GB2066848A - Ferritic Stainless Steel - Google Patents
Ferritic Stainless Steel Download PDFInfo
- Publication number
- GB2066848A GB2066848A GB8011020A GB8011020A GB2066848A GB 2066848 A GB2066848 A GB 2066848A GB 8011020 A GB8011020 A GB 8011020A GB 8011020 A GB8011020 A GB 8011020A GB 2066848 A GB2066848 A GB 2066848A
- Authority
- GB
- United Kingdom
- Prior art keywords
- stainless steel
- ferritic stainless
- titanium
- nitrogen
- columbium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Heat Treatment Of Sheet Steel (AREA)
- Heat Treatment Of Steel (AREA)
- Catalysts (AREA)
- Load-Engaging Elements For Cranes (AREA)
- Treatment Of Steel In Its Molten State (AREA)
- Compounds Of Iron (AREA)
Abstract
A ferritic stainless steel, characterized by superior crevice and intergranular corrosion resistance, consists of, by weight, up to 0.08% carbon, up to 0.06% nitrogen, from 25.00 to 35.00% chromium, from 3.60 to 5.60% molybdenum, up to 2.00% manganese, up to 2.00% nickel, up to 2.00% silicon, up to 0.5% aluminum, up to 2.00% titanium, zirconium and/or niobium, balance iron. The sum of carbon plus nitrogen is in excess of 0.0275%. Titanium, zirconium, and niobium, are in accordance with the following equation: %Ti/6+%Zr/7+%Nb/8>/=%C+%N
Description
SPECIFICATION
Ferritic Stainless Steel
The present invention relates to a ferritic stainless steel.
United States Patent Nos. 3,932,174 and 3,929,473 describe ferritic stainless steels having superior crevice and intergranular corrosion resistance. The steels described therein contain by weight, 29% chromium and 4% molybdenum. They also have a maximum carbon plus nitrogen content of 250 parts per million. Carbon and nitrogen are limited as the corrosion resistance of the steels deteriorates with increasing levels thereof.
The low carbon and nitrogen requirement for the alloys of United States Patent Nos. 3,932,174 and 3,929,473 is disadvantageous in that it necessitates more expensive melting procedures, such as vacuum induction melting.
Through the present invention, there is provided an alloy having properties comparable to that of
Patent Nos. 3,929,174 and 3,929,473, yet one which does not require the expensive melting procedures referred to hereinabove. The alloy of the present invention can, for example, be melted and refined using argon-oxygen decarburization (AOD) procedures.
The present invention provides a ferritic stainless steel consisting essentially of, by weight, up to 0.08% carbon, up to 0.06% nitrogen, from 25.00 to 35.00% chromium, from 3.60 to 5.60% molybdenum, up to 2.00% manganese, up to 2.00% nickel, up to 2.00% silicon, up to 0.5% aluminium, up to 2.00% titanium, zirconium and/or columbium, balance essentially iron; said titanium, zirconium and/or columbium being in accordance with the following equation: %Ti/6+%Zr/7 +%Cb/8 > %C+%N the sum of said carbon plus said nitrogen being in excess of 0.0275%.
As will be seen, the alloy of the present invention has up to 2.00% titanium, zirconium and/or columbium in accordance with the following equation: %Ti/6+%Zr/7+%Cb/8 > %C+%N and a carbon plus nitrogen content in excess of 275 parts per million. It is characterized by superior crevice and intergranular corrosion resistance, by good weldability and by satisfactory toughness both prior to and after welding.
For the reasons noted hereinabove, the alloy of the present invention is clearly distinguishable from that of United States Patent Nos. 3,932,174 and 3,929,473. It is also distinguishable from that of two other alloys, that of United States Patent No. 3,957,544 and that of United States Patent No.
4,119,765. Both of these alloys have maximum molybdenum contents below that specified for the present invention.
Another reference of interest is a paper entitled, "Ferritic Stainless Steel Corrosion Resistance and Economy". The paper was written by Remus A. Lula and appeared in the July 1976 issue of Metal
Progress, pages 24-29. It does not disclose the ferritic stainless steel of the present invention.
In the alloy of the present invention carbon and nitrogen are usually present in respective amounts of at least 0.005% and 0.010%, with the sum being in excess of 0.0300%. Chromium and molybdenum are preferably present in respective amounts of 28.50 to 30.50% and 3.75 to 4.75%.
Manganese, nickel and silicon are each usually present in amounts of less than 1.00%. Aluminium which may be present for its effect as a deoxidizer is usually present in amounts of less than 0.1%.
Titanium, columbium and/or zirconium are added to improve the crevice and intergranular corrosion resistance of the alloy, which in a sense is a high carbon plus nitrogen version of United
States Patent Nos. 3,932,174 and 3,929,473. It has been determined, that stabilizers can be added to high carbon and/or nitrogen versions of United States Patent Nos. 3,932,174 and 3,929,473, without destroying the toughness and/or weldability of the alloy. Although it is preferred to add at least 0.15% of titanium insofar as the sole presence of columbium can adversely affect the weldability of the alloy, it is within the scope of the present invention to add the required amount of stabilizer as either titanium or columbium. Columbium has a beneficial effect in comparison with titanium, on the toughness of the alloy.A particular embodiment of the invention calls for at least 0.15% columbium and at least 0.15% titanium. Titanium, columbium and zirconium are preferably present in amounts up to 1.00% in accordance with the following equation: /OTi/6+%Zr/7+%Cb/8=1.0 to 4.0 (%C+%N)
The ferritic stainless steel of the present invention is particularly suited for use as a welded article having a thickness no greater than 1.78 mm (0.070 inch) (usually no greater than 1.24 mm (0.049 inch)), and in particular, as welded condenser tubing which typically ranges from 0.66 to 0.94 mm (0.026 to 0.037 inch).
The following examples are illustrative of several aspects of the invention:
Ingots from fifteen heats (Heats A through 0) were heated to 1121 OC (20500 F), hot rolled to 3.175 mm (0.125 inch) strip, annealed at temperatures of 1065 or 1121 OC (1950 or 20500F), cold rolled to strip of from about 1.57 to 1.65 mm (0.062 to 0.065 inch) and annealed at temperatures of 1065 or 11 21 C (1950 or 20500 F). Specimens were subsequently evaluated for crevice corrosion resistance. Other specimens were TIG welded and evaluated for crevice and intergranular corrosion resistance. The chemistry of the heats appears hereinbelow in Table I.
Table I
Composition (wt.%)
Heat C N Cr Mo Mn Ni Si Al Ti Cb Fe
A 0.042 0.022 29.09 4.00 0.24 0.31 0.34 0.039 0.31 - Bal.
B 0.064 0.022 28.98 4.01 0.24 0.29 0.34 0.050 0.34 - Bal.
C 0.020 0.021 29.08 4.00 0.24 0.29 0.33 0.023 0.26 - Bal.
D 0.037 0.019 29.05 4.02 0.24 0.29 0.34 0.053 0.40 - Bal.
E 0.039 0.014 28.88 4.02 0.24 0.30 0.33 0.055 0.61 - Bal.
F 0.064 0.013 28.91 4.01 0.24 0.29 0.32 0.055 0.66 - Bal.
G 0.015 0.015 29.10 4.02 0.35 0.41 0.38 0.010 - 0.38 Bal.
H 0.030 0.016 29.10 4.04 0.36 0.45 0.40 0.014 - 0.53 Bal.
I 0.029 0.019 28.92 4.04 0.35 0.54 0.39 0.016 0.20 0.39 Bal.
J 0.030 0.025 28.96 4.20 0.34 0.45 0.36 0.029 0.50 - Bal.
K 0.030 0.026 29.05 4.18 0.34 0.46 0.37 0.029 0.20 0.32 Bal.
L 0.031 0.025 28.96 4.06 0.36 0.45 0.29 0.027 0.09 0.45 Bal.
M 0.034 0.027 28.95 4.20 0.43 0.46 0.37 0.040 0.19 0.41 Bal.
N 0.035 0.026 28.75 4.20 0.40 0.47 0.45 0.025 0.20 0.42 Bal.
0 0.032 0.024 29.52 4.10 0.37 0.51 0.28 0.030 0.31 0.44 Bal.
Additional data pertaining thereto appears hereinbelow in Table II.
Table II Heat %C+%N %Ti/6+%Zr/7+%Cb/8 A 0.064 0.052
B 0.086 0.057
C 0.041 0.043
D 0.056 0.067
E 0.053 0.102
F 0.077 0.110
G 0.030 0.048
H 0.046 0.066
0.048 0.082
J 0.055 0.083
K 0.056 0.073
L 0.056 0.071
M 0.061 0.083 N 0.061 0.086
0 0.056 0.107
Note that Heats A and B are outside the subject invention. They are not in accordance with the following equation: %Ti/6+%Zr/7+%Cb/82%C+%N Crevice corrosion resistance was evaluated by immersing 25.4 mm by 50.8 mm (1 inch by 2 inch) surface ground specimens in a 10% ferric chloride solution for 72 hours. Testing was performed at temperatures of 35 and 500C (95 and 1220 F). Crevices were created on the edges and surfaces by employing polytetrafluoroethylene blocks on the front and back, held in position by pairs of rubber bands stretched at 900 to one another in both longitudinal and transverse directions. The test is described in Designation: G48-76 of the American Society for Testing and Materials.
The results of the evaluation appear below in Table Ill.
Table Ill
10% Ferric Chloride Crevice Corrosion Test
Weight Loss (Grams)
Base Metal As Welded As Welded
Heat 50 C(122 F) 35 C(95 F) 50 C(122 F)
A 0.0 0.0 0.4195
B 0.8519 0.0198 0.5783
C 0.0 0.0001 0.0004
D 0.0 0.0
E 0.0 0.0 0.0
F 0.0 0.0001 0.0
G - - 0.0
H - - I - - 0.0 J - - 0.0003
K - - 0.0
L - - 0.0
M - - 0.0
N - - 0.0
0 - - 0.0013
From Table Ill, it is noted that the crevice corrosion resistance of Heats C through G and I through
O is superior to that for Heats A and B. Base metal from Heat B lost as much as 0.8519 gram. Welded metal from Heats A and B respectively lost as much as 0.4195 and 0.5783 gram. Significantly, Heats
A and B are outside the subject invention. On the other hand, Heats C through G and I through 0 are in accordance therewith.
Intergranular corrosion resistance was evaluated by immersing 25.4 mm by 50.8 mm (1 inch by 2 inch) surface ground specimens in a boiling cupric sulfate - 50% sulfuric acid solution for 120 hours. The usual pass-fail criteria for this test are a corrosion rate of 0.6 mm (24.0 mils) per year (0.05 mm (0.0020 inches) per month) and a satisfactory microscopic examination. This test is recommended for stabilized high chromium ferritic stainless steels.
The results of the evaluation appear hereinbelow in Table IV.
Table IV
Cupric Sulfate -50% Sulfuric Acid Corrosion Test
Microscopic
Corrosion Rate -As Welded Examination as
Heat mm(mlls)/year mm(inches)/month Welded (at 30x)
A 0.208534(8.21) 0.017374(0.000684)
B 3.5814(141) 0.299364(0.011786) C 0.173228 (6.82) 0.014427(0.000568) D 0.252476 (9.94) 0.021031(0.000828) E 0.141986 (5.59) 0.011836(0.000466) F 0.2794(11.0) 0.023216(0.000914) G 0.146304(5.76) 0.012192(0.000480) NA*
H ~ ~ ~ I 0.159766(6.29) 0.013310(0.000524) NA
J 0.167894(6.61) 0.013995 (0.000551) NA
K 0.141986(5.59) 0.011836(0.000466) NA
L 0.133096 (5.24) 0.011100(0.000437) NA
M 0.146812 (5.78) 0.012243 (0.000482) NA
N 0.134112(5.28) 0.011176(0.000440) NA O 0.16129 (6.35) 0.013437 (0.000529) NA
*NA: No Intergranular Attack or Grain Dropping.
From Table IV, it is noted that only Heat B failed the subject test. Heat B had a corrosion rate of
3.5814 mm (141 mils) per year. As stated hereinabove, it is one of the two heats outside the present
invention. The other heat, being Heat A. It is, however, further outside the subject invention than is
Heat A in that it has a lower titanium to carbon plus nitrogen ratio.
Toughness was evaluated by determining the transition temperature using Charpy V-notch
specimens for hot rolled and annealed material (3.1 75x 10.00 mm (0.125x0.394 inch) specimens)
and for as welded material (.157 to 1 .65x 10.00 mm (0.062 to 0.065x0.394 inch) specimens).
Transition temperature was based upon a 50% ductile - 50% brittle fracture appearance. The transition temperatures appear hereinbelow in Table V.
Table V
Transition Temperature C ( F)
Hot Rolled
As Welded AndAnnealed
Heat 0C(0F) 0C(0F) A -4 (25)(1) 74 (165) (3)
B 16 (60)(1) 85 (185) (3)
C 27 (80)(1) 68 (155) (3)
D 46(115)(1) 85 (185) (3)
E 118(245)(1) 91(195)(3)
F 104(220)(1) 88(190(3) G -37 (-35) (2) 35 ( 95) (4)
H - 49(120)(4)
35 (95)(2) 71(160)(4)
J 43(110)(2) 54 (130) (4)
K 16 (60)(2) 49 (120) (4)
L 32 (90)(2) 43(110)(4)
M 41(105) (2) 57 (135) (4)
N 68(155)(2) 60(140)(4) 0 54 (130) (2) 99 (210) (4)
(1) Strip annealed prior to welding at 1121 C (20500 F) - air cooled.
(2) Strip annealed prior to welding at 1065 C (19500F) -water quenched.
(3) Annealed at 1121 C (20500 F) - water quenched; transverse test.
(4) Annealed at 1 0650C (19500 F) - water quenched; transverse test.
The transition temperatures indicate that the steel of the present invention can be cold rolled, formed and welded, although some preheating might at times be desirable. The columbium-bearing specimens had lower transition temperatures than the titanium-bearing specimens. The specimens containing both titanium and columbium had transition temperatures between that of the columbiumbearing and titanium-bearing specimens.
Claims (9)
1. A ferritic stainless steel consisting essentially of, by weight, up to 0.08% carbon, up to 0.06% nitrogen, from 25.00 to 35.00% chromium, from 3.60 to 5.60% molybdenum, up to 2.00% manganese, up to 2.00% nickel, up to 2.00% silicon, up to 0.5% aluminium, up to 2.00% titanium, zirconium and/or columbium, balance essentially iron; said titanium, zirconium and/or columbium being in accordance with the following equation: %Ti/6 +%Zr/7 +%Cb/8 > %C+%N the sum of said carbon plus said nitrogen being in excess of 0.0275%.
2. A ferritic stainless steel according to claim 1, having at least 0.005% carbon and at least 0.010% nitrogen, the sum of said carbon plus said nitrogen being in excess of 0.0300%.
3. A ferritic stainless steel according to claim 1 or 2, having from 28.50 to 30.50% chromium.
4. A ferritic stainless steel according to claim 1,2 or 3, having from 3.75 to 4.75% molybdenum.
5. A ferritic stainless steel according to any one of the preceding claims, having up to 1.00% titanium, zirconium and/or columbium in accordance with the following equation: %Ti/6+%Zr/7+%Cb/8=1 .0 to 4.0 (%C+%N)
6. A ferritic stainless steel according to any one of the preceding claims having at least 0.1 5% titanium.
7. A ferritic stainless steel according to claim 6, having at least 0.15% columbium.
8. A ferritic stainless steel according to any one of the preceding claims having at least 0.005 Ó carbon, at least 0.010% nitrogen, from 28.50 to 30.50% chromium, from 3.75 to 4.75% molybdenum, and up to 1.00% titanium, zirconium and/or columbium in accordance with the following equation:
%Ti/6+%Zr/7+%Cb/8=1.0 to 4.0 (%C+%N) the sum of carbon plus said nitrogen being in sxcess of 0.0300%.
9. A ferritic stainless steel substanaialíy according to any one of the specific Examples of Heats C to 0 therein.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US10937380A | 1980-01-03 | 1980-01-03 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB2066848A true GB2066848A (en) | 1981-07-15 |
| GB2066848B GB2066848B (en) | 1983-06-02 |
Family
ID=22327323
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB8011020A Expired GB2066848B (en) | 1980-01-03 | 1980-04-02 | Ferritic stainless steel |
Country Status (19)
| Country | Link |
|---|---|
| JP (1) | JPS5698459A (en) |
| KR (1) | KR850000995B1 (en) |
| AT (1) | AT376706B (en) |
| AU (1) | AU535724B2 (en) |
| BE (1) | BE882792A (en) |
| BR (1) | BR8001876A (en) |
| CA (1) | CA1163471A (en) |
| CS (1) | CS216220B2 (en) |
| DE (1) | DE3012957A1 (en) |
| ES (1) | ES8105040A1 (en) |
| FR (1) | FR2473069A1 (en) |
| GB (1) | GB2066848B (en) |
| IT (1) | IT1188919B (en) |
| MX (1) | MX6668E (en) |
| NL (1) | NL8001739A (en) |
| NO (1) | NO154585C (en) |
| PL (1) | PL124421B1 (en) |
| SE (1) | SE436577B (en) |
| SU (1) | SU1258328A3 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2193726A (en) * | 1986-07-23 | 1988-02-17 | Jgc Corp | Carbon containing compound treating apparatus with resistance to carbon deposition |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10883160B2 (en) | 2018-02-23 | 2021-01-05 | Ut-Battelle, Llc | Corrosion and creep resistant high Cr FeCrAl alloys |
| JP7278476B2 (en) * | 2020-04-15 | 2023-05-19 | 日鉄ステンレス株式会社 | Ferritic stainless steel material and manufacturing method thereof |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA922543A (en) * | 1969-07-11 | 1973-03-13 | The International Nickel Company Of Canada | Corrosion resistant ferritic stainless steel |
| GB1359629A (en) * | 1971-10-26 | 1974-07-10 | Deutsche Edelstahlwerke Gmbh | Corrosion-resistant ferritic chrome steel |
| US3890143A (en) * | 1972-04-14 | 1975-06-17 | Nyby Bruk Ab | Welded constructions of stainless steels |
| AT338854B (en) * | 1972-09-04 | 1977-09-26 | Ver Edelstahlwerke Ag | FERRITIC OR FERRITIC-AUSTENITIC STEEL ALLOYS FOR OBJECTS THAT ARE CORROSION-RESISTANT TO ACID AND WATER MIXTURES UP TO 70 DEGREES C. |
| JPS5241113A (en) * | 1975-09-30 | 1977-03-30 | Nippon Steel Corp | Ferritic stainless steel having high toughness and high corrosion resi stance |
| GB1565419A (en) * | 1976-04-27 | 1980-04-23 | Crucible Inc | Stainless steel welded articles |
| DE2701329C2 (en) * | 1977-01-14 | 1983-03-24 | Thyssen Edelstahlwerke AG, 4000 Düsseldorf | Corrosion-resistant ferritic chrome-molybdenum-nickel steel |
-
1980
- 1980-03-11 SE SE8001869A patent/SE436577B/en not_active IP Right Cessation
- 1980-03-12 NO NO800713A patent/NO154585C/en unknown
- 1980-03-13 AU AU56418/80A patent/AU535724B2/en not_active Ceased
- 1980-03-25 NL NL8001739A patent/NL8001739A/en not_active Application Discontinuation
- 1980-03-28 BR BR8001876A patent/BR8001876A/en not_active IP Right Cessation
- 1980-03-31 IT IT48299/80A patent/IT1188919B/en active
- 1980-04-01 CA CA000348952A patent/CA1163471A/en not_active Expired
- 1980-04-02 DE DE19803012957 patent/DE3012957A1/en not_active Ceased
- 1980-04-02 GB GB8011020A patent/GB2066848B/en not_active Expired
- 1980-04-07 KR KR1019800001438A patent/KR850000995B1/en active
- 1980-04-15 BE BE0/200229A patent/BE882792A/en not_active IP Right Cessation
- 1980-04-18 FR FR8008817A patent/FR2473069A1/en active Granted
- 1980-05-02 JP JP5935980A patent/JPS5698459A/en active Granted
- 1980-05-06 SU SU2917251A patent/SU1258328A3/en active
- 1980-05-13 AT AT0255980A patent/AT376706B/en not_active IP Right Cessation
- 1980-05-26 MX MX808842U patent/MX6668E/en unknown
- 1980-06-12 ES ES492375A patent/ES8105040A1/en not_active Expired
- 1980-07-30 CS CS805325A patent/CS216220B2/en unknown
- 1980-09-11 PL PL1980226698A patent/PL124421B1/en unknown
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2193726A (en) * | 1986-07-23 | 1988-02-17 | Jgc Corp | Carbon containing compound treating apparatus with resistance to carbon deposition |
| GB2193726B (en) * | 1986-07-23 | 1991-05-22 | Jgc Corp | Carbon containing compound treating apparatus with resistance to carbon deposition |
Also Published As
| Publication number | Publication date |
|---|---|
| ES492375A0 (en) | 1981-05-16 |
| JPS5698459A (en) | 1981-08-07 |
| DE3012957A1 (en) | 1981-09-03 |
| CS216220B2 (en) | 1982-10-29 |
| AU535724B2 (en) | 1984-04-05 |
| FR2473069B1 (en) | 1984-12-07 |
| ES8105040A1 (en) | 1981-05-16 |
| JPH0321625B2 (en) | 1991-03-25 |
| BR8001876A (en) | 1981-07-14 |
| BE882792A (en) | 1980-10-15 |
| ATA255980A (en) | 1984-05-15 |
| KR850000995B1 (en) | 1985-07-15 |
| NO800713L (en) | 1981-07-06 |
| SE8001869L (en) | 1981-07-04 |
| IT8048299A0 (en) | 1980-03-31 |
| SE436577B (en) | 1985-01-07 |
| IT8048299A1 (en) | 1981-10-01 |
| NL8001739A (en) | 1981-08-03 |
| NO154585C (en) | 1986-11-05 |
| MX6668E (en) | 1985-10-07 |
| GB2066848B (en) | 1983-06-02 |
| SU1258328A3 (en) | 1986-09-15 |
| KR830002901A (en) | 1983-05-31 |
| IT1188919B (en) | 1988-01-28 |
| FR2473069A1 (en) | 1981-07-10 |
| PL124421B1 (en) | 1983-01-31 |
| CA1163471A (en) | 1984-03-13 |
| PL226698A1 (en) | 1981-08-07 |
| NO154585B (en) | 1986-07-28 |
| AU5641880A (en) | 1981-07-09 |
| AT376706B (en) | 1984-12-27 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PCNP | Patent ceased through non-payment of renewal fee |
Effective date: 19990402 |