US2548187A - Method of determining the oxygen content of copper - Google Patents
Method of determining the oxygen content of copper Download PDFInfo
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- US2548187A US2548187A US605950A US60595045A US2548187A US 2548187 A US2548187 A US 2548187A US 605950 A US605950 A US 605950A US 60595045 A US60595045 A US 60595045A US 2548187 A US2548187 A US 2548187A
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- copper
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- oxygen
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims description 20
- 229910052760 oxygen Inorganic materials 0.000 title claims description 20
- 239000001301 oxygen Substances 0.000 title claims description 20
- 238000000034 method Methods 0.000 title claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title description 37
- 229910052802 copper Inorganic materials 0.000 title description 36
- 239000010949 copper Substances 0.000 title description 36
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical class [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 230000002939 deleterious effect Effects 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 5
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 4
- 241001124569 Lycaenidae Species 0.000 description 3
- 235000014987 copper Nutrition 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 229910052714 tellurium Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 1
- 229940112669 cuprous oxide Drugs 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/202—Constituents thereof
- G01N33/2022—Non-metallic constituents
- G01N33/2025—Gaseous constituents
Definitions
- a sample of copper is heated in a hydrogen atmosphere or a reducing atmosphere containing a relatively large amount of hydrogen and then cooled in the same atmosphere. Prior to heating the sample, it is measured to determine its diameter and, after the heating and cooling in the reducing atmosphere, it is again measured. ItV has been found that copper containing oxygen will grow when heated to elevated temperatures in the presence of hydrogen, apparently due to the formation of voids at the grain boundaries when the oxygen and hydrogen y combine.
- copper rods of from as smallras .25" in diameter to as large as approximately .8 in diameter and just under one inch long are heated to' an elevated temperature in the presence of either pure hydrogen or a gas such as ammo gas containing '75% H2, 25% N at temperatures from'1550" F. to1850 F. and then are cooled in the same atmosphere, whereupon a comparison of the diameter ofthe samples prior to and after heat treat- 'ing' will indicate whether or not there is oxygen at the grain boundaries and'probably some of it escapes as steam, leaving voids at the boundaries.
- the combining of thehydrogen and oxygen at these high temperatures will form steam which requires more space than the oxides, thus leaving the voids and increasing the overall dimensions of the sample.
- the percent increase in diameter of; tough pitch copper when treated at temperatures ranging from 1550 F. to 1850 F. in atmospheres containing principally hydrogen, gradually increases from approximately 1.29% to approximately 2.04%. This apparently indicates that as the treating temperature is raised, the amount of expansion or growth of the sample increases progressively. However, there is a limit to the temperature which may be used since somewhere j-ust above 1850 the copper becomes so plastic as it approaches the molten stage that the measurement oi it would not be accurate.
- the samples of tough pitch copper tested were approximately- 1/2" in diameter and almost one inch in length and their growth in diameter followed the line l.
- a number of phosphorous deoxidized copper samples having some tellurium in them were tested under the same temperature and atmospheric conditions and they Yexhibited a growth from where their percentage of increase in diameter, after heat treatment, and cooling, ranged from .458% at 15.50 F. to 1.65% at 1850 F., as indicated by the line 2.
- a number of samples of oxygen-free high conductivity copper oontaining a small amount of tellurium changed in diameter from an increase of from .04% at 1550 F. to a maximum of .128% at. 185.0 F., as indicated by the line 5.
- vated temperatures in a hydrogen atmosphere and it, is also believed to be iair to, assumer that a.
- Small amount of oxygen in Copper will cause the copper tov increase in size, when treated as described hereinbeiore.
- the copper increases in diameter less than .20%, it is acceptable and does not warp or become embrittled to a detectable extent when used in the manufacture of electrical apparatus which is later treated ina hydrogen atmosphere.
- the method of determining the deleterious effect of the oxygen content of copper which comprises determining the dimensions of a sample of copper, heating said sample to from approximately 1550 F. to approximately 1850 F. for from fteen to twenty minutes, cooling the sample to room temperature, maintaining a hydrogen atmosphere around the sample during the heating and cooling, and then again determining said dimensions to indicate variations in said measurement above and below .20% of the original dimensions.
- the method of grading various samples of coppers in cylindrical form by determining the deleterious eiect of the oxygen content in each sample, which comprises determining the diameter of each sample of copper, heating each sample to from approximately 1550 F. to approximately 1850" F. for from fifteen to twenty minutes, cooling each sample to room temperature, maintaining a hydrogen atmosphere around each sample during the heating and cooling, and then again determining said diameters to ascertain whether the percent increase in diameter for each sample falls below a predetermined value.
- the method of grading coppers by determining the deleterious effect of the oxygen content in various samples of the. coppers, which comprises determining a particular dimension of each sample of copper, heating each of said samples to a predetermined temperature within the range of 1550 F. to approximately 1850 F. for from fteen to twenty minutes, cooling each sample to room temperature, maintaining a reducing atmosphere Vcontaining hydrogen around each sample during the heating and cooling, and then again determining said dimension of each individual sample to ascertain the percent change in size relative to a predetermined value to determine the grading of each sample.
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- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Description
$235353??? `\co, ,vw
TELLuR/UM c. M, ANDERSON 4Err AL Filed my 19, 1945 THF@ wmu METHOD OF DETERMINING THE OXYGEN CONTENT 0F' COPPER April 10, 1951 w. M/ mmmwm New m @MLM MM40. f Raw Patented Apr. 10, 1951 UNITED STATES PATENT OFFICE v METHOD OF DETERMINING THE OXYGEN CONTENT OF COPPER Carl M. Anderson, Chicago, Robert A. Harris, Oak Park, and Charles C. Patton, Chicago, Ill., assignors to Western Electric Company, Incorporated, New York, N. Y.
York
, a corporation of New Application July 19, 1945, Serial No. 605,950
3 Claims. (Cl. 23-230) This invention relatesto a method of determining the oxygen content of copper. l
In the manufacture of some articles from copper, it becomes necessary to braze or treat the articles in a reducing atmosphere as a step incident to the manufacture of the articles. In such articles, the presence of even very small quantities of oxygen in the copper cause warping of the copper parts and, as a consequence of this distortion, the articles are defective. Accordingly, it has become of primary importance to determine the purity of copper to be used in such processes.
It is an object of the present invention to provide a method of determining oxygen in the copper.
In accordance'with one embodiment of the invention, a sample of copper is heated in a hydrogen atmosphere or a reducing atmosphere containing a relatively large amount of hydrogen and then cooled in the same atmosphere. Prior to heating the sample, it is measured to determine its diameter and, after the heating and cooling in the reducing atmosphere, it is again measured. ItV has been found that copper containing oxygen will grow when heated to elevated temperatures in the presence of hydrogen, apparently due to the formation of voids at the grain boundaries when the oxygen and hydrogen y combine.
A complete understanding of the invention may be had'by reference to the following detailed description when considered in conjunction with the accompanying drawing, wherein the single gure illustrates graphically the percent oi in-y crease in diameter of various commercial brands of pure copper when treated in accordance with the present invention. f
In accordance with theY present invention, copper rods of from as smallras .25" in diameter to as large as approximately .8 in diameter and just under one inch long are heated to' an elevated temperature in the presence of either pure hydrogen or a gas such as ammo gas containing '75% H2, 25% N at temperatures from'1550" F. to1850 F. and then are cooled in the same atmosphere, whereupon a comparison of the diameter ofthe samples prior to and after heat treat- 'ing' will indicate whether or not there is oxygen at the grain boundaries and'probably some of it escapes as steam, leaving voids at the boundaries. The combining of thehydrogen and oxygen at these high temperatures will form steam which requires more space than the oxides, thus leaving the voids and increasing the overall dimensions of the sample.
Examination of copper treated in this manner when a microsection is examined at a suitable magnication, such as 75X, shows voids at the v grain boundaries, which probably-accountsfor Commercial electrolytic copper, known as` I tough pitch copper, is known to contain from approximately .03% to approximately .05% of cuprous oxide and for most manufacturing purposes, Where a high degree of conductivity is required, copper containing -a maximum of .07% of oxygen is acceptable. However, in the manufacture of some parts which are later to be treated in a reducing atmosphere, the amount of oxygen in commercially pure or electrolytic copper is too great and the parts to be manufactured become embrittled and warped, whereas the material known as oxygen-free high conductivity copper is suiliciently low in its oxygen content so that no deleterious embrittlement or warping will occur when parts made from this vmaterial are treated in reducing atmospheres,
the dimensional growthofthe samples. It has been further noticed inthe course of experiments that the diameter of a rod exhibits a vmuch greater tendency Yto growithan a comparable length of rod. This apparently has resulted from'the distortion of the grain structure in the formation of the rod, thus providing more boundaries in the cross-sectional area of the rod Yfor a given dimension than in the length of the phorous deoxidized copper containing a small amount of tellurium, andthe product known asV tested. The samples tested indicated that growth occurs when there is oxygen present in the samples.
As indicated in the drawing, the percent increase in diameter of; tough pitch copper, when treated at temperatures ranging from 1550 F. to 1850 F. in atmospheres containing principally hydrogen, gradually increases from approximately 1.29% to approximately 2.04%. This apparently indicates that as the treating temperature is raised, the amount of expansion or growth of the sample increases progressively. However, there is a limit to the temperature which may be used since somewhere j-ust above 1850 the copper becomes so plastic as it approaches the molten stage that the measurement oi it would not be accurate. The samples of tough pitch copper tested were approximately- 1/2" in diameter and almost one inch in length and their growth in diameter followed the line l.
A number of phosphorous deoxidized copper samples having some tellurium in them were tested under the same temperature and atmospheric conditions and they Yexhibited a growth from where their percentage of increase in diameter, after heat treatment, and cooling, ranged from .458% at 15.50 F. to 1.65% at 1850 F., as indicated by the line 2. A number of samples of oxygen-free high conductivity copper oontaining a small amount of tellurium changed in diameter from an increase of from .04% at 1550 F. to a maximum of .128% at. 185.0 F., as indicated by the line 5.
In tests where the same conditions were.. maintained, a number of samplesy of oxygen-free high conductivity copper treated at 1550 F., 160'?e 1650 F., 1750 F., and 1850 F. were measured and three of the samples, as indicated by the encircled dots at. 3, apparently shrunk, whereas four samples, as indicated by the. encircled dots 4, apparently maintained exactly the same diameter. This is believed to indicate that the oxygen-free high conductivity copper did not grow in size and, inasmuch as the, three samples which apparently shrunk are within the range of accuracy of the measurements made, it. is safe. to assume that there will be no Change in size of copper samples which are free from oxygen when the copper is treated at. the ele.-
vated temperatures in a hydrogen atmosphere and it, is also believed to be iair to, assumer that a. Small amount of oxygen in Copper will cause the copper tov increase in size, when treated as described hereinbeiore. When the copper increases in diameter less than .20%, it is acceptable and does not warp or become embrittled to a detectable extent when used in the manufacture of electrical apparatus which is later treated ina hydrogen atmosphere.
What is claimed is:
1. The method of determining the deleterious effect of the oxygen content of copper which comprises determining the dimensions of a sample of copper, heating said sample to from approximately 1550 F. to approximately 1850 F. for from fteen to twenty minutes, cooling the sample to room temperature, maintaining a hydrogen atmosphere around the sample during the heating and cooling, and then again determining said dimensions to indicate variations in said measurement above and below .20% of the original dimensions.
2. The method of grading various samples of coppers in cylindrical form by determining the deleterious eiect of the oxygen content in each sample, which comprises determining the diameter of each sample of copper, heating each sample to from approximately 1550 F. to approximately 1850" F. for from fifteen to twenty minutes, cooling each sample to room temperature, maintaining a hydrogen atmosphere around each sample during the heating and cooling, and then again determining said diameters to ascertain whether the percent increase in diameter for each sample falls below a predetermined value.
3. The method of grading coppers by determining the deleterious effect of the oxygen content in various samples of the. coppers, which comprises determining a particular dimension of each sample of copper, heating each of said samples to a predetermined temperature within the range of 1550 F. to approximately 1850 F. for from fteen to twenty minutes, cooling each sample to room temperature, maintaining a reducing atmosphere Vcontaining hydrogen around each sample during the heating and cooling, and then again determining said dimension of each individual sample to ascertain the percent change in size relative to a predetermined value to determine the grading of each sample.
CARL M. ANDERSON. ROBERT A. HARRIS. CHARLES C. PATTON.
REFERENCES CITED The following references are of record in the le of this patent:
N.l B. Pilling, Action of Reducing Gases on Hot Solid Copper, Trans. A. I. M. E. 1919, vol. 60, p. 3.22.
Metals Handbook, American Society for Metals, 1939, Cleveland, Qhio, p. 1391.
Rhines et al., Trans. A. I, M, E., vol. 143, 1941, pages S12-325.
Claims (1)
1. THE METHOD OF DETERMINING THE DELETERIOUS EFFECT OF THE OXYGEN CONTENT OF COPPER WHICH COMPRISES DETERMINING THE DIMENSIONS OF A SAMPLE OF COPPER, HEATING SAID SAMPLE TO FROM APPROXIMATELY 1550* F. TO APPROXIMATELY 1850* F. FOR FROM FIFTEEN TO TWENTY MINUTES, COOLING THE SAMPLE TO ROOM TEMPERATURE, MAINTAINING A HYDROGEN ATMOSPHERE AROUND THE SAMPLE DURING THE HEATING AND COOLING, AND THEN AGAIN DETERMINING SAID DIMENSIONS TO INDICATE VARIATIONS IN SAID MEASUREMENT ABOVE AND BELOW 20% OF THE ORIGINAL DIMENSIONS.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US605950A US2548187A (en) | 1945-07-19 | 1945-07-19 | Method of determining the oxygen content of copper |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US605950A US2548187A (en) | 1945-07-19 | 1945-07-19 | Method of determining the oxygen content of copper |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2548187A true US2548187A (en) | 1951-04-10 |
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ID=24425888
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US605950A Expired - Lifetime US2548187A (en) | 1945-07-19 | 1945-07-19 | Method of determining the oxygen content of copper |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2901327A (en) * | 1955-05-23 | 1959-08-25 | Beckman Instruments Inc | Method for measuring traces of dissolved oxygen |
| US3118736A (en) * | 1959-06-30 | 1964-01-21 | Fisher Scientific Co | Method for blood gas analysis |
-
1945
- 1945-07-19 US US605950A patent/US2548187A/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| None * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2901327A (en) * | 1955-05-23 | 1959-08-25 | Beckman Instruments Inc | Method for measuring traces of dissolved oxygen |
| US3118736A (en) * | 1959-06-30 | 1964-01-21 | Fisher Scientific Co | Method for blood gas analysis |
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