US2685546A - Method for reducing the permeability of alloys by hydrogen - Google Patents
Method for reducing the permeability of alloys by hydrogen Download PDFInfo
- Publication number
- US2685546A US2685546A US265207A US26520752A US2685546A US 2685546 A US2685546 A US 2685546A US 265207 A US265207 A US 265207A US 26520752 A US26520752 A US 26520752A US 2685546 A US2685546 A US 2685546A
- Authority
- US
- United States
- Prior art keywords
- hydrogen
- alloy
- permeability
- reducing
- temperature
- 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.)
- Expired - Lifetime
Links
- 239000001257 hydrogen Substances 0.000 title claims description 34
- 229910052739 hydrogen Inorganic materials 0.000 title claims description 34
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims description 32
- 229910045601 alloy Inorganic materials 0.000 title claims description 18
- 239000000956 alloy Substances 0.000 title claims description 18
- 230000035699 permeability Effects 0.000 title claims description 9
- 238000000034 method Methods 0.000 title claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 239000011651 chromium Substances 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 229910001120 nichrome Inorganic materials 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- -1 alloy steels Chemical class 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000599 Cr alloy Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000788 chromium alloy Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
Definitions
- This invention relates to metal containers for holding hydrogen at elevated temperatures and to a method for treating metals to reduce the permeability thereof by hydrogen at elevated temperatures.
- alloys comprising iron, nickel and chromium, such as stainless steel, etc. when heated at an elevated temperature in contact with hydrogen for a prolonged period of time become gradually less permeable by hydrogen and after prolonged heating in contact with hydrogen for several days their permeability by hydrogen may be reduced one hundrediold or more.
- the temperature used should not be substantially less than that at which the gas is fully mobile with the metal being treated. In general, this temperature is about 600 C. In the treatment of such alloys I have obtained good results by heating at a temperature between about 600 C. and 900 C. but I prefer to employ a temperature of about 800 C. A higher temperature may be used but usually is not necessary.
- the advantageous results thus obtained can be destroyed to a large extent if the heated metal is exposed to air at room temperature and to a greater extent if the treated metal is exposed to air while heated at an elevated temperature. Therefore, in order to preserve the imparted property of low permeability by hydrogen, the treated metal or the treated fabricated article or at least one surface thereof should be kept in an environment free of oxygen, such for example as hydrogen, argon or other monatomic gas.
- the invention is illustrated further by the following specific examples showing the difiusion rate of hydrogen through specific iron, nickel and chromium alloys.
- the difiusion rate was measured with a mercury slug flow meter which was connected by a hermetically sealed connection to one end of the metal tube being tested.
- a thermocouple well of silica was inserted through the other end and the latter was hermetically sealed.
- Example 2 In this example, after heating the 304-Alloy stainless steel tube for 78 hours, the tube was cooled to room temperature, the hydrogen pumped out and air admitted for thirty minutes. It was then evacuated, filled with hydrogen and heated at 800 C. The difiusion rate now was 0.0434 cc./cm. /hr. The hydrogen in the tube then was replaced by air and the tube heated about minutes at 800 C. The air in the tube then was replaced by hydrogen and the tube heated at 800 C. for about twenty hours and the diffusion rate was 0.0650 cc./cm. /hr.
- Example 3 In this example, a 3l6-Alloy stainless steel tube was treated.
- the hydrogen loss is given as cubic centimeters of hydrogen at room tempera Nichrome ture per square centimeter of surface per hour per millimeter of thickness.
- Example 4 In this example, a 347 -A11oy stainless steel tube was treated. The hydrogen loss is given in the same terms indicated in Example 3.
- Example 5 13-1055 7 7 Hours heated gig fgp era Example 5
- a Nichrome tube was treated.
- the hydrogen loss is given in the same terms indicated in Examples 3: and 4.
- the method for reducing the permeability of an alloy by hydrogen which comprises heating the alloy in an atmosphere consisting essentially of hydrogen at a temperature not less than about 600 C. for a period of time not less than 24 hours, said alloy comprising iron, nickel, chromium and not more than about 0.10 per cent carbon.
- the method for reducing the permeability of an alloy by hydrogen which comprises heating the alloy in an atmosphere consisting essentially of hydrogen at a temperature not less than about 600 C. for a period of time not less than 24 hours, said alloy comprising iron, nickel, chromium and not more than about one per cent columbium.
- the method for reducing the permeability of an alloy by hydrogen which comprises heating the alloy in an atmosphere consisting essentially of hydrogen at a temperature not less than about 600 C. for a period of time not less than 24 hours, said alloy comprising iron, nickel, chromium and between about 1.75 to 2.50 per cent molybdenum.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Heat Treatment Of Articles (AREA)
Description
Patented Aug. 3, 1954 UNITED STATES 1' OFFICE I METHOD FOR REDUCING THE PERMEA- BILITY F ALLOYS BY HYDROGEN States Atomic Energy Commission No Drawing. Application January 5, 1952, Serial No. 265,207
Claims.
This invention relates to metal containers for holding hydrogen at elevated temperatures and to a method for treating metals to reduce the permeability thereof by hydrogen at elevated temperatures.
It is well known that metals, such as alloy steels, Nichrome, etc., commonly used for hydrogenation equipment and other hydrogen containers, laboratory equipment, etc. are permeable by hydrogen at elevated temperatures resulting in large loss of hydrogen from such equipment. Because of such losses, the determinations of the dissociation temperatures, etc. of many compounds which evolve hydrogen at elevated temperatures have varied greatly and have been unreliable or only approximate.
I have discovered that alloys comprising iron, nickel and chromium, such as stainless steel, etc., when heated at an elevated temperature in contact with hydrogen for a prolonged period of time become gradually less permeable by hydrogen and after prolonged heating in contact with hydrogen for several days their permeability by hydrogen may be reduced one hundrediold or more. The temperature used should not be substantially less than that at which the gas is fully mobile with the metal being treated. In general, this temperature is about 600 C. In the treatment of such alloys I have obtained good results by heating at a temperature between about 600 C. and 900 C. but I prefer to employ a temperature of about 800 C. A higher temperature may be used but usually is not necessary. I have further discovered that the advantageous results thus obtained can be destroyed to a large extent if the heated metal is exposed to air at room temperature and to a greater extent if the treated metal is exposed to air while heated at an elevated temperature. Therefore, in order to preserve the imparted property of low permeability by hydrogen, the treated metal or the treated fabricated article or at least one surface thereof should be kept in an environment free of oxygen, such for example as hydrogen, argon or other monatomic gas.
, The invention is illustrated further by the following specific examples showing the difiusion rate of hydrogen through specific iron, nickel and chromium alloys. In each of these examples the difiusion rate was measured with a mercury slug flow meter which was connected by a hermetically sealed connection to one end of the metal tube being tested. A thermocouple well of silica was inserted through the other end and the latter was hermetically sealed. The tube Element 304-Al1oy 3l6-A11oy 347-Alloy 0 08 max 0.10 max... 0.10 max-.. 0. l0 2 00 max 2.00 max... 2.00 max... 1 00 max... 1.00 max.-. 0 04 max 0.04max...
. 0.04max...
Molybdenum. Columbium- Iron Example 1 In this example the material treated was a 304-Alloy stainless steel tube having a Wall thickness of 0.9 mm. (0.036"). The hydrogen loss as indicated is cubic centimeters of hydrogen at room temperature per square centimeter of surface per hour.
H-loss T m er Hours heated cc./cm. /hr. tu s? 1 Example 2 In this example, after heating the 304-Alloy stainless steel tube for 78 hours, the tube was cooled to room temperature, the hydrogen pumped out and air admitted for thirty minutes. It was then evacuated, filled with hydrogen and heated at 800 C. The difiusion rate now was 0.0434 cc./cm. /hr. The hydrogen in the tube then was replaced by air and the tube heated about minutes at 800 C. The air in the tube then was replaced by hydrogen and the tube heated at 800 C. for about twenty hours and the diffusion rate was 0.0650 cc./cm. /hr.
Example 3 In this example, a 3l6-Alloy stainless steel tube was treated. The hydrogen loss is given as cubic centimeters of hydrogen at room tempera Nichrome ture per square centimeter of surface per hour per millimeter of thickness.
H-loss Tempera- Hours heated ccJcmJl mm./hr. o
Ewample 4 In this example, a 347 -A11oy stainless steel tube was treated. The hydrogen loss is given in the same terms indicated in Example 3.
13-1055 7 7 Hours heated gig fgp era Example 5 In this example, a Nichrome tube was treated. The hydrogen loss is given in the same terms indicated in Examples 3: and 4.
Q 7 H-loss I Tempera- Hours heated tum, a
heating the steel in an atmosphere consisting essentially of hydrogen at a temperature not less than about 600 C. for a period of time not less than about 24 hours.
3. The method for reducing the permeability of an alloy by hydrogen which comprises heating the alloy in an atmosphere consisting essentially of hydrogen at a temperature not less than about 600 C. for a period of time not less than 24 hours, said alloy comprising iron, nickel, chromium and not more than about 0.10 per cent carbon.
4. The method for reducing the permeability of an alloy by hydrogen which comprises heating the alloy in an atmosphere consisting essentially of hydrogen at a temperature not less than about 600 C. for a period of time not less than 24 hours, said alloy comprising iron, nickel, chromium and not more than about one per cent columbium.
5. The method for reducing the permeability of an alloy by hydrogen which comprises heating the alloy in an atmosphere consisting essentially of hydrogen at a temperature not less than about 600 C. for a period of time not less than 24 hours, said alloy comprising iron, nickel, chromium and between about 1.75 to 2.50 per cent molybdenum.
References Cited in the file of this patent UNITED STATES PATENTS Heat Treatment of Stainless Steels, page 13, published by Rustless Iron and Steel Corp, Baltimore, Md.
Claims (1)
1. THE METHOD FOR REDUCING THE PERMEABILITY OF AN ALLOY BY HYDROGEN WHICH COMPRISES HEATING THE ALLOY IN AN ATMOSPHERE CONSISTING ESSENTIALLY OF HYDROGEN AT A TEMPERATURE NOT LESS THAN ABOUT 600* C. FOR A PERIOD OF TIME NOT LESS THAN ABOUT 24 HOURS, SAID ALLOY COMPRISING IRON, NICKEL AND CHROMIUM.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US265207A US2685546A (en) | 1952-01-05 | 1952-01-05 | Method for reducing the permeability of alloys by hydrogen |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US265207A US2685546A (en) | 1952-01-05 | 1952-01-05 | Method for reducing the permeability of alloys by hydrogen |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2685546A true US2685546A (en) | 1954-08-03 |
Family
ID=23009482
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US265207A Expired - Lifetime US2685546A (en) | 1952-01-05 | 1952-01-05 | Method for reducing the permeability of alloys by hydrogen |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2685546A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2732092A (en) * | 1956-01-24 | Closure device | ||
| US4797252A (en) * | 1986-09-19 | 1989-01-10 | Crucible Materials Corporation | Corrosion-resistant, low-carbon plus nitrogen austenitic stainless steels with improved machinability |
| US4884708A (en) * | 1987-10-26 | 1989-12-05 | Mannesmann Ag | Pressure vessel |
| US5152452A (en) * | 1992-03-10 | 1992-10-06 | York Industries, Inc. | Pressure vessel and method |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1829118A (en) * | 1926-04-01 | 1931-10-27 | Krupp Ag | Process for making steel insensible to the action of hot gases and vapors |
| US1876091A (en) * | 1929-04-23 | 1932-09-06 | Krupp Ag | Steel article insensible to the action of hot gases, vapors, and liquids |
| US2057518A (en) * | 1934-08-21 | 1936-10-13 | Int Nickel Co | Apparatus for bright annealing metallic products |
| US2395608A (en) * | 1943-12-10 | 1946-02-26 | United States Steel Corp | Treating inherently precipitationhardenable chromium-nickel stainless steel |
| US2486283A (en) * | 1946-04-24 | 1949-10-25 | American Steel & Wire Co | Heat-treatment for high carbon high chromium steel |
| US2557862A (en) * | 1947-11-19 | 1951-06-19 | Armco Steel Corp | Internal-combustion engine valve |
| US2587613A (en) * | 1948-12-02 | 1952-03-04 | Crucible Steel Company | High temperature high strength alloys |
-
1952
- 1952-01-05 US US265207A patent/US2685546A/en not_active Expired - Lifetime
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1829118A (en) * | 1926-04-01 | 1931-10-27 | Krupp Ag | Process for making steel insensible to the action of hot gases and vapors |
| US1876091A (en) * | 1929-04-23 | 1932-09-06 | Krupp Ag | Steel article insensible to the action of hot gases, vapors, and liquids |
| US2057518A (en) * | 1934-08-21 | 1936-10-13 | Int Nickel Co | Apparatus for bright annealing metallic products |
| US2395608A (en) * | 1943-12-10 | 1946-02-26 | United States Steel Corp | Treating inherently precipitationhardenable chromium-nickel stainless steel |
| US2486283A (en) * | 1946-04-24 | 1949-10-25 | American Steel & Wire Co | Heat-treatment for high carbon high chromium steel |
| US2557862A (en) * | 1947-11-19 | 1951-06-19 | Armco Steel Corp | Internal-combustion engine valve |
| US2587613A (en) * | 1948-12-02 | 1952-03-04 | Crucible Steel Company | High temperature high strength alloys |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2732092A (en) * | 1956-01-24 | Closure device | ||
| US4797252A (en) * | 1986-09-19 | 1989-01-10 | Crucible Materials Corporation | Corrosion-resistant, low-carbon plus nitrogen austenitic stainless steels with improved machinability |
| US4884708A (en) * | 1987-10-26 | 1989-12-05 | Mannesmann Ag | Pressure vessel |
| US5152452A (en) * | 1992-03-10 | 1992-10-06 | York Industries, Inc. | Pressure vessel and method |
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