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"Surface Activation for Phosphating. Grain Size Issues"



Current postings:

Ed. note: Please!
No abstract questions.
Huh?

September 14, 2021

Q. Titanium based weak alkali chemical.

How to make this?

Santosh Kumar Yadav
- greater noida, India
^


"Electrolytic and Chemical Conversion Coatings"
by Biestek & Weber
from Abe Books
or

Affiliate Link
(commissions from your purchases make finishing.com possible)

September 2021

A. Hi Santosh. Finishing shops do not usually mix this chemical, they buy it from suppliers of the process chemistry.

You did not introduce yourself, but if you are a process supplier wanting to develop a line of surface activation chemistry rather than being a finishing shop employee, you might want to consult Biestek & Weber's "Electrolytic and Chemical Conversion Coatings" which discusses several different possibilities including 1% to 2% disodium phosphate with 0.1 to 0.5 mg of Ti per liter, with the Ti supplied as a titanium orthophosphate solution. Good luck!

Regards,

pic of Ted Mooney
Ted Mooney, P.E. RET
Striving to live Aloha
finishing.com - Pine Beach, New Jersey
^


September 27, 2021

Q. How to make phosphating solution ? Anyone tell me?

Santosh kumar Yadav [returning]
- greater noida, India
^


September 28, 2021

Q. How can I make cold phosphating solution?

Can you tell me please?

Santosh kumar Yadav [returning]
- greater noida, India
^


October 5, 2021

Can you tell me please how to make phosphating bath chemicals?

Santosh kumar Yadav [returning]
Employee - greater noida, India
^


October 2021

A. Hi cousin Santosh. Perhaps the mail we send to you gets lost in a spam filter because we've replied countless times, yet you continue to try to post the same abstract questions to thread after thread after thread here. Hopefully you'll eventually see this :-)

There are numerous good books on phosphating chemistry, many of which are listed on this page if you want to look for them in a library, but they run 250 pages or so. There are countless patents and expired patents you can read on the subject at patents.google.com, and hundreds of technical articles you can read on the subject at scholar.google.com or elsewhere.

There are countless variations in phosphating chemistry, and they are complicated, and virtually all phosphating is done using trade secret proprietary chemistry anyway. So, unfortunately, the idea that anyone can & will tell you in the couple of paragraphs appropriate to a public forum how to formulate, operate, control, and troubleshoot phosphating solutions in general, plus cold phosphating solutions, plus titanium-enhanced phosphating solutions isn't realistic.

But when you can pose a highly specific question which can be answered in a paragraph or so, I suspect that readers will enthusiastically & cheerfully do so. Best of luck!

Regards,

pic of Ted Mooney
Ted Mooney, P.E. RET
Striving to live Aloha
finishing.com - Pine Beach, New Jersey
^




Closely related Q&A's, oldest first:

Ed. note: Please!
No abstract questions.
Huh?

2002

Q. In zinc phosphating what is importance of activation ? What is chemical composition of activators ? How can it maintained ?

Vishwas M.
painting shop - Indore, India
^


"Phosphating of Metals"
by Werner Rausch
from Abe Books
or

Affiliate Link
(commissions from your purchases make finishing.com possible)

2007

A. Surface Activation chemicals activate the metal to obtain fine crystalline structure during phosphate coating which will increase corrosion resistance and adhesion properties. Crystalline structure less than 10 Microns always preferable.If we are not using activation rinse, the phosphate crystal size may be large and results in voids in Phosphate coating (Gap between structure will be large). Corrosion will take place at the voids.

Basically it is a Titanium based weak alkali chemical.

pH and Alkalinity are the parameters to be maintained daily.

P.M.Saravanan
P.M.Saravanan
paint shop manager
Chennai, Tamilnadu, India

^


Ed. note: Please!
No abstract questions.
Huh?

March 2, 2022

Q. @PM Saravanan,
Can you explain detailly about surface Activation process in pt line?

M nivedha
Employee - Bangalore, India
^


March 2022

A. Hi nivedha.

T.S.N. Sankara Narayanan offers quite a bit of detail below.

If you are a supplier trying to develop your own titanium activation solution, patent DE 10 2008 054 407 B4 looks like a good start (https://patents.google.com/patent/DE102008054407B4/en?q=titanium+activation+phosphating&oq=titanium+activation+phosphating).

Saravanan's posting was from 15 years ago so I'm afraid he is unlikely to see it. Please introduce yourself and your situation that motivates you to find his reply insufficient so we can move in the direction you need. Do you not yet have a titanium-based activation process in your PT line, or you do have one but it is not accomplishing what Saravanan says it should? Or do you lack the technical data sheets from the solution supplier to operate it? Or are you a chemical distributor trying to find a supplier of this process, or a student writing a thesis?

As forum curator I am trying to answer so the thread doesn't devolve into a long string of unanswered questions, but I don't have genuine experience in this topic, and short questions are rarely answered by knowledgable readers because they create so many ifs-ands-&-buts that readers don't want to start and get lost in a morass; so a good strategy is to please try to make your follow-up question longer than the answer you seek :-)

Luck & Regards,

pic of Ted Mooney
Ted Mooney, P.E. RET
Striving to live Aloha
finishing.com - Pine Beach, New Jersey
^



To minimize search efforts and to offer multiple viewpoints, we combined previously separate threads onto this page. Please forgive any resultant repetition, failures of chronological order, or what may look like readers disrespecting previous responses -- those other responses may not have been on the page at the time :-)



Necessity of Grain refiner for phosphating

2005

Q. In the process of looking for alternative suppliers for grain refiner for zinc phosphating I realized that I do not even know what the grain refiner is. Our MSDS say nothing about ingredients because apparently none of them are "hazardous". I have looked in reference materials such as Metal Finishing Guide Book, Electroplating Engineering Handbook, Chemical Surface Treatments of Metals (book), and Conversion Coatings (book) and have not seen any discussion of what the refiner is and how it works. Are you aware of resources that discuss this?

Tim Denhof
Job Shop Engineer - Chicago, Illinois, USA
^


2005

"Phosphating & Metal Pretreatment"
by D.B. Freeman
from Abe Books
or

Affiliate Link
(commissions from your purchases make finishing.com possible)

A. Grain refiners are chemical compounds usually added in activation (pre-dip) bath and/or the phosphating bath to reduce the crystal size in manganese and zinc phosphating processes.

Grain refinement in phosphate coating could be achieved by activating the surface using colloidal titanium phosphate prior to phosphating. During activation, the colloidal titanium phosphate particles are physically adsorbed on the metal surface and when the activated substrate comes in contact with a zinc phosphating bath, an ion exchange between the sodium ions on the surface of the titanium phosphate particles and the zinc ions of the phosphating solution takes place. The ion-exchanged particles act as nucleation agents for the zinc phosphate crystals because they have nearly the same stoichiometry and offer a crystallographic plane for an epitaxial growth.

The process for activating steel surface prior to phosphating was given in many patents. Use of 1-2% disodium phosphate solution containing 0.01% of titanium compounds have been extensively used in industries. Dilute solutions of cupric or nickel sulphates, oxalic acid and polyphosphonates also help in increasing the number of initial nuclei formed during phosphating and their subsequent growth, to yield thin and compact coatings of fine-grained nature.

The incorporation of calcium ions in a zinc phosphating enables a reduction in the grain size of the phosphating coating. The reduction in grain-size (25 micrometer to 4 micrometer) and the improvement in the compactness of the coating and corrosion resistance make this kind of modification of zinc phosphating baths as an important type of phosphating and it has been classified as calcium-modified zinc phosphating.

Similarly, addition of manganese and nickel ions in the zinc phosphating bath proves to be useful in refining the crystal size and improving the corrosion resistance of the resultant phosphate coatings.

T.S.N. Sankara Narayanan
T.S.N. Sankara Narayanan
- Chennai, Tamilnadu, India
(ed.note Nov. 2017: The good doctor has a fascinating blog at https://advancementinscience.wordpress.com)
^



Nickel in zinc phosphate solution

2005

Q. Sir,

we supply zinc phosphate solutions which are nickel free to customers who use for paint-base applications on MS. however I would like to know if its alright to add nickel if we want to broaden our range of applications.
Thanks,

Sonali Kokane
electroplating chemicals - Thane, Maharashtra and India
^


2005

A. Modification of the phosphating baths with nickel salts assumes significance with the introduction of pre-coated steels such as zinc, zinc alloy coated steels, etc., for automotive body panels which present challenges regarding the stability of phosphate coatings. These pre-coated steels show good performance with regard to formability and weldability. The extent of perforation and cosmetic corrosion is also less with these materials and they also posses a good surface appearance. When zinc and zinc alloy coated steels is phosphated using a nickel-free zinc phosphating bath the resultant coating will comprise only the hopeite (zinc phosphate) phase. Phosphate coating on these substrates having only the hopeite phase is not desirable for subsequent cathodic electrophoretic painting.

Nickel modified low-zinc phosphating formulations are the most significant modification proposed to cope up with the cathodic coating, particularly in the automobile industry. The presence of Ni2+ ions in these phosphating baths has several advantages. Although there is a decrease in coating weight, crystal formation occurs at an early stage and the crystal size is fine. The Ni2+ ions participate in the formation of phosphate crystal and enables crystal refinement. In this perspective, nickel addition in zinc phosphating baths is beneficial. However, the metal finishing industries are facing stringent regulations in effluent disposal and there is a transition from Cr(VI) free, Cd free and Pb free processes. Nickel is also carcinogenic. So you might consider other alternatives.

One possible alternative:

Addition of manganese salts in zinc phosphating bath could also perform a similar role as that of nickel in phosphating of zinc and zinc alloy coated steels. The addition of Mn2+ ions in the phosphating bath helps to increase the rate of formation of coating and also the working width of the phosphating bath. Also, the presence of manganese in the zinc phosphate coating resists the formation of white spots on galvanized steel. Manganese modified zinc phosphate coating possesses better corrosion resistance.

T.S.N. Sankara Narayanan
T.S.N. Sankara Narayanan
- Chennai, Tamilnadu, India
(ed.note Nov. 2017: The good doctor has a fascinating blog at https://advancementinscience.wordpress.com)
^


2005

thumbs up signShri Narayanan,

Thank you for the reply. Our inclination is to go Ni-free.

Sonali Kokane
electroplating Chemicals - Thane, Maharashtra and India
^



To minimize search efforts and to offer multiple viewpoints, we combined previously separate threads onto this page. Please forgive any resultant repetition, failures of chronological order, or what may look like readers disrespecting previous responses -- those other responses may not have been on the page at the time :-)



Building small zinc phosphate crystals

2007

Q. I am zinc phosphating using an immersion system, soap,rinse,pretreatment,zinc phosphate, rinse sealer, then RO rinse. The problem I am having is I am getting a few large crystals growing with many voids in between them, I am getting 400 mg coating weight which is ok but I want more and smaller crystal growth to give me a better feel for not having adhesions issues in the field.

Todd Dirkes
Production Manager - Longmont, Colorado, USA
^


simultaneous 2007

A. Though it has been some years since I was involved with phosphating, I recall that one of the important factors in regulating the property you speak of is the type, and concentration of catalyst present in the solution. I don't know that this is something that the user controls directly. When I did process control analysis on these baths, the only things that I tested for were total and free acid, and iron.

Talk to your vendor. They may have a "solution B" or something of that nature that will boost the catalyst and give you finer grain structure.

dave wichern
Dave Wichern
Consultant - The Bronx, New York
^


2007

A. For a really nice zinc phosphate surface, consider using a calcium modified zinc phosphate from one of the advertisers at this site. I had great luck with it.

James Watts
- Navarre, Florida
^


2007

A. Dear Sir

I think you need to check your cleaner alkalinity and rinsing. Also sludge in the phosphating. I feel that your cleaner is not getting washed off properly and thats the reason for a big size crystal deposit.

Regards,

Anurag Kanaujia
- New Delhi, INDIA
^



Zinc Phosphate grain size problem

April 28, 2010

Q. Dear friends.

I been having trouble with my zinc phosphate process
1.- degrease
2.- rinse
3.- rinse
4.- rinse
5.- acid (HCl)
6.- Phosphate
7.- rinse

The appearance of phosphate looks with big grains and some parts of the pieces with out phosphate, we can see the substrate.

Thanks for your comments I hope you can help us.

Alexandro Ramirez
plating shop employee - Saltillo Coahuila Mexico
^


"Preparation of Metals for Painting"
by Samuel Spring from Abe Books
or

Affiliate Link
(commissions from your purchases make finishing.com possible)

May 3, 2010

A. Dear Alexandro Ramirez,
For the bigger grain's causes
1) More sludge deposition on your phosphating bath
2) If you have the agitation tank, air pressure may be high or rpm of the stirrer is high
3) Or do the continuous filtration.

or may be the chemical is suitable for only making the Big Grains, better check with the chemical supplier.
Because for the powder coating or paint for the under coats , big grains are advisable for higher finishing thickness.

Kannan Boopathi
- Salem, Tanil Nadu, India
^


May 7, 2010

A. Hi Alexandro,

Without having seen how your operation is set up, I have to ask some questions and this may lead to a solution. I wonder why you have an HCl stage right before the phosphating stage. The drag-in from the HCl stage will contaminate the phosphating stage and lead to problems like an uneven coating and will make it difficult to control the bath. The extra acid will mess up your titrations.

If it is feasible for your operation, I would do the following. Switch the HCl stage with one of the three preceding rinse stages. Ideally, I would put the HCl stage in Stage 3; this way, you have a rinse between each chemical stage.

I would also ask your chemical supplier about a grain refiner and put it in the rinse stage prior to phosphating. This will decrease crystal size and help keep coating deposition uniform.

George Gorecki
- Naperville, Illinois
^



April 22, 2011 -- this entry appended to this thread by editor in lieu of spawning a duplicative thread

Q. I am a job coater.My process flow is KOD-water rinsing(2 times)-surface conditioning-Phosphating-E.D.coating.
My customer's requirement is --Phosphating grain size less than 10 microns.
How to achieve it?
Parameters are as follows-
T.A.-20 to 22
F.A.-.8-1.1
Accelerator-3.1-3.5
Temp. 43 °C.

Avinash vidhate
Plating shop employee - Nasik, Maharashtra, INDIA
^



March 13, 2013

Q. How can I prepare a surface activation chemical and which raw materials are used to prepare it and in what quantity?
Thanks.

dpak kumar
- Balasore, Orissa, India
^


March 13, 2013

A. Hi Dpak. If you prefer not to buy a proprietary activator, then Saravanan's information that it is a titanium based weak alkali should be a good basis for your in-house development efforts. Also, it is very easy today to do a search for expired patents and get some further ideas from them.

But nobody can openly publish the exact formulation of trade secret products. Good luck.

Regards,

Ted Mooney, finishing.com
Ted Mooney, P.E.
Striving to live Aloha
finishing.com - Pine Beach, New Jersey
^



Zinc Phosphate Crystals Too Big for Wire Drawing

February 5, 2016 -- this entry appended to this thread by editor in lieu of spawning a duplicative thread

Q. Dear Members,

I am using zinc phosphate on Carbon Wire Rods using the following parameters:

1) Acid cleaning (HCl at room temperature). Normally for 30 mins
2) Jet Wash
3) Rinse 1 (Ph above 3)
4) Rinse 2 (PH above 4)
5) Phosphate Bath ( 10-12 mins at 70-75 Degrees, TA 40-50, FA 7-8, TA/FA = 5-7), Accelerator 2-4
6) Rinse
7) Borax

Problem is the phosphate bath starts forming large crystals too soon which hinders the drawing process as they break too quickly in drawing. Another indication of disturbed chemistry of the bath is that its color changes to BLACK.

I have the following questions:

1) How do I prevent the bath from making large crystal or turning black?
2) If large crystals are being formed, how do we bring the bath back to its original form making smaller fine crystals?
3) How do I check the Fe content of the phosphate bath? Is it similar to testing the Fe content of Acid?

Thanking the members in advance for their anticipated valued input.

Saud Mahmood
- Karachi, Pakistan
^


February 13, 2016

A. You can test iron in the bath as the following: Iron points --

Reagents:
   0.1 N potassium permanganate solution, sulfuric acid (50 %), Urea.
Procedure:
   1. Pipette 100 ml bath sample into 250 ml conical flask.
   2. Add 2 ml sulfuric acid (50 %).
   3. Add 2 g urea.
   4. Stir the solution until the urea has dissolved and wait for approx. 3 min.
   5. Titrate with 0.1 N potassium permanganate solution to a stable pink color (stable for at least 15 s).

Consumption in ml = iron points
Fe (II) = iron points x 0.5585 g/l

Mahmoud Farahat
- Egypt , Cairo
^


March 29, 2016

A. Hello Mr Saud,

Crystals turning black can mean you have iron in your bath. You can easily know if there is with filter paper strips (qualitative grade, any brand) imbibed in 1% alcoholic orthophenanthroline. You let the papers dry, and dip them in the phosphate. If they turn reddish, you have iron in solution. Then, you must add accelerant until your phosphate bath is white in color and there is no reaction in the paper test strips.

You can measure as Mahmoud said the iron content, it must not rise from 0.3 g/l.

Then, you have EVERYTHING in the right level, and you still have the big-crystal-problem: I advise you talk with your vendor, there are many solutions but every one depends on the phosphate bath formulation. I cannot advise any of them without knowing the bath formula...

So, I hope you can solve your problem! Regards,

Daniel

Daniel Montañés
TEL - N FERRARIS - Cañuelas, Buenos Aires, Argentina
^


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