IL30770A - Preparation of self-supporting films of oxides of refracting metals - Google Patents
Preparation of self-supporting films of oxides of refracting metalsInfo
- Publication number
- IL30770A IL30770A IL30770A IL3077068A IL30770A IL 30770 A IL30770 A IL 30770A IL 30770 A IL30770 A IL 30770A IL 3077068 A IL3077068 A IL 3077068A IL 30770 A IL30770 A IL 30770A
- Authority
- IL
- Israel
- Prior art keywords
- metal
- film
- structure according
- blank
- thickness
- Prior art date
Links
- 229910052751 metal Inorganic materials 0.000 title claims description 25
- 239000002184 metal Substances 0.000 title claims description 25
- 150000002739 metals Chemical class 0.000 title description 3
- 238000002360 preparation method Methods 0.000 title description 2
- 239000010408 film Substances 0.000 claims description 51
- 150000004706 metal oxides Chemical class 0.000 claims description 21
- 229910044991 metal oxide Inorganic materials 0.000 claims description 17
- 230000005855 radiation Effects 0.000 claims description 7
- 230000002285 radioactive effect Effects 0.000 claims description 7
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 7
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052721 tungsten Inorganic materials 0.000 claims description 7
- 239000010937 tungsten Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 5
- 239000003792 electrolyte Substances 0.000 claims description 5
- 229910052715 tantalum Inorganic materials 0.000 claims description 5
- 239000002775 capsule Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 239000010955 niobium Substances 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 3
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 3
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 2
- -1 ammonium halide Chemical class 0.000 claims 1
- 239000011888 foil Substances 0.000 claims 1
- 230000001427 coherent effect Effects 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000007743 anodising Methods 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229910052705 radium Inorganic materials 0.000 description 2
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 0.000 description 2
- 231100000241 scar Toxicity 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000013013 elastic material Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- VVRQVWSVLMGPRN-UHFFFAOYSA-N oxotungsten Chemical group [W]=O VVRQVWSVLMGPRN-UHFFFAOYSA-N 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J5/00—Details relating to vessels or to leading-in conductors common to two or more basic types of discharge tubes or lamps
- H01J5/02—Vessels; Containers; Shields associated therewith; Vacuum locks
- H01J5/18—Windows permeable to X-rays, gamma-rays, or particles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J47/00—Tubes for determining the presence, intensity, density or energy of radiation or particles
Landscapes
- Measurement Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
Description
metal oxide structures and their manufacture STATE OF invention relates to a metal oxide structure in which the film consists of the oxide of one of the metals tungsten or Films of these oxides have been for in electrolytic For this use the oxide film has produced as a coating on a support of the same anodizing the metal All these known metal oxide are supported by the metal support over their entire invention has the object to provide metal oxide film structures including a thin film of an oxide of one of the metals or in which a substantial part of the area of the oxide unencumbered by the The invention consis s in a metal oxide film structure comprising a thin film of an oxide of tungsten or which film is integral at its edges with a rigid frame of the metal of which the film an oxide and freely spans the space enclosed by the the oxide film having a thickness not exceeding an order of magnitude A o of about angstrom and being permeable to radioactive radiation but meable to electrically uncharged gas In connection with this invention the term means coherent film which is impermeable to uncharged gas molecules but permeable to especially radioactive radiation includin and The thickness of the film is of the order of of to The absence of a support over a large area of the oxide film enables these metal oxide film structures to be used for various purposes where the use of a metal oxide is most advantageous but such films could not be used up to now owing to the presence of the metal support over the entire She metal oxide film structures of the invention for excellent radiation windows of capsules containing radium or other radioactive of the mica films used hitherto for this which are more expensive to make and less resistant to the deleterious effects of the In radiation counters the metal oxide structures according to the invention can advantageously be used as a window instead of the conventional alumlnized polyester In this metal oxide film is much more resistant to the effects of the radiation than the polyester In electrolytic cells the metal oxide structures according to the invention with great replace the conventional parchment in the anodic oxidation of organic invention for films on tantalum metal metal is and films on zirconium metal The metal oxide film will as a rule be the invention also contemplates other The invention also provides a method for the manufacture of metal oxide film structures of the kind set out which comprises the steps providing a shaped blank of Sr applying to one surface of the blank a mask in a central portion of tha submitting the masked blank to a first electrolytic operation at a voltage in the range from 6 to 520 volts for producing a thin oxide film on the surface and edge areas of the blanks removing the mask from the submitting the connected as to a second electrolytic operation at a voltage which is in the range from 1 to 20 volts and does not exceed about the voltage used in the first electrolytic and continuing the second electrolytic operation until all the metal not oxidized the electrolytic operation dissolved f om the unmasked area of the previously masked surface of the blank through the thickness of the blank until the inner of the metal oxide at the opposite surface of the In the first electrolytic which is a conventional anodizing a coherent metal oxide film is formed on the whole of the surface of the on the edge of the and on the marginal part of the masked The metal enclosed between the marginal parts of both surfaces and the edge of the blank Is not attacked in the second electrolytic operation but reaaine intact in the form of a frame integral with the oxide The blank may have any desired suitable circular or according to the contemplated retains the form of the a circular blank produces an annular a square blank a square and so Where the oxide film is to be both surfaces of the blank are plane and for a film is one surface of the blank one which is not masked in the will be cambered It found that a particularly advantageous electrolyte for use in the second electrolytic operation is a saturated or halide solution where water content does not exceed by he metal halide is preferably an alkali metal or ammonium The mask may for a piece o adhesive teflon or the Any other means may be used an of an adequately elastic material resistant to the enclosing the area of the blank to be masked and tightly pressed against the of the blank by any suitable Since the in its use as an anode in both electrolytic has to be held and to be connected with the current a preferred feature of the invention provides to make the blank initially integral with a tail or stem laterally from the which serves as a holder and a will be cut off at the edge of the blank after the second electrolytic cutting remains not covered by the oxide but this fact does not interfere with any contemplated use of the structure since the scar is located on the edge while all usee ed a a the oxide The accompanying drawings illustrate the invention by way 1 is a side view of a blank with tail according to either 2 2 is a plan view of a circular is a plan view of a 4 shows the underside of the blank of 2 with a mask applied 5 is a on line of of the same blank after the first electrolytic 6 is a similar to of the same blank after the removal of the 7 shows similarly the same blank after the second electrolytic 8 shows similarly the finished metal oxide film 9 is an axial section of a radium capsule whose window is ormed by the metal oxide film structure of The blank of 1 is a disc 1 made integrally with a tail 2 shows a disc la which is The tail projects laterally from the edge in a radial In the case of a square disc as shown in the tail projects at right angles from the middle of one of the side The blanks of 2 and 3 are made of one of the metal tungsten or 4 shows a blank according to 2 with circular mask 3 applied to one of the surfaces of the may for of an adheeive tape of It must be impermeable to the electrol tes used in the electrolytic By the first electrolytic operation the disc of 4 is covered with an oxide comprising a part covering the whole a part covering the and a part covering the marginal part of the masked The parts 4b and 4c of the film form a coherent The tail 2 is not covered by an oxide f lm since it stays clear of the In the stage illustrated by 6 the mask has been removed and the blank is then submitted to the second electrolytic This dissolves a circular disc of metal whose surface area is identloal with the area of the previously masked surface while its thickness the same as that of the remaining metal That the dissolution of the metal goes through to the inner side of the surface part of the oxide The edge portion of the metal enclosed between the oxide film parts 4b and remains unaffected by the electrolytic operation and forms a ring which constitutes a structural the metal oxide the tail 2 is cut whereby the finished structur of 8 produced At the place where the tail 2 has been severed from the there remains a blank metal not covered by the metal The scar cannot be seen in 9 illustrates the use of a structure according comprises a metal block 5 with a cavity 6 which accommodates the radioactive preparation cavity is covered with a structure according to has been referred to generally by the arrow The structure is tightened against the capsule by any suitable conventional means which have not been illustrated since they are The invention is illustrated by the following Examples Example 1 A tantalum mm thick and mm in diameter and integrally made with a of mm length corresponding to is decreased by flushing with then immersed for 30 minutes in a concentrated aqueous solution and thereafter rinsed with a large amount of The mask is applied to the disc and the disc is by of its tail 2 which serves as a holder and as the anode in an electrolytic circuit which comprises a platinum cathode and an electrolyte constituted by a aqueous boric acid A potentia is applied with a current density of 10 and a voltage of 200 At this magnitude the voltage is set constant and the current density is allowed to drop below mi By this a coherent tantalum oxide film is formed in the parts of the disc Then the blank is removed from the the mask 3 removed and the blank is connected as the anode in a oiroult having a platinum cathode and an electrolyte alcohol content by A current density of 50 at a voltage of 10 volts is and the disc is left in the electrolyte until all the metal except the ring enclosed by the parts 4c of the oxide film has dissolved There remains merely a ring of metal which forms a structural support of the tantalum oxide film thickness o the film is about 3000 Example 2 A niobium blank of the same size and shape as the tantalum blank of Bxample 1 is subjected to the same treatment as described in Bxample In the niobium oxide film structure thus produced the niobium oxide film has a thickness of about 5400 A tungsten blank of the same size and shape as the tantalum disc of Example 1 is subjected to the same treatment as described Example In the tungsten oxide structure thus produced the tungsten oxide not film has a thickness of about 4000 Bxample 4 A zirconium disc of the same size and shape as the tantalum disc of Bxample l is subjected to the same treatment as described in Example In the zirconium oxide film structure thus produced the zirconium oxide film has a thickness of about 4000 insufficientOCRQuality
Claims (2)
1. CLAIMS A metal oxide film structure comprising a thin film of an oxide of tungsten or which film is integral at its edges with a rigid frame of the metal of which the film is an and freely the space enclosed by the A structure according to Claim wherein oxide film has a thickness not exceeding an order of magnitude of about to radioactive radiation but impermeable to electrically uncharged gas A structure according to
2. Claim 2 wherein the thickness of 2 o film is of the order of magnitude from 10 to A structure according to any one of Claims 1 to wherein the frame consists of tantalum metal and the consists of tantalum A structure according to wherein the tantalum oxide film has a thickness of about A structure according to any one of 1 to wherein the frame consists of niobium metal and the film consists of niobium A structure according Claim wherein the niobium oxide a thickness of about A structure according to iany one of Claims 1 to wherein the frame consists of tungsten metal and the film consists of tungsten A structure according to Claim wherein the tungsten oxide a thickness of about 4000 A structure according to any one of Claims 1 to wherein the frame conslets of zirconium metal and the film consists of zirconium A structure according to Claim wherein the zirconium film has a thickness of about 4000 A method for the manufacture of metal oxide film structures according to y one of Claims 1 to which comprises the steps providing a blank of or Zr applying to one surface of the blank a mask in a central position of that submitting the masked as an to a first electrolytic operation for producing an oxide film on the surface and edge areas of the blankj removing mask from the and submitting the connected as to a second electrolytic operation until all the metal in the first electrolytic operation is dissolved from the unmasked area of the previously masked surface of the blank through the thickness of the blank until the inner side of the metal oxide film at the opposite surface of the A method according to Claim wherein a patch of adhesive foil is used as a A method according to 12 or wherein the electrolyte 221171 electrolytic operation is a saturated aqueous for solution of a metal hallde or ammonium halide A method according to any one of Claims 12 to wherein the rst electrolytic operation is carried out at a voltage in the range from to 320 volte for producing an oxide of a not about A method according to any one of Claims 12 to wherein the electrolytic operation is carried out at a voltage which is in the range from 1 to 20 volts and does not exceed about the voltage used in the first electrolytic A radioactive device comprising a capsule containing a radioactive and a radiation window constituted by a oxide film structure according to any one of Claims 1 to For the Applicants insufficientOCRQuality
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IL30770A IL30770A (en) | 1968-09-26 | 1968-09-26 | Preparation of self-supporting films of oxides of refracting metals |
| US859310A US3675021A (en) | 1968-09-26 | 1969-09-19 | Metal oxide film structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IL30770A IL30770A (en) | 1968-09-26 | 1968-09-26 | Preparation of self-supporting films of oxides of refracting metals |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| IL30770A0 IL30770A0 (en) | 1969-04-30 |
| IL30770A true IL30770A (en) | 1972-07-26 |
Family
ID=11044645
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| IL30770A IL30770A (en) | 1968-09-26 | 1968-09-26 | Preparation of self-supporting films of oxides of refracting metals |
Country Status (2)
| Country | Link |
|---|---|
| US (1) | US3675021A (en) |
| IL (1) | IL30770A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3970855A (en) * | 1975-05-23 | 1976-07-20 | The United States Of America As Represented By The Secretary Of The Navy | Positron probes for mechanical fatigue detection system |
| US20080014421A1 (en) * | 2006-07-13 | 2008-01-17 | Aharon Inspektor | Coated cutting tool with anodized top layer and method of making the same |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| LU36045A1 (en) * | 1957-05-04 | |||
| US2992726A (en) * | 1959-07-10 | 1961-07-18 | United Aircraft Corp | Specimen holder for radioactive samples |
| US3332859A (en) * | 1963-12-27 | 1967-07-25 | Gen Electric | Process for producing tantalum foil for capacitors |
| GB1131143A (en) * | 1964-12-17 | 1968-10-23 | British Cellophane Ltd | An improved x-ray gauging apparatus |
| US3488502A (en) * | 1966-06-02 | 1970-01-06 | Industrial Nucleonics Corp | Nonshifting radiation source capsule |
-
1968
- 1968-09-26 IL IL30770A patent/IL30770A/en unknown
-
1969
- 1969-09-19 US US859310A patent/US3675021A/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| IL30770A0 (en) | 1969-04-30 |
| US3675021A (en) | 1972-07-04 |
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