Joe Skulan
Member
- Joined
- Mar 10, 2016
- Messages
- 14
Hello. I am new here. I've read the guidelines and searched the archives, and I believe this topic is both new and appropriate for this forum.
I am exploring the possibility of fabricating osmium ingots or other objects that will not oxidize in room temperature air from osmium powder, without melting or sintering.
Before I write another word I need to say that I am fully aware of the hazards of osmium tetroxide, and would never actually attempt what I describe without adequate protection against those hazards. I have worked with hazardous materials, including the fantastically dangerous bromine pentafluoride, in well equipped labs and know what precautions are needed for this kind of thing. What I would like here is comments on the workability of process itself. The same process could be used for ruthenium, iridium, rhodium, and other rare refractory metals that are too brittle to machine.
OsO4 can be reduced to a crystalline metal by thermal decomposition of an OsO4-olefin complex. This process has been used to produce thin (ca 1000 Å) films of Os for mirrors, etc. In this work the goal was to produce the thinnest Os layer possible. What I would like to know is if the process could be modified to produce thicker layers, either in one step by the thermal decomposition of a larger volume of the OsO4-olefin complex, or by building up a thick layer by repeated deposition of thin films. I also wonder if Os crystals could be grown on a heated needle suspended in the OsO4-olefin complex.
The basic system would consist of a Os powder loaded into a quartz reaction chamber heated to 1000-1200°C. OsO4 would be generated by slowly passing O2 over the hot metal. The hot OsO4 gas would be cooled to below the boiling point and dissolved in tert-Butyl alcohol or hexamine. This allows OsO4 to be safely stored in a non-volatile form.
The OsO4 solution would then be dissolved in an olefin, like pinene, to form the OsO4-olefin complex, which would then be decomposed to Os metal at 300°C in a high-temperature plastic or ceramic mold (the ceramic could later be broken away and the ingot cleaned in HF).
If the thermal decomposition is done in a reducing atmosphere (H2, or an H2/argon mix) osmium recovery is quantitative. No OsO is generated.
Creating a 1mm thick layer of Os through deposition of a 1000 Å layer every three minutes would take about two weeks. Can anyone think of a way to speed this up?
Again, this is a general concept, not device I’m actually getting ready to build.
Comments?
I am exploring the possibility of fabricating osmium ingots or other objects that will not oxidize in room temperature air from osmium powder, without melting or sintering.
Before I write another word I need to say that I am fully aware of the hazards of osmium tetroxide, and would never actually attempt what I describe without adequate protection against those hazards. I have worked with hazardous materials, including the fantastically dangerous bromine pentafluoride, in well equipped labs and know what precautions are needed for this kind of thing. What I would like here is comments on the workability of process itself. The same process could be used for ruthenium, iridium, rhodium, and other rare refractory metals that are too brittle to machine.
OsO4 can be reduced to a crystalline metal by thermal decomposition of an OsO4-olefin complex. This process has been used to produce thin (ca 1000 Å) films of Os for mirrors, etc. In this work the goal was to produce the thinnest Os layer possible. What I would like to know is if the process could be modified to produce thicker layers, either in one step by the thermal decomposition of a larger volume of the OsO4-olefin complex, or by building up a thick layer by repeated deposition of thin films. I also wonder if Os crystals could be grown on a heated needle suspended in the OsO4-olefin complex.
The basic system would consist of a Os powder loaded into a quartz reaction chamber heated to 1000-1200°C. OsO4 would be generated by slowly passing O2 over the hot metal. The hot OsO4 gas would be cooled to below the boiling point and dissolved in tert-Butyl alcohol or hexamine. This allows OsO4 to be safely stored in a non-volatile form.
The OsO4 solution would then be dissolved in an olefin, like pinene, to form the OsO4-olefin complex, which would then be decomposed to Os metal at 300°C in a high-temperature plastic or ceramic mold (the ceramic could later be broken away and the ingot cleaned in HF).
If the thermal decomposition is done in a reducing atmosphere (H2, or an H2/argon mix) osmium recovery is quantitative. No OsO is generated.
Creating a 1mm thick layer of Os through deposition of a 1000 Å layer every three minutes would take about two weeks. Can anyone think of a way to speed this up?
Again, this is a general concept, not device I’m actually getting ready to build.
Comments?
