. The distinguishing feature of the
cold spray process compared with conventional thermal spray processes is its ability to produce
deposits with preheated gas temperatures in the range of 0 to 800° C, a range that is generally
lower than the melting temperature of the coating particle materials. The nozzle exit temperature
is substantially lower than the gas pre-heat temperature, further lowering the temperature
excursions experienced by the feedstock particles and substrate materials. The range of
operation for the stationary and portable cold spray systems is provided in Table I. The values in
the table are representative of values currently in use but are not necessarily limiting values for
the systems.

4.3.1.1 Gauges, meters, and sensors. If a minimum accuracy is required on these

instruments, it shall be defined in the contract or purchase order (see (6.2).

4.3.1.2 Checks. Process control procedures shall be checked during cold spraying to
assure that the specified operating parameters on the control sheet are maintained (see Figure 3).
The nozzle shall be checked between runs for internal wear / deposition. The operator shall
determine if the nozzle needs to be replaced and/or cleaned.

TABLE I. Operating parameters.

High-Pressure System Low-Pressure System

Working gas N2, He, air N2, air
Gas pressure, MPa 2.5 – 4.5 0.5 – 1.0
Gas preheat, °C 20 - 800 20 - 550
3
Gas flow rate, m /hour 50 - 150 15 - 30
Maximum Gas Mach # 1-3 1-3
Powder flow rate, g/s 0.1 – 1.0 0.1 – 1.0
Particle size, μm 5 - 100 10 - 80

4.3.2 Surface preparation.

4.3.2.1 Cleaning. Surfaces to receive deposits shall be thoroughly cleaned to remove oil,
grease, dirt, paint and other foreign material. Final cleaning shall take place no more than four
hours prior to coating. Cleaning procedures shall not embrittle, pit, or damage surfaces to be
coated.

4.3.2.2 Handling and storage.

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4.3.2.2.1 Handling. All surfaces requiring cold spraying shall be handled with clean lint-
free gloves, tongs, or other means that will avoid surface contamination.

4.3.2.2.2 Storage. If a delay in spraying occurs beyond 2 hours but less than 20 hours
(except for magnesium which shall be limited to 8 hours), special measures shall be employed to
protect the surface to be coated from dust, dirt, moisture, and other contaminants such as flash
rust or excessive oxidation that would reduce adhesion of the cold-sprayed deposit. Protection
shall be in the form of covering or inserting the parts in clean plastic bags. Alternative methods
may be to store parts overnight in a moderate temperature oven maintained at approximately 95°
± 3° C or in a vacuum chamber under low pressure. Should the delay in spraying, after proper
surface preparation, exceed 20 hours the parts shall be reprocessed in accordance with 4.3.2.1.

4.3.2.3 Overspray protection. Areas adjacent to the area to be cold spray coated shall be
suitably protected from overspray by masking or shielding.

4.3.3 Abrasive blast. When required, all surfaces designated for cold spray coating shall
be cleaned by abrasive blasting with the abrasive media specified in the qualified procedure.

4.3.3.1 Blast contamination. All blast media shall be free of contamination that will
affect the base material, such as, utilizing a blasting cabinet that has been used for ferrous
substrates in the past and is now being used for nonferrous substrates such as aluminum or
magnesium.

4.3.4 Preheating. When required as specified in the contract or purchase order (see 6.2),
surfaces shall be preheated by a suitable and controllable source. The following shall apply:

a. Preheating is performed to remove moisture and minimize the thermal shock effect
encountered during deposition. Preheating of the substrate is also known to improve
deposition efficiency and bond strength as well.

b. Temperature of the part, during the preheating and coating application, shall be
controlled to prevent discoloration, oxidation, distortion and other conditions detrimental
to the coating or substrate.

c. Temperature of the part after preheat and prior to spraying shall be measured using the
appropriate pyrometric devices in accordance with AMS 2750.

CAUTION: Special care must be taken to avoid overheating nonferrous alloys with low melting
temperatures such as aluminum and magnesium.

4.3.5 Coating deposition. The coating material shall be deposited on the designated
surfaces to a sufficient thickness to provide, after subsequent operations, a finished composition
and thickness which will meet the engineering specifications.

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VENDOR: Sheet ___ of ___

VENDOR PROCESS #:
PURCHASE ORDER NUMBER:
PART NUMBER: S/N:
AREA TO RECEIVE DEPOSITION:
COLD SPRAY (CS) MANUFACTURER:
PART MATERIAL:
CS TYPE: NOZZLE:
PART PREPARATION
METHOD OF CLEANING:
MASKING INFORMATION:
GRIT TYPE AND SIZE:
GRIT BLAST PRESSURE (MPa) :______ + Suction : _________ Pressure : _________
GAS (1) PRIMARY: Temperature Deg. C ____________+
Main Gas Pressure MPa______________ + Main Gas Flow (1) m3/hour. _______ +
Feeder Gas Pressure MPa_____________ + Feeder Gas Flow (2) m3/hour. ______ +
COATING POWDER
Powder material:_______________________ Powder size:_____________________
Supplier:____________________________ Material Lot # :____________________
COATING DATA
Elapsed Time Between Surface Prep and Spraying:______________________________
Powder Feed Rate (kg/hr): ___________________________________________
Powder Meter Wheel: _______________________________________________
Nozzle to Work Distance:_____________________________________________
Traverse rate (mm/s):_________________
Preheat Temp:
Increment (mm):____________________
Deposition Thickness as Sprayed: Method of Preheat:
Number of Passes Per Layer: Number of Layers:
Method of Cooling (if any): __________________________________________
NOTES:

CERTIFICATION #:_____________________________________________
APPROVAL: __________________________________________________
FIGURE 3. Typical cold spray control sheet.

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4.3.6 Identification. Unless otherwise specified in the contract or purchase order (see
6.2), each coated part shall be identified by applying the symbol CS as a prefix to the serial
number (e.g., CS S/N 1234) or as a prefix to the Federal manufacturer code on non-serialized
parts. The prefix shall be applied in the same manner as specified on the engineering drawing
for the part number unless otherwise specified in the contract or purchase order (see 6.2). In the
event that available space precludes application of the symbol as a prefix, the symbol shall be
applied as closely as possible to the serial number or Federal manufacturer code. In no case shall
the symbol be applied as a suffix to the serial number or Federal manufactures code.

4.4 Operator certification.

4.4.1 Cold spray operator. The cold spray operator shall demonstrate proficiency in the
operation of the cold spray equipment and in the performance of other related items by
successfully preparing and coating a set of qualification test panels and specimens as described
in 5.1.2 through 5.1.2.2.4. In the event an operator fails the test, the operator shall be permitted
to submit two more samples of the qualification test panels or specimens which failed to pass the
specified test. If any of the second set fail to conform to the specified acceptance requirements,
the operator shall be disqualified. If reexamination is still desired after failing to pass the second
set the operator shall be required to submit a complete series of qualification test panels and
specimens as specified in 5.1.2 through 5.1.2.2.4 after the operator receives the necessary
training in the process prior to being retested. In addition, the operator shall be required to
submit one additional set of the qualification test panels or specimens which resulted in the
initial disqualification. A cold spray operator of semiautomatic or automatic equipment shall
meet all the requirements of a manual spray operator.

4.4.1.1 Continuance of certification. The certification status of a cold spray operator may
be maintained by a continuous record of satisfactory proficiency or by the annual successful
preparation and coating of a set of test panels and specimens as described in 5.1.2.
Re-certification of a cold spray operator shall be required when there is evidence of a lack of
proficiency.

5. DETAILED REQUIREMENTS

5.1 General.

5.1.1 Certification. To ensure supplier capability to consistently deliver a satisfactory

product, the supplier facilities and general procedures shall be certified before parts for
production are supplied unless otherwise specified in the contract or purchase order (see 6.2). If
such certification is to be waived by the acquisition authority it must be specified in the contract
or purchase order.

5.1.1.1 Certification samples. The supplier shall submit test samples as specified in 5.1.2,
together with the sample parts required for examination by the acquisition authority. The
supplier shall apply the cold spray to the base metal combination as specified by the acquisition
authority. Sample parts submitted shall be prepared in accordance with 5.1.3.2.

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5.1.1.2 Re-certification. In the event a supplier has not supplied cold sprayed parts or
test specimens for over one year, the supplier shall be required to re-certify in a manner
equivalent to the original certification unless otherwise specified in the contract or purchase
order (see 6.2).

5.1.2 Test samples. A minimum of one panel for micro-examination and three bond
strength specimens shall be cold sprayed. The microscopic examination panels and bond
specimens shall be fabricated from the same materials as the parts to received the cold spray or
as specified by the acquisition authority.

5.1.2.1 Metallographic test specimens. Test panels shall be prepared as follows:

a. Size: Approximately 40 x 40 x 10 millimeters..

b. Material: Same as parts to receive the cold spray or as specified by the
acquisition authority.
c. Deposition Material: Specified by acquisition authority.
d. Deposition thickness: 0.2 to 0.3 millimeters unless otherwise specified in the
contract or purchase order (see 6.2).

5.1.2.1.1 Specimen configuration. Specimen configuration shall be specified in the

contract or purchase order (see 6.2) and shall require the approval of the procuring activity.

5.1.2.2 Bond strength specimens. The contract or purchase order (see 6.2) shall specify
the pass/fail criteria for an acceptable bond for the specific application and the bond strength
specimen shall be prepared as follows:

5.1.2.2.1 Size. Three specimens shall be prepared to the dimensions as specified in

ASTM C633. Other specimen configurations may be used providing written permission is
obtained from the acquisition authority, unless otherwise specified in the contract or purchase
order (see 6.2).

5.1.2.2.2 Material. One specimen of the selected alloy as specified in 5.1.2 and one
specimen of any suitable material for the uncoated end of the test specimen.

5.1.2.2.3 Deposit. The deposit shall be as specified by the acquisition authority (see 6.2).

NOTE: The uncoated specimen shall be suitably identified (e.g., slotted along the outside
diameter).

5.1.2.2.4 Deposition thickness. The deposition thickness shall be at least 0.4

millimeters, unless other specified in the contract or purchase order (see 6.2)..

5.1.3 Process approvals.

5.1.3.1 Processing data. Operation sheets covering the process shall be established for
each part number by the cold spray source. Figure 3 shows a typical operation sheet, the format

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is optional provided all pertinent information is provided. Processing procedures shall not be
dependent upon part function or the critical nature when in service. The engineering
requirements as specified on the drawing shall prevail during any acceptance testing.

5.1.3.2 Sample part. A sample part, or a simulated part shall be processed in accordance
with the procedure established in 5.1.3.1 and submitted to the acquisition authority for approval
prior to production parts being cold sprayed.

5.1.3.3 Rework. Discrepant parts with damaged or imperfect deposits shall be reworked
by a qualified source approved by the acquisition authority. The number of reworks will also be
an acquisition authority decision based on degree discrepancy and method of repair.

5.1.3.3.1 Stripping. Reworking to completely remove the defective coating is

permissible by minimally aggressive mechanical methods. Non-mechanical (chemical) stripping
shall be subject to approval by the acquisition authority.

5.1.3.4 Metallographic test sample. Metallographic test samples shall be prepared in

accordance with 5.1.2.1 and cold sprayed along with the first production lot of parts and each
subsequent lot (see 3.3) and submitted to the acquisition authority with the parts. If specified in
the contract or purchase order (see 6.2), the cold spray supplier may submit photomicrographs of
the coating in lieu of the test samples.

5.1.4 Process certification. Unless otherwise specified in the contract or purchase order
(see 6.2), the supplier shall furnish three copies of a certificate stating the following information:

a. Purchase order number.

b. Part number and revision letter.
c. Serial number of parts coated (when applicable).
d. Cold spray lot numbers.
e. Quantity and serial numbers of rejected parts stripped and
recoated.
f. Test results per 5.2.1 through 5.2.4.
g. Statement of conformance to this standards latest revision.

5.2 Test methods.

5.2.1 Visual. All parts and assemblies (before and after machining), test panels, and test
specimens, shall be visually inspected to verify that cold spray deposit is adherent to the
substrate material and has a uniform continuous surface free from spalling, chipping, flaking,
cracking, and other objectionable imperfections.

5.2.2 Micro examination. A microscopic examination of a specimen cut normal to the

coating surface shall not reveal any cracks, excessive or massive oxides or porosity when
examined at a magnification of 100x in accordance with the procedures outlined in ASTM E3
and ASTM E407. In accordance with ASTM E407 and the results desired, the cold spray deposit

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material shall determine the etchant number. The etchant composition and procedure shall be
determined from the corresponding etchant number.

5.2.3 Oxides and porosity. Excessive porosity shall be defined as not greater than 5
percent when viewed at 200x after etching. Excessive or massive oxides shall be defined as not
greater than 3 percent for coatings where oxygen is not an integral part of the material.
Examination of the part for oxides shall be at 100x after etching.

5.2.4 Bond strength test. A bond strength test specimen (see 5.1.2.2) shall be bonded
(glued) to an uncoated specimen to form a single test specimen and the test specimen shall be
tensile strength tested to verify conformance to the applicable coating material requirements as
per ASTM C633:

a. Remove masking materials.

b. Verify that bonding end of the uncoated section of the test specimen has been
cleaned, dried, and abrasive-blasted.
c. Apply a thermosetting epoxy adhesive to the bonding ends of the coated and
the uncoated sections of the test specimen.
d. Accurately align and join the ends of the two specimens.

NOTE: A fixture may be used to facilitate bonding of the test specimen.

e. Cure the adhesive in a hot air circulating oven at the temperature recommended
by the manufacturer.
f. After bonding, dress the edge of the coating flush with the outside diameter of
the test specimen.

NOTE: An abrasive disc or wheel may be used for this purpose but care shall be taken that the
disc or wheel moves parallel to the centerline of the test specimen. Care shall be taken during
dressing to ensure the temperature does not increase to affect the bond adhesion.

g. Test the bond specimen with a standard laboratory tensile tester equipped with
universal joint grips for each end of the joined specimens. Use a fixture
that assures uniaxial loading of the specimen. Set the no-load cross-head
speed at approximately 1 millimeter per minute.

6. NOTES

(This section contains information of a general or explanatory nature that may be helpful, but is
not mandatory.)

6.1 Intended use. This military standard is intended to ensure cold spray coating
operations on parts for military components meet prescribed requirements.

6.2 Acquisition requirements. Acquisition documents should specify the following:

a. Title, number, and date of the standard.

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 MIL-STD-3021

b. If the powder is to be controlled by a specification (see 4.2.2.2).

c. If a minimum accuracy is required on the instruments (see 4.3.1.1).
d. If the surfaces are to be pre-heated (see 4.3.4).
e. If the symbol to be applied is different (see 4.3.6).
f. How the prefix is to be applied for identification (see 4.3.6).
g. If the supplier’s facility and general procedures needs to be certified before
parts are supplied or waived (see 5.1.1).
h. The manner in which the supplier needs to re-certify (see 5.1.1.2).
i. If the coating thicknesses on the metallographic test specimens are different
(see 5.1.2.1).
j. Specify specimen configuration (see 5.1.2.1.1).
k. Specify the bond strength accept/reject criteria (see 5.1.2.2).
l. If other configurations can not be specified (see 5.1.2.2.1).
m. Specify coating material (see 5.1.2.2.3).
n. Specify coating thickness or range if different (see 5.1.2.2.4).
o. If photomicrographs can be submitted in lieu of the test samples (see 5.1.3.4).
p. If the supplier can state different information than that listed (see 5.1.4).

6.3 Issue of DoDISS. When this standard is used in acquisition, the applicable issue of
the DoDISS must be cited in the solicitation (see 2.2.1 and 2.2.2).

6.4 Safety. Use of cold spray equipment involves exposure to certain safety hazards,
such as, pressurized gases and metal powders. Guidelines for the handling of these substances is
found in OSHA Safety and Health Standards (29 CFR 1910), General Industry.

6.4.1 Material safety data sheets (MSDS). The contracting activity should be provided a
material safety data sheet for each part at the time of contract award. The MSDS should be
provided in accordance with OSHA section 1910.1200, 29 CFR Chapter XVII and found as part of
FED-STD-313. OSHA section 1910.1200 requires reporting threshold criteria for known or
suspected human carcinogens on MSDS 0.1 percent or greater, and 1 percent or greater for other
health hazards. The MSDS should be included with each unit of issue of material covered by the
specification, when specified. Contracting officers will identify those activities requiring copies of
completed material safety data sheets prepared in accordance with FED-STD-313. The pertinent
Government mailing addresses for submission of data are listed in FED-STD-313.

6.5 English units. When English divisions are required, units for meter, kilogram, meter
per second, and mega Pascal may be converted to the English equivalent by multiplying them by
the following conversion factors:
Metric SI unit Multiply by Equals English
meter (m) 39.37 = inch
meter (m) 3.28 = foot
kilogram (kg) 2.205 = pound
meter per second (m/s) 3.2808 = feet/sec
mega Pascal (MPa) 145.038 = pounds/sq. inch

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6.6 Subject term (key word) listing.

Adhesion
Coating
Cohesion
Cold gas dynamic spray
High velocity powder
Impaction process
Kinetic energy metallization
Kinetic spraying
Particles
Powder
Propelling gas
Thermal spray

CONCLUDING MATERIAL

Custodian: Preparing activity:

Army - MR Army - MR
Navy - AS
Air Force - 11 Project MFFP-2007-006

Review activities:
Army – AV, PT
Navy – EC, MC, NP, SH
Air Force – 19, 84, 99
DLA- DH, GS4

NOTE: The activities listed above were interested in this document as of the date of this
document. Since organizations and responsibilities can change, you should verify the currency
of the information above using the ASSIST Online database at http://assist.daps.dla.mil/.

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