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topic 45728

How to eliminate powdery condition of Alodine 1200S


A discussion started in 2007 but continuing through 2018

(2007)

Q. Hello!

I have chemical conversion coating process with Alodine 1200S.
I want to correct of powdery coating condition on my parts since a month ago (at that time I¡¯ve dumped and recharged my Alodine bath totally).
In my processing, small parts are free from powder and show very beautiful appearance, but unusually, big skins (which is aluminum 2524-T3 Clad, 4.8 by 1.8 m big) show powdery condition.
At this time the pH is 1.44 (1.3~1.8 control) and the concentration is 2.12 oz/gal (1.2~2.8 control).

I want to make sure what kinds of variables are affected to powdery condition and how can I solve this problem.
Thanks in advance.

D.Y.YOO
ENGINEER - BUSAN, KOREA


simultaneous (2007)

A. Get the 'Technical Process Bulletin' for Alodine® 1200S, available from its manufacturer, Henkel. Your concentration is 2x the usual upper limit. From page 3:

"If the ALODINE coating is powdery, the cause may be one or more of the following:

A. The work has been improperly cleaned and/or rinsed.
B. The concentration of the ALODINE coating chemical(s) in the bath is too high.
C. The ALODINE 1200S bath has become contaminated with phosphates, sulfates, chlorides, or some other contaminant (analysis required).
D. The coating time is too long.
E. The bath temperature is too high.
F. The Free Acid of the DEOXYLYTE final rinse is too high (should not exceed 7.0)
G. The pH of the bath is too low for the concentration selected."

Your solution parameters (low pH, excessively high concentration) probably have greatly accelerated the coating rate. This makes it difficult to immerse and remove large parts with any expectation of a uniform coating top-to-bottom. The cladding is high purity aluminum (99.3%) which must coat very rapidly in your conditions.

Try using a pH 1.65-1.70 & a concentration of 0.95-1.05 oz(wt)/gallon [store 1/2 the solution in clean polyethylene drums for future make-up]. Also, the bath life is greatly increased by using DI water for rinsing prior to the ALODINE bath and for solution make-up.

Ken Vlach
- Goleta, California
contributor of the year

Finishing.com honored Ken for his countless carefully
researched responses. He passed away May 14, 2015.
Rest in peace, Ken. Thank you for your hard work
which the finishing world continues to benefit from.



(2007)

A. Do not know your process, just talk in general:
1. do not caustic etch 2xxx alloys;
2. pH is better at 1.6-1.8
3. immediate spray rinsing after Alodining followed by immersion rinsing with manual agitation (less than 30 sec.)

John Hu
- Singapore


(2007)

A. First be sure you are using a mixed acid deoxidizer on that high copper alloy.

Raise the pH to 1.8 with ammonium hydroxide, and that will slow the reaction then lower the concentration to 1.8 oz/gal and that will slow the reaction, then the coating will not "powder".

robert probert
Robert H Probert
Robert H Probert Technical Services
supporting advertiser
Garner, North Carolina
Editor's note: Mr. Probert is the author of Aluminum How-To / Aluminio El Como



August 5, 2012 -- this entry appended to this thread by editor in lieu of spawning a duplicative thread

Q. Dear Sir,

How come aluminum parts sometimes come out with powder presence when Alodine 1200s is applied (immersion process)? Does it have to do with the immersion duration time?

Regards!

BEATRIZ ENRIQUEZ
- Chihuahua, Mexico


August 7, 2012

A. Hi Beatriz.

As you can see, a similar question was asked and answered in the past, so we appended your inquiry to that thread. If you have remaining issues after reviewing this, I'd bet that Robert Probert [a finishing.com supporting advertiser] can help. Good luck.

Regards,

Ted Mooney, finishing.com Teds signature
Ted Mooney, P.E.
finishing.com
Pine Beach, New Jersey



October 9, 2017 -- this entry appended to this thread by editor in lieu of spawning a duplicative thread

Q. Alodine 1200S is running 1.08 oz/gal. and 1.55 pH and 6061-T6 test panels are coming out a little powdery (parts are looking good). Could it be because of the test panels or is my concentration and pH off?

Clay Cheatham
- Magnolia, Arkansas, USA


October 10, 2017

A. Try a new deox in a bucket AND review the calibration of the pH meter, especially at that low pH.

robert probert
Robert H Probert
Robert H Probert Technical Services
Garner, North Carolina


October 11, 2017

A. Clay

I believe your pH may be the cause. Take a bucket of the Alodine and incrementally bump the pH to see what works. We have found better results at the higher end of the pH limit.

Willie Alexander
- Green Mountain Falls, Colorado



Troubles with Alodine 1200s

May 22, 2018

Q. Good Morning!

Summary of Problems: Inconsistent coating, Salt Spray Failure, Powdery Finish, Clear Finish, Finish bouncing back and forth between extremes when troubleshooting or changing parameters.

I have read as many discussions on this topic as I could, tried everything I could, to no avail. Here I am, please bear with me as this will be a long post with many details!

As a history, our company moved into a new facility in February, and switched proprietary brands from Iridite 14-2 to Alodine 1200S at that time, to open doors for Boeing Accreditation on Chemical Conversion coating. I had the Iridite 14-2 dialed in perfectly at the last shop. Perfect Salt Spray results (on 2024-T3), and a stable composition/maintenance schedule.

From day 1 of Alodine, we have experienced issues all over the board.

-10/26/17: Initial Bath makeup of 2.058 oz/Gal (Boeing guidelines recommend 1-3 oz/Gal for Alodine 1200s immersion, Henkel recommends 1.0 oz/Gal for immersion, 2.0 for brush application) (Bath sat unused until January 2018)
Initial Salt Spray results qualified us at a 15 second immersion for Class 3 coatings (electrical conductivity) and a 45 second immersion for Class 1A (maximum corrosion protection).
Coatings were spotty with runs/sagging colors, non-uniform appearance, some alloys powdered or didn't take coating at all, etc... pH fluctuated between 1.4-1.7.
We tried etching, no etching, deox, no deox, short immersions, long immersions, higher temperatures, lower temperatures, high pH, lower pH, etc...
Re-read the technical data sheet and decided to cut the concentration of the bath.

-2/26/2018: Bath Cut to reduce concentration to 1.33 oz/Gal. pH of 1.6, set point of 75 °F.

-3/5/2018: Initial Salt Spray Failure @ 1 minute processing. (pH of 1.8 that day)
We seemed to dial in the visual appearance for a few weeks, though Salt Spray had failed.
Panels and parts looked pretty good for a while, but still issues with inconsistent visual coating. Very spotty, some areas look clear, others are iridescent gold/orange/pink.
Then slowly the coating lost coloration until all parts ran were almost clear (including our Salt Spray panels).
-4/3/2018: Replacement Salt Spray Failure @ 3 minutes processing. pH of 1.5, 1.29 oz/Gal.
-4/3/2018: April Salt Spray panels Failed at the same parameters as the replacement test.
-5/3/2018: Upon receipt of the April failure notification, we immediately dumped the bath and rebuilt @ 1.28oz/Gal. 1.6 pH, and management mandated constant air agitation in the gold chem tank, unless parts were being ran. We proved with our previous proprietary gold chem that that was incredibly detrimental to coatings, but if we didn't agitate at all, we would slowly lose color in the gold chem coatings. We ran tests and narrowed down an air agitation schedule that worked to retain the color of the coating, but did not cause dark powdery coatings. This schedule was Monday, Wednesday, and Friday mornings for 1 hour.
Since management mandated the constant agitation, we have since had dark powdery coatings that wipe off or are removed with tape during the masking process.
(I would also like to note here that we do not wait 24 hours for the gel to cure prior to masking parts)
-5/17/2018: I provided Management with my failure investigations, which discussed Silica contamination in our tank. Between finding silicone plugs in the tank during the rebuild, we have been etching/deoxing a lot of Cast Aluminum parts lately. Testing showed 44 ppm of SiO2 in our Chemfilm bath. (I sent out a sample of the original bath alongside the new bath built on 5/3. New bath tested at 33 ppm of SiO2.) After this information we scheduled an immediate rebuild of the brand new tank...
-5/19/2018: Dump of tank, scrubbed out the tank with dilute NaOH & red abrasive pads, much rinsing, and rebuild.
-5/21/2018: Powdery coatings rubbing off, tape pulling coating off, etc... Waiting on results from SiO2 testing of this new New bath, plus our incoming tap water.
-5/22/2018: The panels ran last night by our swing shift that the coating was 'wiping off' of, and are now set, and will not wipe off.

Our Process:
Alkaline Clean: ~140 °F, ≥ 9.5pH, 17oz/Gal
Spray Rinse (pulled from Immersion Rinse next to it)
Immersion Rinse
Alkaline Etch (used only when required): 4.0 oz/Gal, Pre-penetrant/Boeing regulated parameters. 99 ° F.
Spray Rinse (pulled from Immersion Rinse next to it)
Immersion Rinse
Nitric/Iron based Deoxidizer: <1.0 pH, 50 g/L Fe2SO4 content, 34 g/L Nitric content. Cu content of <0.4 g/L (Usually sits at 0.026 g/L) 80 °F
Spray Rinse (pulled from Immersion Rinse next to it)
Stage 2 Counter flow Immersion Rinse
Stage 1 Counter flow Immersion Rinse
Alodine 1200s: 2-4 minute immersion, 1.6-1.7pH, 1.3 oz/Gal, 80 °F.
Spray Rinse (pulled from immersion next to it)
Ambient Immersion rinse: 3-5 minute immersion

I am about to drop the temperature, raise the pH, stop agitating the tank constantly, and see where that gets us.
Any insight or suggestions on what else I can do would be very much welcome!!

Kai Gussman
Lab Manager - Arlington, Washington, USA


May 22, 2018

A. 1. Look at the panels with a 10X loop before you process.

2. Review the reliability of your pH measurements, sounds like you are constantly too low - causes wipe off.

3. Be sure the ferric sulfate deox is air agitated to keep it re-oxed back up from ferrous to ferric.

4. Has the soil changed, is it waxy, parafinic, maybe you are not cleaning.

There should be no difference in results Alodine versus Iridite.

robert probert
Robert H Probert
Robert H Probert Technical Services
Garner, North Carolina


simultaneous May 23, 2018

thumbs up sign Thank you for your response!

1. I previously examined the panels with a 10x loop and I did find atmospheric pitting in the graining on the 2024-T3. We ordered new material with the plastic covering. We then ran the old material and the new material under the same parameters but on different days, and sent both for Salt Spray testing. At that time, the New material Failed, and the Old material (with the pitting) Passed!! Still stumped on that one, unless it was a completely different issue.

2. We use a three point pH verification; 1.07, 4.65, and 9.23 with a temperature considered pH meter. We calibrate the meter daily before use, and re-calibrate or re-verify if a reading seems off.

3. We continuously agitate the air in the Deox.

4. We have had problems in the past with processors not deoxidizing/desmutting panels/parts long enough. I am still arguing with Managers and Processors about that. I will look into this as a potential - especially with the research I have done with the silica contamination (from etching/deoxing cast aluminum) potentially hiding out in the deox. We have replaced the Alodine bath (and scrubbed) but we have not replaced the Deox yet. I suppose that is next on our list.

Update: Yesterday I raised the pH to 1.8, dropped the temperature to 75F, and physically locked out the airline that was being used to agitate the Alodine bath (the lab holds the only key to the lock and we will be agitating the bath for 1 hour three times a week, which is what gave us such wonderful results with the Iridite previously).
Our Ops Manager ran panels at 2 minutes, and they were powdery. I told him to run at 30 seconds, 1 minute, and 1:30. 30 seconds - 1 minute looks BEAUTIFUL. 1:30 and it starts to powder. Now the challenge is to ensure we pass Salt Spray at those immersion times... If we can't, Boeing will not accredit us.

Thank you very much Mr. Probert, I thought there shouldn't be a difference...and thank you immensely for the confirmation!

Kai Gussman [returning]
Aero Finishing, LLC - Arlington, Washington, USA


May 23, 2018

A. Good Morning Kai

Please refer to the following Finishing .com letter no.: 44433. "Close Looping" an Aluminum De-Ox System … starting at November 2nd.

I have to say this forum is great … Thank You to all the past contributors who have aided my success.
I am glad I can give back from my experience. I do not consider my self to be an expert, I have just done this more than 0 (ZERO) times.

I have just completed the journey you are starting.
It has been 6 months with passing results on both 2024-T3, 6061-T6 coupons to MIL-DTL-5541F Type 1 and Class 3 Specifications. Testing includes, 168 Hour Salt Spray, Contact Resistance and Paint Adhesion Testing to a 5A Rating.

The lessons learned:

#1 Do not use the Caustic Etch.
#2 If using a proprietary product (the product manufacturer you stated), consult their experts for guidance. They will tell you to use their full line of proprietary chemistries, Cleaner/Deox/Chromate. This was the path I had followed.
#3 Do Not Use DI water after the Deox.
#4 A semi Automated Titration System enabled the daily titrations to be performed in under one hour. Allowing for higher accuracy and control of the bath chemistries. If you are performing manual titrations do not allow for distraction. The bath composition is critical.
#5 Track the daily Chemistry measurements on an Excel Spreadsheet and this will aid in monitoring drag out and adds. I am still tracking trends for understanding when to perform additions and when to dump the tank.

The process I follow is:
Cleaner Immersion 140 °F 15% / Vol:      5 Minutes
Closed Loop DI Ambient Immersion Rinse: 15 Seconds
Closed Loop DI Ambient Spray Rinse      15 Seconds
Water Break Test                         1 Minute

C-IC-6MU DEOX/NITRIC Ambient Immersion 96.07 g/L and 6.55 g/L (Suppliers Recommended Proprietary Product Mixture)
Immersion Time:                  8 Minutes
Static Tap Water Immersion Rinse 1 Minute
Static Tap Water Immersion Rinse 1 Minute
Tap Water Spray Rinse            1 Minute

Chromate Ambient Immersion currently running 14.3 mg/mL and 1.44 pH
Immersion time for Class 3 is:          1 Minute
DI Immersion Rinse
Closed Loop DI Ambient Immersion Rinse 15 Seconds

Drip Dry-Dab the bottom of the panel-No Compressed Air is used to Dry the Coupon panels.
Wear Clean cotton or Nitrile glove before handling.

Stand the panels in a Blue Metro Tote on edge.
Wait a Minimum of 24 Hours to semi cure.

Individually Wrap in Uni Wrap 30 MPI VCI Paper.

Perform the testing regiment. Wait for Results

I hope this helps you in your success.

Cheers

Kurt Krueger
- Lexington, Massachusetts


May 25, 2018

A. Good, some progress has been made. If it was good at 60 seconds and bad at 90 seconds, that tells me the pH is still a tad low. Go back and standardize ONLY on the pH 1.02 which is closer to where we want to measure, do not set the 4 and 10. And we need some "moderate" agitation in the tank. Now, regarding the final rinse, it does not have to be squeeky clean and perfect - just dry on a little yellow water and that will enhance the protection.

robert probert
Robert H Probert
Robert H Probert Technical Services
Garner, North Carolina


May 25, 2018

thumbs up sign Good Afternoon and Happy Friday!

Mr. Krueger,
Your referenced post is actually the one that helped me discover our Silicate contamination problem!

Mr. Probert,
This morning, our tank read at 1.7 pH with our normal calibration.
I just re-calibrated the meter to a single point, with our 1.07 buffer. Sure enough, our pH now reads at 1.56 . I am issuing a change request to bring it up to an actual 1.8!
I will be changing our tank monitoring process for anything under 2.0 from now on. Thank you!

Yesterday I added an electric filter unit (sans filter) into the bath to provide mild manual circulation into the tank.

You recommended to leave a slight chem residue on the parts to dry (please correct me if I am misunderstanding) to aid in corrosion protection...
Our processors currently spray rinse and then 'soak' the Gold Chem in an ambient temperature immersion rinse for 3-5 minutes immediately post chemfilm. Is this something that will harm our coating? Right after that, parts come off the line and they are blow dried with compressed air nozzles, and stored in our "Dry Room" which is controlled to rise no higher than 120 °F. (My validation panels do not get compressed air, nor are they placed in the heated room. They are air dried in the Lab where I can keep my eye on them.)

I want to thank both of you, and this entire forum, for the help and resources provided. Absolutely invaluable.

Kai Gussman [returning]
Aero Finishing, LLC - Arlington, Washington, USA


May 25, 2018

A. Just let the final rinse be slightly yellow, and that will not violate many specs and will help enhance the protection. Always standardize the pH meter as close to the level you want to measure. When I do my bi-weekly service in a local NadCap shop, we use 7 for the water and nickel seal, then 4 for the tri-V chromate, then 1.63 for the 14-2 and the type I Chromic Acid Anodizing. I am glad you are making progress.

robert probert
Robert H Probert
Robert H Probert Technical Services
Garner, North Carolina



August 17, 2018

Q. How much pressure should be applied to detect the powdery condition tested in Alodine 1200S (yellow - brown)with 2024 aluminum?

When we run this material 2024, it has some powdery if the cloth is pressed a little bit, other alloys does not show powder even if the cloth is applied "hard" - rubbed to the surface.

Is there an "appropriate" level or specification of pressure to be applied?

Mauro Cardenas
Consultant - Mexicali, BC, Mexico



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