En Troubleshooting Guide
En Troubleshooting Guide
En Troubleshooting Guide
: EN Troubleshooting Guide
Revision: 04/30/04T-626
IMDS ID No.: Not Relevant
Technical Information
Electroless Nickel
Troubleshooting Guide
Subject
General Troubleshooting Guidelines
Discussion of Impurities in EN Plating Solutions
Critical Contaminant Levels in EN Plating Solutions
Specific EN Plating Problems:
Low Deposition Rate
No Deposition (New EN Solution Will Not Plate)
Pitted Deposits
Rough Deposits
Porous Deposits
Non-Uniform Deposits
Blistering (Ferrous & Non-Ferrous Metals)
Poor Adhesion
Streaky or Patterned Deposits
Skip Plating
Turbid or Milky Appearing Solution
Deposition on Tank Walls and/or Equipment
Rapid Solution pH Change
Test Procedures
Metric Conversion Tables
Temperature Conversion Tables
Page
2
3-5
6
7
8
8
9
10
10
10
11
11
12
12
13
13
14
15-16
17
PAGE 2
PAGE 3
PAGE 4
Chlorides
The presence of chlorides in an electroless nickel solution usually results in increased porosity and reduced
corrosion resistance of the deposited coating. Their presence can also lead to etching and corrosion of
anodically protected stainless steel tanks. Chlorides are generally introduced into the bath by drag-in of
hydrochloric acid from the pre-treatment line. Whatever the source and cause of anion contamination, once
they are present, they can be very difficult to remove. Thus, baths contaminated with anions are generally
discarded.
Orthophosphite
The build-up of orthophosphite in an electroless nickel solution is inevitable. It is the reaction product formed
when hypophosphite reduces nickel. For each gram of nickel reduced, about 4 grams of orthophosphite are
produced. When its concentration exceeds 100-150 g/l, orthophosphite tends to be co-deposited in the coating
and degrade its performance. Coatings deposited from baths containing excessive orthophosphite typically
exhibit high tensile stress, increased porosity and exhibit greatly reduced corrosion resistance. The presence of
excessive orthophosphite also tends to reduce plating rate and can cause the bath to white-out.
Silicon Compounds
The presence of some types of silicon compounds can cause instability in an electroless nickel solution and
produce rough deposits. Typically, this results from those silicon compounds, such as colloidal silica, that are
not soluble in the solution. Soluble compounds such as sodium silicate seem to have a minimal effect upon the
bath and its deposit. Silicon contamination is most commonly introduced into the bath as airborne particles of
dust or sand, as cleaner residues left on the part, or from improperly filtered deionized water. Colloidal silica,
which is often present in groundwater, can be as small as 0.25 m in diameter. Accordingly, the filters used in a
deionized water system must be adequately sized and properly maintained.
Contamination Levels
Some common contaminants of electroless nickel solutions and their critical concentrations are shown in the
following table. These levels are only guidelines. Their effect can vary depending upon bath formulation and
operation. The level at which most contaminants become a problem is dependent upon such factors as bath
loading, the nature of the substrate being plated and the activity of the solution (pH, temperature and
concentration). In addition, many contaminants have a synergistic effect and together may produce problems at
lower concentration levels than they would individually.
Bismuth, when present by itself, stabilizes electroless nickel solutions and can reduce plating rate and produce
skip plating. When antimony is also present, bismuth causes the coating's internal stress to become highly
tensile.
Tin at low concentrations, especially when introduced into electroless nickel solutions as a lubricant
component, can cause severe instability of electroless nickel solutions. At high concentrations, tin typically acts
as a stabilizer.
The performance of zinc contaminated electroless nickel solutions is dependent upon the loading factor of the
bath. Bulk plating facilities with large ratios can tolerate high levels of zinc without effect. Facilities with low bath
loading may experience problems at lower contaminant levels.
PAGE 5
Silicon compound may be introduced into electroless nickel solutions in many different forms, as silica,
silicates, silicones, etc. Analysis to determine which form is present can be difficult. Common analytical
techniques probably measure only a small part of the total silicon present.
Every contaminant present in an electroless nickel solution changes the properties of the deposit obtained.
Engineering properties, such as corrosion resistance, can be greatly degraded. Solutions contaminated at
levels where operating characteristics are normal may still produce inferior deposits. Thus, it is good practice to
eliminate the source of a contaminant rather than keeping contamination levels within acceptable limits.
PAGE 6
Problem Level
>150 ppm
1-3 ppm
>3 ppm
1-3 ppm
1 ppm
1-2 ppm
Symptom
Reduced rate
Reduced rate
Skip plating
High Stress
No plating
Skip plating
Reduced rate
Skip plating
Copper deposits
Remedy
Discard
Increase activity or discard
Discard
Increase activity or discard
Increase activity or discard
Increase activity
Palladium
1 ppm
Reduced rate
Dark deposit
Reduced rate
No plating
Skip plating
Reduced rate
Skip plating
Decomposition
Platinum
1-3 ppm
Decomposition
Discard
Tin
1-3 ppm
Instability
Discard
>75 ppm
Lead*
2-5 ppm
Manganese
Tin
Titanium
Zinc
Organics
Sulfides
Nitrates
Chlorides
Not determined
3-10 ppm
Not determined
>15 ppm
Not determined
>1 ppm
> 50-75 ppm
Not determined
Orthophosphite
> 150-250 g/l
Silicon
Compounds
>6 ppm
Dull deposit
Reduced rate
Reduced rate
Skip plating
Reduced rate
Dark deposit
Fine pitting
Reduced rate
Dark deposit
Dark deposit
Streaky deposit
Porous deposits
White out
Stressed deposits
Porous Deposits
Roughness
Instability
* NOTE: Heavy metals such as Cd and Pb are typically used in trace quantities as brightening and stabilizing
additives in most proprietary electroless nickel baths.
PAGE 7
Corrective Action
Low pH
Bath is over-stabilized
Nitrate contamination
Excessive agitation
Reduce agitation
PAGE 8
Corrective Action
Low pH
Nitrate contamination
Solution contamination
Pitted Deposits
Possible Cause
Corrective Action
Poor filtration
Improve filtration
PAGE 9
Rough Deposits
Possible Cause
Corrective Action
Poor filtration
Insufficient agitation
pH is too high
Localized overheating
PAGE 10
Porous Deposits
Possible Cause
Corrective Action
Organic impurities
Improve filtration
Porous substrate
Non-Uniform Deposits
Possible Cause
Corrective Action
Corrective Action
EN bath is over-stabilized
Corrective Action
Improve cleaning and acid activation
PAGE 11
Poor Adhesion
Possible Cause
Corrective Action
Incorrect pre-treatment
Poor cleaning
Poor activation
Contaminated solution.
Corrective Action
Poor agitation
Gas patterns
Drag-in of silicates
PAGE 12
Skip Plating
Possible Cause
Corrective Action
Improper cleaning
Improper activation
Contaminated EN bath
Contaminated rinses
Corrective Action
pH is too high
additions
Hypophosphite content is too high
Improve rinsing
PAGE 13
Corrective Action
Inadequate filtration
Improve filtration
Excessive additions
Localized overheating
Corrective Action
Filter bath out; strip tank and equipment with nitric acid
PAGE 14
TEST PROCEDURES
Porosity Tests
Ferroxyl (Steel)
Immerse a cleaned EN plated sample in a solution containing 25 grams of potassium ferrocyanide and 15
grams of sodium chloride in one liter of deionized water at ambient temperature for 30 seconds. Blue spots
appearing on the sample indicate porosity in the EN coating.
Hot Deionized Water (Steel)
Immerse a cleaned sample in boiling deionized water for five minutes. Remove article and rinse in methanol
and dry. Rust spots appearing on the sample indicate porosity in the EN coating.
Copper Sulfate (Steel)
Immerse or swab the sample with a solution of saturated copper sulfate for 15 seconds. Pore sites are
indicated by copper-colored spots.
Hydrochloric Acid. (Steel and Aluminum)
Immerse a cleaned sample in 50% by volume hydrochloric acid for two minutes at ambient temperature.
Gassing indicates porosity over steel. Black spots indicate porosity over aluminum.
Alizarin (Aluminum)
Immerse a cleaned sample in a 10% (by wt.) solution of sodium hydroxide in water at ambient temperature (6575o F). After three minutes, the sample shall be removed, rinsed in water, and then immersed in ambient
temperature alizarin sulfonate solution. After four minutes, the sample shall be removed and repeatedly dipped
in glacial acetic acid until the violet color disappears. Any remaining red spots indicate porosity. The alizarin
sulfonate solution is prepared by dissolving 1.5 grams of methyl cellulose in 90 ml. of boiling deionized water to
which, after cooling, a solution of 0.1 grams alizarin sulfonic acid dissolved in 5 ml of ethanol is added.
PAGE 15
by
To Obtain
Cubic centimeters
0.061
cubic inches
Cubic centimeters
2.65x 10-4
gallons
Cubic centimeters
0.0338
ounces (fluid)
Cubic feet
28317
cubic centimeters
Cubic feet
1728
cubic inches
Cubic feet
7.48
gallons
62.37
pounds
Cubic inches
16.39
cubic centimeters
Cubic meters
35.3145
cubic feet
Cubic feet
0.0283
cubic meters
Multiply
by
To Obtain
Cubic feet
28.3162
liters
Cubic inches
0.0164
liters
Gallons
3785.4
cubic centimeters
Gallons (U.S.)
231
cubic inches
Gallons (U.S.)
3.785
liters
Gallons (U.S.)
128
ounces (fluid)
Liters
0.2642
gallons (U.S.)
Liters
0.0353
cubic feet
Liters
61.025
cubic inches
Multiply
by
To Obtain
Grams
0.0353
ounces
Kilograms
2.205
pounds
Ounces
28.35
grams
Pounds
453.6
grams
Capacity
Weight
PAGE 16
Length
Multiply
by
To Obtain
Centimeters
0.3937
inches
Inches
2.54
centimeters
Feet
0.3048
meters
Meters
3.2808
feet
Miles
1.6093
kilometers
Kilometers
0.6214
miles
Multiply
by
To Obtain
psi
7,000
MPa
Pressure
PAGE 17
C
-17.8
-17.2
-16.7
-16.1
-15.6
-15.0
-14.4
-13.9
-13.3
-12.8
-12.2
-11.7
-11.1
-10.6
-10.0
-9.44
-8.89
-8.33
-7.78
0 to 18
F/C
0
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
C
-7.22
-6.67
-6.11
-5.56
-5.00
-4.44
-3.89
-3.33
-2.78
-2.22
-1.67
-1.11
-0.56
0
0.56
1.11
1.67
2.22
2.78
19 to 37
F/C
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
F
32.0
33.8
35.6
37.4
39.2
41.0
42.8
44.6
46.4
48.2
50.0
51.8
53.6
55.4
57.2
59.0
60.8
62.6
64.4
C
3.33
3.89
4.44
5.00
5.56
6.11
6.67
7.22
7.78
8.33
8.89
9.44
10.0
10.6
11.1
11.7
12.2
12.8
13.3
38 to 56
F/C
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
C
13.9
14.1
15.0
15.6
16.1
16.7
17.2
17.8
18.3
18.9
19.4
20.0
20.6
21.1
21.7
22.2
22.8
23.4
23.9
57 to 75
F/C
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
F
100.4
102.2
104.0
105.8
107.6
109.4
111.2
113.0
114.8
116.6
118.4
120.2
122.0
123.8
125.6
127.4
129.2
131.0
132.8
C
24.4
25.0
25.6
26.1
26.7
27.2
27.8
28.3
28.9
29.4
30.0
30.6
31.1
31.7
32.2
32.8
33.3
33.9
34.4
76 to 94
F/C
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
93
94
C
35.0
35.6
36.1
36.7
37.2
37.8
43.0
49.0
54.0
60.0
66.0
71.0
77.0
82.0
88.0
93.0
99.0
100.0
101.7
95 to 215
F/C
95
96
97
98
99
100
110
120
130
140
150
160
170
180
190
200
210
212
215
F
66.2
68.0
69.8
71.6
73.4
75.2
77.0
78.8
80.6
82.4
84.2
86.0
87.8
89.6
91.4
93.2
95.0
96.8
98.6
F
168.8
170.6
172.4
174.2
176.0
177.8
179.6
181.4
183.2
185.0
186.8
188.6
190.4
192.2
194.0
195.8
197.6
199.4
201.2
F
134.6
136.4
138.2
140.0
141.8
143.6
145.1
147.2
149.0
150.8
152.6
154.4
156.2
158.0
159.8
161.6
163.4
165.2
167.0
F
203.0
204.8
206.6
208.4
210.2
212.0
230.0
248.0
266.0
284.0
302.0
320.0
338.0
256.0
374.0
392.0
410.0
413.0
419.0