Low Hydrogen Embrittlement (LHE) Zinc-Nickel (Zn-Ni

Low Hydrogen Embrittlement (LHE) Zinc-Nickel (Zn-Ni)

Qualification Test Result and Process Parameters

Development

Dave Frederick, USAFCraig Pessetto, ES3

Steve Gaydos, Boeing

9 February 2011

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4. TITLE AND SUBTITLE Low Hydrogen Embrittlement (LHE) Zinc-Nickel (Zn-Ni) QualificationTest Result and Process Parameters Development

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Technical Objectives

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•

Small Business Innovative Research (SBIR) Phase I Feasibility Study•

The specific technical objectives of the SBIR Phase II effort are as follows:▪

Successfully pass the following performance parameters, using a prototype tank installation:

•

Installation of a prototype tank for plating demonstration on test coupons and full size components

•

Adhesion•

Hydrogen Embrittlement•

Re-embrittlement•

Liquid and Solid Metal Embrittlement (LME/SME)•

Fatigue•

Corrosion•

Brush Plating for repair of damaged LHE Zn-Ni coatings (Touch Up)•

Torque Tension •

Review requirements for Non Destructive Inspection (NDI)•

Optimize conversion coating•

Option 1: Develop an accelerated hydrogen embrittlement test procedure :

Prototype Tank Implementation

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▪

ES3 implemented a tank of approximately 325 gallons for the purpose of demonstrating the LHE Zn-Ni plating process on some full sized gear components

▪

The demonstration tank was used to develop uniform plating thicknesses and process parameters on test coupons and full scale landing gear components

▪

During the plating operations Quality Assurance testing has been conducted to ensure the alkaline LHE Zn-Ni solution is within proper process limits

Dipsol IZ-C17+ LHE Zn-Ni Plating Tank

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Tri-Chromium Conversion Coat Tank

Prototype Tank ImplementationI[~&~

ES3

5

Bend to Break Adhesion Test Coupons

•

Adhesion of the LHE Zn-Ni coating to the substrate was tested per ASTM B571

•

All adhesion test coupons were manufactured from 1”x 4”x 0.040”

4130 steel sheet

•

Results: All Test coupons passed

Adhesion Test Coupons

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Dipsol™ LHE Zn-Ni Test Panels After Dry and Wet Tape Adhesion Test of Primer

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Deft 44-GN-072

J

Wet Dry Wet

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Dry and Wet Paint Adhesion Test Results per ASTM D3359

I[~&~

ES3

Scribed Dl'Y and Wet Tape Adhesicm Test Results

4'' x 6" x 0.040" 4130 Steel Sub~tr:ate

DRY TAPE AOH.E!I~ WET TJ!I>E ADHES!ION

PERCENTAGE

P·P~NEJL liD PRETREATMENT COA.TitfG OOATII'IG REMOVED

1 0

2 LJ-lEZn-Ni

0 Plaling

3 Deft

0

44-GN-72 1

Cdl Plated wf 0

2 Hex Or

0 Conversion

3 Coaling

0

4 0

5 LJ-lE Z rr-Ni

0 Pla'ling

6 Deft

0

44-GN-008 0 4

Cdl Plated wf

5 Hex Or

0 Conversion

6 Coaling

0

Panels iiTil'IEf'5ed in cis'llled wat:r at room tempet<XLJ"e for .24 holi"S. [1} ASTM D 335Q Criteria:

5A- No peEling or removal ~A -Trace peefrlg1 or rEmOval along incisions

3A-Jagged remoYal along incisions~ to 1118 inch on a1her side 2A-Jagged remoYal along llllOst af incisiions up to 118 PCh on either side 1 A- RermYal from most ci !he area of 1lle "X' under lfle tape OA- RermYal beymd the .¥ea~ ci the "X"

[2} The primEf' sha'll show no a!liesim failure.

AS.TM, Pass r PERCENTAGE ASTM D$353 Fall COAHiiG D 3353

I' I [21 REMOVED Il l

5A Pass 0 4A

5A Pass 2 4A

5A Pass 0 5A

5A Pass 0 5A

5A Pass 0 5A

5A Pass 0 5A

5A Pass 0 5A

5A Pass 0 5A

5A Pass 10 4A

5A Pass 0 5A

5A Pass 0 5A

5A Pass 0 5A

Pass r Fall PI

Pass

Fail

Pass

Pass

Pass

Pass

Pass

Pass

Fail

Pass

Pass

Pass

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LHE Zn-Ni Hydrogen Embrittlement Testing

•

Coupons manufactured per ASTM F519 specifications (4340)

•

Coupons plated and tested 28th

April, 2009 upon initial installment of LHE Zn-Ni demonstration tank

•

Additional coupons plated and tested at additional dates

•

All coupons tested per ASTM F519 and passed the 200 hour sustained load tests @ 75% of the tensile notch fracture strength

ASTM F519 Type 1A.1 Test Coupons

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Cad Plated in Bldg 505 for 5 mins - 200x

9

HE Plated Cross Section

.772 mils

.274 mils

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LHE Zn-Ni Plated @ 40 ASF for 20 mins - 200x

10

HE Plated Cross Section

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LHE Zn-Ni Re-Embrittlement Testing Machine

LHE Zn-Ni Hydrogen Re-Embrittlement Testing

I[~&~

ES3

12

Re-Embrittlement results: •Coupons tested by an ISO 9001 certified facility. Coupons tested

IAW ASTM F519. The coupons tested immersed in solutions of Water, 3.5% Salt Water, Dilute* Calla 296, Dilute* Calla 602LF, Concentrated Calla 296, and Concentrated Calla 602LF.*NOTE –

Dilute means mix cleaning solution to manufacturer’s recommended use concentration and heat to manufacturer’s maximum recommended use temperature.

• Cleaning solutions used in testing were:Calla 296Calla 602LF

• LHE Zn-Ni performs better than IVD and as well as Cad

Re Embrittlement Test Matrix

Plating

Test Solution

Distilled Water @ Room Temp

Tested 45% NFS for 150Hrs

3.5% Salt Water @ Room Temp

Tested 45% NFS for 150Hrs

Dwg 9825019* Diluted Calla 296 @ Max Temp 180

°F Tested 75% NFS for 200Hrs

Dwg 9825019* Diluted Calla 602 LF Max Temp 160

°F Tested 75% NFS for 200Hrs

Concentrated Calla 296 @ Room Temp tested 45% NFS for 150Hrs

Concentrated Calla 602LF @ Room Temp

tested 45% NFS for 150Hrs

LHE Zn-Ni Pass Failed Pass Pass Pass PassCadmium Pass Failed Pass Pass Pass Pass

IVD Failed Failed Not Tested Not Tested Not Tested Not Tested

*The specimens were immersed in the cleaning compound at the manufacturer's maximum recommended temperature, and appropriate cleaning concentration, for 30 minutes. Removed. Air dried and loaded to 75% NFS for 200Hrs.

LHE Zn-Ni Hydrogen Re-Embrittlement Testing

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Liquid/Solid Embrittlement Testing

•

Liquid and Solid Metal Embrittlement (LME and SME) occur when one metal, either as a liquid or solid, intrudes into the structure of another, potentially causing embrittlement in the base metal

•

Melting points for the coating metals are as follows: ▪

Cadmium ~610°F▪

Zinc ~787°F▪

Nickel ~2650°F

Temp/NFS Material LHE Zn-Ni200Hr

Cad200Hr

LHE Zn-Ni Step Load

Cad Step Load

600F/85% 300M Pass Fail 100% NFS -N/A-500F/85% 300M Pass Fail 100% NFS 87% NFS400F/85% 300M Pass Fail 100% NFS 91% NFS400F/75% 300M Pass Fail 100% NFS 81% NFS

14

LHE Zn-Ni and Cad Type 1a.1 Specimens After ISL Test to Determine the NFS After Exposure to 400oF for 200 Hours

Liquid/Solid Metal Embrittlement Testing

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Fatigue Testing

•

Phase II LHE Zn-Ni fatigue testing is an extension of Phase I work

•

Phase II LHE Zn-Ni fatigue testing continues to broaden the data base and increase the statistical validity of the data

•

Manufacturing of coupons and Fatigue Testing IAW ASTM E466▪

All coupons were plated per manufacture’s plating solution limits

16

Phase I Fatigue Testing (Shotpeened Coupons)

C-17 P2 Program Fatigue Data (2005) (IZ-C17 with Hex conversion coating)

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Phase II Fatigue TestingI[~&~

ES3

t

~~ Stress Loads (KSI) R= -0.3 Total Shotpeened Coupons 160 180 200 Quantity

Bare 5 5 5 15 Cad Plated 5 5 5 15

~n-Ni Plated Tri Chrome 5 5 5 15 ~n-Ni Plated Hex Chrome 5 5 5 15 ~Zn·Ni Plated Atotech Tri Chrome 5 5 5 15

~n-Ni Plated Atotech Hex Chrome 5 5 5 15

Total Fatigue Coupons 90

fk Bake before Tri CC

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Phase II Fatigue TestingI[~&~

ES3

210

200

190

180

Test load (KSI)

R= -0.3

170

160

150 10,000

I

I

Peened Fatigue Coupon Test Results

I I I I I I I I

,., ... ... - TIT

_, ... L , ... 1'*, ...- - - --- I ·- - - - --j

I

._ - .I - - I ...;_ l l -- ---1 -- ,- ~ ~ -·- 1- ·-

I I I I I I I I 100,000 1,000,000

Number of Cycles

+ Bare • cad .AZn-Ni Tri CC (Dipsol) e zn-Ni Hex CC (Dipsol) .A Zn-Ni Tri CC (Atotech) e zn-Ni Hex CC (Atotech)

Phase II Fatigue Testing

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I[~&~

ES3

Means Compared@ 95% limits: 200 ksi Peened I I I I I I

70542 bare r-

33104 Cad r- -

26275 ZnNi3 r-

. ,-... -. .......

30496 ZnNi6 r- -

33482 Atot3 r- -

31037 Atot6 r- -.......

I I I I I I

1 2 3 4 5 6 7 8 The means of groups Cad and bare are significantly different x 104


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I[~&~

ES3

Means Compared@ 95% limits: 180 ksi Peened

170644 bare

160097 Cad

70904 ZnNi3

100406 ZnNi6

110794 Atot3

112736 Atot6

0 0.5 1 1.5 2 2.5 No groups have means significantly different from Cad x 1 0o


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I[~&~

ES3

Means Compared@ 95% limits: 160 ksi Peened

661968 bare

746212 Cad

748266 ZnNi3

624663 ZnNi6

581027 Atot3

476921 Atot6

1 2 3 4 5 6 7 8 9 10 11 No groups have means significantly different from Cad x 1 0o

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Corrosion Performance

•

Corrosion tests were conducted on LHE Zn-Ni coupons with cadmium as the baseline

•

Testing was also performed on both cadmium and LHE Zn-Ni coated coupons with a prime/paint topcoat after being scribed (See Table below). All test coupons were 4”x 6”x 0.040”

4130 steel sheet•

All testing was performed per ASTM B117•

Test specimens were both scribed and un-scribed

# of steel Panels Plating Scribed Prime/Paint

3 LHE Zn-Ni Yes No

3 LHE Zn-Ni No No

3 Cd Yes No

3 Cd No No

3 LHE Zn-Ni Yes Yes

3 Cd Yes Yes

Corrosion Test Matrix

Cadmium Coatings – Phase II ASTM B 117 Panels @ Boeing Unscribed)

Cad

miu

m w

ith H

exav

alen

tChr

ome

Con

vers

ion

Coa

ting

Uns

crib

ed–

AST

M B

117

Figu

re 3

Test Panel Removed From

Salt Spray Cabinet –Excess Amount

of Red Rust Detected













1000 hours

3000 hours

5000 hours










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Zinc Nickel Coatings – Phase II ASTM B 117 Panels @ Boeing (Unscribed)

1000 hours

3000 hours

5000 hours

IZ-C

17+

Zn-N

i with

Triv

alen

t Chr

ome

Con

vers

ion

Coa

ting

Uns

crib

ed–

AS

TM B

117

Fi

gure

4

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Cadmium Coatings – Phase II ASTM B 117 Panels @ Boeing (Scribed)
















1000 hours

3000 hours

5000 hours

Cad

miu

m w

ith H

exav

alen

tChr

ome

Con

vers

ion

Coa

ting

Scr

ibed

–A

STM

B 1

17Fi

gure

5










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Zinc Nickel Coatings – Phase II ASTM B 117 Panels @ Boeing (Scribed)

1000 hours

3000 hours

5000 hours

IZ-C

17+

Zn-N

i with

Triv

alen

t Chr

ome

Con

vers

ion

Coa

ting

Scr

ibed

–AS

TM B

117

Figu

re 6

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Cadmium Coatings – Phase II ASTM B 117 Panels @ Boeing (Painted/Scribed)













1000 hours

3000 hours

5000 hours

Cad

miu

m w

ith H

exav

alen

tChr

ome

Con

vers

ion

Coa

ting

Scr

ibed

Pai

nted

–A

STM

B 1

17Fi

gure

9










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Zinc Nickel Coatings – Phase II ASTM B 117 Panels @ Boeing (Painted/Scribed)

1000 hours

3000 hours

5000 hours

IZ-C

17+

Zn-N

i with

Triv

alen

t Chr

ome

Con

vers

ion

Coa

ting

Scr

ibed

Pai

nted

–A

STM

B 1

17Fi

gure

10




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G 85 SO2 Corrosion-Cad

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I[~&~

ES3

120 hours

168 hours

336 hours

G 85 SO2 Corrosion-LHE Zn-Ni

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I[~&~

ES3

120 hours

168 hours

336 hours

Brush Plating Repair

•

In order for a brush LHE Zn-Ni plating to qualify it must pass the following tests:▪

Hydrogen Embrittlement (HE) testing per ASTM F519

▪

Bend to break adhesion test per ASTM B571▪

Corrosion testing per ASTM B117•

SIFCO recommended procedures were used to plate several sets of HE type 1a.1 coupons, adhesion coupons, and corrosion coupons, using SIFCO 4018 No Bake LHE Zn-Ni brush plating solution

•

Test Results Summary:▪

Passed HE testing▪

Passed adhesion testing on steel and LHE Zn-Ni plated steel

▪

Corrosion test performance is excellent


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Torque Tension

•

Robins AFB Cad plating replacement on threaded fastener and components▪

Typical chart for run on –

break away test showing Cad vs. LHE Alkaline Zn-Ni

32

Typical Run-On & Breakaway Torque - Cad Bare

-80

-60

-40

-20

0

20

40

60

80

-2500 -2000 -1500 -1000 -500 0

Rotation Degree

Torq

ue (I

N-L

B)

Run 0

Run 1

Run 2

Run 3

Run 4

Typical Run-On & Breakaway Torque - Zn-Ni Bare

-80

-60

-40

-20

0

20

40

60

80

-2500 -2000 -1500 -1000 -500 0

Rotation Degree

Torq

ue (I

N-L

B)

Torque Tension

•

Robins AFB Cad plating replacement on threaded fastener and components▪

Typical chart for Torque Tension Test showing Cad vs. LHE Alkaline Zn-Ni with MIL-PRF-83483 Anti-seize grease lubricant

33

Typical Torque Tension - Cad w/ Anti-Seize Grease

0

2000

4000

6000

8000

10000

12000

0 5 10 15 20 25 30 35 40

Applied Torque (FT-LB)

Tens

ile L

oad

(LB

)

Run 0

Run 1

Run 2

Run 3

Run 4

Typical Torque Tension - Zn-Ni w / Anti-Seize Grease

0

2000

4000

6000

8000

10000

12000

0 5 10 15 20 25 30 35 40

Applied Torque (FT-LB)

Tens

ile L

oad

(LB

)

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Non-Destructive Inspection (NDI)

•

OSHA Permissible Exposure Limits (PELs) for LHE Zn-Ni are high enough, such that, the LHE Zn-Ni plating does not have to be removed during the overhaul process (currently all cadmium plated landing gear components which come into the overhaul facility are stripped and cleaned per OSHA PELs)

•

There is no NDI interference due to the LHE Zn-Ni coating itself, consequently we can do the following inspections without

removing the LHE Zn-Ni coating:▪

Fluorescence Magnetic Particle Inspection (FMPI)▪

Ultra Sonic Inspection▪

Eddy current▪

X-Ray

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Conversion Coating Optimization

•

Testing was conducted to determine the optimal conversion coating (CC) (Hexavalent vs. Trivalent) and parameters:▪

Baking before and after conversion coating•

Hexavalent CC: must be applied after bake•

Trivalent CC: can be applied before or after bake (process time savings)

▪

Paint adhesion performance per ASTM D3359•

Hex-CC –

Passed•

Tri-CC –

Passed▪

Corrosion performance per ASTM B117•

Hex-CC –

Passed•

Tri-CC –

Passed (performs slightly better)▪

Hydrogen embrittlement per ASTM F519•

Hex-CC –

Passed•

Tri-CC –

Passed

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Conversion Coating Optimization

▪

Fatigue Performance per ASTM E466•

Hex-CC –

Passed •

Tri-CC –

Passed▪

Process parameters•

Submerge in conversion coat solution for 1–2 minutes▪

Environmental concerns•

DoD is currently trying to eliminate Hex-CC use

•

Recommend Trivalent CC

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Development of an Accelerated HE Test

•

Accelerated HE Test Development▪

Necessary to production process▪

Accelerated results in < 24 hours▪

Must correlate to 200 hour test•

Three rapid hydrogen embrittlement test methods have been identified for potential use at Hill AFB▪

The Messier-Dowty 16 Hour Hydrogen Embrittlement Test

▪

ASTM F 1940 Rapid Hydrogen Embrittlement Test for High Strength Steel Fasteners

▪

ASTM F 1624 –

09 Determination of Hydrogen Embrittlement Threshold Using the ISL (Incremental Step Load) Test Method Rising Step Load Apparatus

•

The preferred method to carry out a rapid hydrogen embrittlement test is ASTM F1624 which is as follows:▪

Using the incremental test method in ASTM F 1624, determine the NFSF1624

for new –

unplated ASTM F 519 Type 1a.1 test specimens. NFSF1624

will be lower than NFSE8

▪

Qualified rapid hydrogen embrittlement test method (< 20 hrs):

•

Load Type 1a.1 test specimen in Rising Step Load machine and perform step load using ISL conditions (20,5,1) = (20 steps, 5% NFSF1624

per step, hold for 1 hour at each step). Determine load where test specimen breaks, this is threshold load Pth

•

%NFS = 100 x Pth

/ NFSF1624

•

If %NFS >

90% then process is non-

embrittling

38

Rising Step Load Apparatus

Development of an Accelerated HE Test

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Phase III - Efforts

•

Phase III –

tasks consisted of the following:▪

Waste stream characterization and mitigation•

Similar wastewater treatment as cadmium▪

Permitting for hazardous material•

New source sheets ready to submit•

Awaiting finalization of the LHE Zn-Ni plating line (i.e. tank size and location)•

Will apply for Title V air permit when the LHE Zn-Ni plating line is installed▪

Process validation▪

Specification and source control drawings▪

Prototype depot LHE Zn-Ni process line•

With landing gear components▪

Process orders and Process Orders Document and Display System (PODDS) support

▪

Engineering and Program Management Support

•

Critical LHE Zn-Ni process parameters were established for the following:▪

Type of Anode•

Nickel 200▪

Plating fixtures•

Fixture material can be either stainless (prefered) or carbon steel▪

Current density•

40–60 Amps per square foot (ASF)▪

Plating time•

10–20 minutes▪

Plating thickness and type of conversion coating•

Class▫

I –

minimum of 0.0005”

~ (40 ASF for 20 minutes)▫

II –

minimum of 0.0003”

~ (40 ASF for 13 minutes)▫

III –

0.0001 –

0.0002”

~ (40 ASF for 10 minutes)•

Type▫

I –

No conversion coat▫

II –

Trivalent or Hexavalent conversion coat

40

Process Validation Plan

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•

Critical LHE Zn-Ni process parameters were established for the following:▪

Bath chemistry•

Requires bi-weekly chemical analysis of the LHE Zn-Ni plating tank using titration

▫

Zinc▫

Nickel▫

Carbonate▫

Sodium Hydroxide•

Requires bi-weekly chemical analysis of the Trivalent CC tank:▫

pH level▫

Cr level •

Requires quarterly chemical analysis for trace contamination metals for both tanks

▪

Agitation requirements•

Agitation should be sufficient enough to re-circulate the tanks plating solution a minimum of 3 times per hour

•

No air agitation

41


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▪

Tank chemical maintenance•

Chemical maintenance for the LHE Zn-Ni process is based on usage and production rates

•

Analysis and adjustment should be performed on an amp-hour used basis, or on a weekly basis

•

Some degree of tracking will be required to establish a historical database of information, which can then be used to recommend regular analysis intervals

•

Specific limits and analysis instructions are provided in the LHE Zn-Ni specification drawing

▪

Effects of precipitation (carbonate) build up•

Carbonate formation will decrease the plating efficiency, and perhaps the adhesion performance

•

The best solution is to continually treat out carbonates rather than batch treat in the winter and deal with cyclic carbonate levels and larger replenishment additions

•

A Carbolux™

system is recommended for treatment of the carbonates▫

It is a mechanism which continually removes solution, precipitates out carbonates, places them in a disposal hopper, and then returns the treated solution back to the plating tank

42


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1669 E. 1400 S ●

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▪

Quality compliance testing•

The following monthly compliance testing is required:▫

Bend to break adhesion coupons per ASTM B571 on plated 1”x 4”x 0.040”

coupons (4ea)

▫

Neutral salt spray corrosion testing per ASTM B117 on plated 4”x 6”

coupons (2ea)▫

Hydrogen embrittlement testing per ASTM F519 on plated Type 1.a1

coupons (4ea)

43


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1669 E. 1400 S ●

Clearfield, UT 84015 (801) 926-1150 ●

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1669 E. 1400 S ●

Clearfield, UT 84015 (801) 926-1150 ●

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Phase III Effort Prototype Process Line

Prototype Part MatrixComponent Part #C-5 MLG Stop Plate 4G11453-101B

F-15 MLG Outer Cylinder 68A412702-1001/1002

B-1 MLG Axle 1881B85

F-15 MLG Lower Drag Brace 68A410792-2001

A-10 MLG Torque Arm 19046-1

F-16 NLG Inner Cylinder 2007644-103

C-5 MLG Rotation Collar 4G13565-101A/-101B

A-10 NLG Axle 18800-3

Phase III Effort Prototype Parts

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A-10 NLG Axle A-10 MLG Torque Arm


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B-1B MLG Axle C-5 MLG Rotation Collar


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F-15 MLG Cylinder F-16 NLG Inner Cylinder F-15 MLG Lower Drag Brace

Phase III Effort Prototype Anode Design

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C-5 MLG Rotation Collar

Plating B-1 Bushings LHE Zn-Ni Plated LHE Zn-Ni B-1 Bushings

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Phase III Effort Prototype B-1 Bushing

50

Phase III Effort Proposed Prototype Plating Line

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I[~&~

ES3

5 I 4 I 3 I 2 I 1 REVISIONS

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ES3

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WARNING THIS DOCUMENT CONTAINS TECHNICAL DATA WHOSE EXPORT IS RESTRICTED BY THE ARMS EXPORT CONTROL ACT (T ITLE 22, U.S.C. SEC 2571 EJ SEQ.) OR EXECUT)VE ORDER 12470. VIOLATIONS OF THESE EXPORT LAWS ARE SUBJECT TO SEVERE CRIMINAl PENALTIES. DISSEMINATION OF THIS DOCUMENT IS CONTROLLED UNo~ DOD DIRECTIVE 5230.25 AND AFI 61-204.

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1669 E. 1400 S ●

Clearfield, UT 84015 (801) 926-1150 ●

fax (801) 926-1155

I[~&~

ES3

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WARNING THIS DOCUMENT CONTAINS TECHNICAL DATA WHOSE EXPORT IS RESTRICTED BY THE ARMS EXPORT CONTROL ACT (TITLE 22, U.S.C. SEC 2571 ET SEO.) OR EXECUl)VE ORDER 12470. VIOLATIONS OF THESE EXPORT LAWS ARE SUBJECT TO SEVERE CRIMINAL PENALTIES. DISSEMINATION OF THIS DOCUMENT IS CONTROlLED UNO~ DOD DIRECTIVE 5230.25 AND AFt 61-204.

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QuestionsI[~&~

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Documents

Low Hydrogen Embrittlement (LHE) Zinc-Nickel (Zn-Ni