CA1194701A - Bulk production of alloys by deposition from the vapour phase and apparatus therefor - Google Patents

Bulk production of alloys by deposition from the vapour phase and apparatus therefor

Info

Publication number
CA1194701A
CA1194701A CA000392301A CA392301A CA1194701A CA 1194701 A CA1194701 A CA 1194701A CA 000392301 A CA000392301 A CA 000392301A CA 392301 A CA392301 A CA 392301A CA 1194701 A CA1194701 A CA 1194701A
Authority
CA
Canada
Prior art keywords
collector
alloy
reuseable
deposition
coating
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
Application number
CA000392301A
Other languages
French (fr)
Inventor
Robert L. Bickerdike
Garyth Hughes
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
UK Secretary of State for Defence
Original Assignee
UK Secretary of State for Defence
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by UK Secretary of State for Defence filed Critical UK Secretary of State for Defence
Application granted granted Critical
Publication of CA1194701A publication Critical patent/CA1194701A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0005Separation of the coating from the substrate
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/01Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching

Abstract

ABSTRACT
The invention relates to a process for the bulk production of alloy by deposition from the vapour phase and a reuseable collector for use therein. The collector employs a coating of solder alloy on the deposition surface such that after deposition has been completed the solder alloy may be melted and the depo-sited alloy removed from the collector without the necessity of destroying the collector. The process comprises coating the deposition surface of a collector with a solder alloy, depositing alloy vapour onto the solder alloy, melting the solder alloy coating and removing the deposited alloy from the collector.

Description

_~Y~

l 22762-38~

IMPROVEMENTS IN OR RELATING TO Tl-IE BULK PRODUC'['ION OF ~LLOYS BY DePOSI'I'ION FROM
THE VAPOUR PIIASE AND APPARATUS 'I'HEREFOR
This invention relates to the bulk production of alloy material by de-position from the vapour phase and in particular to the removal of deposited alloy from a collector used in such a process.
Presently evaporated alloys are produced by deposition of alloy vapour from an evaporator onto a collector. In the process described in UK
Patent Application Number 2,079,32~ ~published on January 20, 1982) the col-lector in the form of a rotating drum is positioned above the evaporator. Both the collector and the evaporator are housed within a vacuum or low pressure chamber. An unacceptable temperature rise at the surface of the deposited alloy is prevented by a combination of controlled cooling via the internal sur-face of the collector and also by control of the speed of rotation of the col-lector itself so that a particular area of the collector surface is not exposed over-long to the evaporating metal. Under conditions o~ controlled cooling and speed of rotation the collector is continuously rotated above the evaporator until the required thickness of deposit is obtained. The collector is then re-moved from the vacuum chamber and the collector itself machined from the de-posited alloy using a boring tool. The remaining deposit is -then cut into arcuate plates which may be formed into sheets by conventional metal working processes.
It will be appreciated that a major problem in such a process lies with the complete destruction of the collector.

~ ' JX/59~7/05 , 4'~

If the type of collector chosen for the process does not rely on gas-gap cooling assemblies for t~mperature control but on more conventional forms such as pipes carrying cooling fluid for example, then the interior of the collector drum will be far from a smooth bored cylinder and will in fact represent a major item of expenditure in terms of added value in machining time on attachment points for heaters, cooling pipes and heat conduction devices etc.
The present invention provides a collector which is re-usabl0 and which may be removed and re-installed within the VRcUUm chamber without a requirement to completely dismantle and re-fit the supporting shafts and temperature con~rol equipment.
According to the present invention a collector for use in a process for the bulk production of an alloy is coated with material having a melting temperature or temperature at which the onset of fusion occurs above the peak operating temperature at the deposition surface during operation of the process, such that on completion of deposition the material between the collector surface and the deposited alloy may be melted rendering the deposited alloy detachable from the collector.
According to a feature of the invention the collector is constructed such that minor movements of the deposited alloy due to localised thermal and mechanical stresses result in flexing of the collector surface and continuous metal-lurgicai and thermal contact between the collector surface and the deposited alloy.
Preferably the melting temperature or temperature at which the onset of fusion occurs of the coating material is below the temperature at which the onset of rapid, irreversible precipita-tion reactions will occur within the deposited alloy.
The deposited alloy may be removed from the collector by cutting the alloy into discrete slabs prior to removal from the 4~

collector. ~he cutting operation may be assisted by the provision of grooves filled with the coating material in the deposition surface of the collector corresponding to paths traversed by a cutter, thereby avoiding damage to the collector surface by the cutter. Where the collector is a drum collector the grooves preferably extend axlally between the drum ends so that the deposited alloy may be cut into arcuate plates~
The coating material is preferably a solder of the eutectic type, that is, having a melting/solidification temperature as opposed to a melting/solidification temperature range. The solder is preferably applied to the surface of the collector by a spraying process such as, for example, flame or plasma-arc spraying. Where the collector is manufactured from an aluminium based material it ma~ be necessary for the collector surface to have an initial deposit of copper to allow 'wetting' by the subsequent solder coating~
An embodiment of the present invention will now be described by way of example only iwth reference to the following figures of which:
Figure 1 shows a schematic sectional elevation of a drum collector positioned within the deposition apparatus, and Figure 2 shows a transverse section of the drum of Figure 1 together with an enlarged view of the cutting grooves in the drum.
Referring to Figure 1 a collector drum 10, manufactured from an aluminium alloy~ is mounted on stub shafts 11 and includes gas-gap cooling assemblies 12 for connection to a temperature control unit 13 by means of pipes 1~.
As shown by Figures 1 and 2 the drum 10 has six equi~spaced cutting grooves 15 therein which extend axially between the drum ends to facilitate the cutting of deposited alloy on the drum.

l~
r~le surface of the drum 10 is prepared for use by alumina blasting its outer surface and thereafter providing that surface with a thin copper plating 16. Such surface treatment is necessary for the effective bonding of a coating of solder 17 which is sprayed onto the surface of the drum 10~ The coating of solder 17 has a melting temperature of approximately 300C
and a composition of 1.5% silver, 5% tin and 93.5% lead.
Before the coating of solder 17 is applied to the surface of the drum the cutting grooves 15 are plugged with solder strips 0 10 to provide continuity at the drum surface.
Once the drum 10 is prepared for use it is mounted within a vacuum chamber 19 above an evaporator 20. The drum 10 is coupled to a drive unit 21 and the cooling assemblies 12 linked by pipes 14 to the temperature control unit 13n As part of the evaporation process the chamber 19 is evacuated and the drive unit 21 activated to rotate the drum 10 at the required rate. By means of a radiant heater 22 the drum 10 is pre-heated to an operating temperature of 250C.
~he drum 10 is filled with helium gas for cooling purposes and the evaporator 20 charged with the molten alloy 23 required for evaporation.
An electron beam from an electron beam gun 24 is directed onto the surface of the molten alloy 2~ to Benerate alloy vapour which rises from the evaporator 20 and is deposited 25 onto the coating of solder 17. The rate of alloy evaporation is such`that a layer of alloy approximately 10~m thick is deposited on the drum 10 for each rotation thereof. As the drum 10 rotates the surface of the deposit is mechanically worked by a peening device 25 which improves the micro-structure of the deposited alloy. The evaporation process is continued until the deposit is approximately 50 mm thick.
Heat generated by the evaporation process is removed from the drum 10 by the cooling assemblies 12. The rate of heat transfer and hence the drum temperature is controlled by ,.

'7~

varying the pressl~e of the helium gas within the drum 10.
Since the mass of the drum 10 is high the temperature at the deposition surface can be maintained at a substantially constant temperature of 250C and alloy vapour deposited thereon is rapidly cooled.
When the evaporation process is complete the electron beam gun 24 is switched off and the upper section of the vacuum chamber 19 removed. A rotary cutter 26, (not shown), arranged to traverse the length of -the drum is positioned above the drum 10 and the drum rotated until one of the cutting grooves 15 is coincident with the line of travel of the cutter 26.
The cutter 26 is then lowered so that its depth of cut is almost to the base of the cutting groove 15. The cutter 26 is set in motion and the deposited alloy is eventually cut into six discreet and equally sized arcuate plates by repetition of the cutting procedure along the rPm~ining five cutting grooves 15.
The arcuate plates are removable from the collector drum 10 by heating of the deposited alloy with the radiant heater 22 to a temperature slightly in excess of 300C whereupon the solder 17 bonding coat becomes molten thereby releasing the deposited alloy from the collector drum 10 for further processing~
Once all the deposited alloy has been removed the drum 10 may be cooled and prepare for re-use by removing and replacing the damàged solder strips and re-spraying with a further coating of solder.
In a modification of the invention the outer skin of the collector drum is fabricated from a thin sheet of aluminium based material and the inner surface of the fabricated skin is coated with copper, by for example, electroplating. The copper plating facilitates wetting of the skin inner surface by a subsequently applied solder coating, applied by a spraying ~34~7~L

process or, becaue of the much lower thermal capacity of the thin skin, by conventional dipping in a solder bath.
Immediately below the thin cylindrical skin of the collector the main drum periphery structure comprises a plurality of axial bars formed, for example, from machined aluminium alloy extrusions. Each axial bar is machined such as to allow a close sliding fit between itself and each of its immediate nei~hbours. E~ch axial bar is mounted on a plurality of spokes extending radially and along the length of a central hub and shaf~ arrangement. Each axial bar i9 adjustably and resiliently mounted on its o~n set of spokes by, for example, a screw thread and coil or disc spring arrangement such that each bar is allowed a limited degree of radial mo~ement in either direction from its normal position. Moreover, each axial bar is so machined such that multiple radial flexure in either direction is permitted simultaneously within a single axial bar.
Each axial bar may be provided with holes in which rod heaters may be inserted, although of course the radiant heater above the drum assembly ~ay be used for initial heating of the collector at process startup. Additionally each axial bar is provided with attachment points to which cooling pipes, for example, may be clamped.
Each axial bar, if made of aluminium or some other material not easily wetted by solder is copper plated and that area of each bar~which will form a portion of the outer surface of the assemblad bars is coated with solder, preferably by spraying.
When all the axial bars are assembled on the spoke array the outer surface defined by the assembly is a cylinder.
The thin pre-coated collector skin is now positioned o~er the a~ial bar drum assembly and the screw thread and spring me~ns adjusted such that each axial bar bears with substantially equal pressure resiliently against the outer skin. lhe outer skin is heated by the radiant heater within the process ~9~'7~

apparatus whilst the drum is rotating eventually reaching a temperature where the solder coatings are caused to fuse.
Alternatively the drum can be heated from the interior by the rod heaters and achieve the same result.
The resulting drum has a conformable surface which is thus able to accommodate minor movements of the deposited alloy due to thermal and mechanical stresses without rupture of the so]der interface layer.
It will be realised that the deposited alloy need not be detached from the drum in-situ and that the drum may be removed from the vacuum chamber so that an already prepared drum can be installed, thus reducing the down-time of the process to a m; n; ml~m q Although the invention of using a solder interface has been described with respect to a drum collector it is equally applicable to a slab type collector.

Claims (19)

1 A reuseable collector for use in a process for the production of an alloy by deposition from the vapour phase and comprising a main collector structure with a deposition surface, an alloy coating on said deposition surface, said alloy coating having a melting temperature or temperature at which the onset of fusion occurs above -the peak operating temperature at said deposition surface during said deposition process, and whereby, said alloy coating between said collector deposition surface and deposited alloy from the vapour phase may be melted rendering said deposited alloy detachable from said collector.
2 A reuseable collector for use in a process for the production of an alloy by deposition from the vapour phase, the collector comprising a thin outer cylindrical skin the outer surface of which constitutes a deposition surface a main drum structure comprising a plurality of axial bars arranged to accommodate thermal and/or mechanical stresses (by flexural movement), resilient support means axially and adjustably carrying said axial bars an alloy between said main drum structure and said outer cylindrical skin said alloy having a melting temperature or temperature at which the onset of fusion occurs above the peak operating tem-perature at said deposition surface, and whereby, said alloy may be melted upon completion of deposition from the vapour phase rendering said deposited alloy and said outer cylindrical outer skin detachable from said main drum structure.
5. A reuseable collector as claimed in claim 1 and wherein said alloy coating on said collector deposition surface is a solder alloy.
4. A reuseable collector as claimed in claim 2 and wherein said alloy between said main drum structure and said outer cylindrical skin is a solder alloy.
5. A reuseable collector as claimed in claim 3 or claim 4 and wherein said solder alloy is of a eutectic type.
6. A reuseable collector as claimed in claim 3 or 4 and wherein said solder alloy is of a eutectic type and has substantially the com-position expressed below in weight per cent;
Silver 1.5 Tin 5.0 Lead Remainder
7. A reuseable collector as claimed in claim 3 and wherein a first coating of a metal to facilitate wetting by a subsequently applied coating of said solder alloy is on said deposition surface.
8. A reuseable collector as claimed in claim 7 and wherein said first coating metal is copper.
9. A reuseable collector as claimed in claim 3 and wherein said solder alloy coating is applied by a spraying process.
10. A reuseable collector as claimed in claim 2 and wherein said plurality of axial bars comprising said main drum structure are each formed from aluminium alloy extrusions.
11. A reuseable collector as claimed in claim 10 and wherein at least the area of each of said axial bars comprising said main drum structure to be subsequently coated with said solder alloy is first copper plated.
12. A reuseable collector as claimed in claim 2 and wherein a first coating of copper is on the inner surface of said outer cylindrical skin.
13. A reuseable collector as claimed in claim 2, 4 or 10 and wherein a solder alloy coating is on either or both of said inner surface of said outer cylindrical and the outer surface of said main drum structure prior to assembly of said outer cylindrical skin onto said main drum structure.
14. A reuseable collector as claimed in claim 1 and wherein said deposition surface is cylindrical.
15. A reuseable collector as claimed in claim 14 and wherein said deposition surface has at least one axial groove.
16. A reuseable collector as claimed in claim 15 and wherein said at least one groove in said deposition surface is filled with solder alloy.
17. A reuseable collector as claimed in claim 1 or claim 2 and having heaters and coolers.
18. A process for the bulk production of an alloy by deposition from the vapour phase and comprising the steps of coating the deposition surface of a temperature controllable collector with a solder alloy depositing alloy from the vapour phase onto said solder alloy coating in a low pressure environment and on completion of deposition from the vapour phase melting said solder alloy coating and removing said deposited alloy from said collector.
19 A process for the bulk production of an alloy by deposition from the vapour phase and comprising the steps of placing a solder alloy coating between an outer cylindrical skin and a main drum structure depositing alloy from the vapour phase onto the outer surface of said outer cylindrical skin in a low pressure environment on completion of deposition from the vapour phase melting said solder alloy coating and removing said deposited alloy and said outer cylindrical skin.
CA000392301A 1980-12-16 1981-12-15 Bulk production of alloys by deposition from the vapour phase and apparatus therefor Expired CA1194701A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB8040242 1980-12-16
GB8040242 1980-12-16

Publications (1)

Publication Number Publication Date
CA1194701A true CA1194701A (en) 1985-10-08

Family

ID=10518013

Family Applications (1)

Application Number Title Priority Date Filing Date
CA000392301A Expired CA1194701A (en) 1980-12-16 1981-12-15 Bulk production of alloys by deposition from the vapour phase and apparatus therefor

Country Status (5)

Country Link
US (1) US4517027A (en)
EP (1) EP0055542A1 (en)
JP (1) JPS57123940A (en)
CA (1) CA1194701A (en)
GB (1) GB2116214B (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB8328858D0 (en) * 1983-10-28 1983-11-30 Atomic Energy Authority Uk Metal vapour deposition
US4654275A (en) * 1985-11-27 1987-03-31 Allied Corporation Storage life of Pb-In-Ag solder foil by Sn addition
GB2248852A (en) * 1990-10-16 1992-04-22 Secr Defence Vapour deposition
US5310512A (en) * 1990-11-15 1994-05-10 Norton Company Method for producing synthetic diamond structures
US20060038302A1 (en) * 2004-08-19 2006-02-23 Kejun Zeng Thermal fatigue resistant tin-lead-silver solder

Family Cites Families (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2306667A (en) * 1942-02-13 1942-12-29 American Smelting Refining Alloy
DE1143077B (en) * 1954-04-12 1963-01-31 Union Carbide Corp Device for the continuous production of metal foils by depositing metal layers from vaporous metal compounds
US2915384A (en) * 1956-10-02 1959-12-01 Nat Res Corp Method of producing zirconium
DE1176615B (en) * 1962-05-16 1964-08-27 Leybold Hochvakuum Anlagen Process and device for the production of the finest dispersions
US3380821A (en) * 1965-10-21 1968-04-30 Gen Motors Corp Heat treatable creep resistant solder alloy
GB1206586A (en) * 1966-09-07 1970-09-23 Mini Of Technology Vacuum deposition process of forming alloys
US3615275A (en) * 1967-12-12 1971-10-26 Texas Instruments Inc Homogeneously fine-grained vapor-deposited material in bulk form
US3717914A (en) * 1971-06-24 1973-02-27 Union Carbide Corp Reusable mandrel for structures having zero draft or re-entrant geometries
US3895671A (en) * 1972-11-15 1975-07-22 Nippon Musical Instruments Mfg Method of manufacturing a thin sheet of beryllium or an alloy thereof
SU618452A1 (en) * 1974-11-10 1978-06-23 Государственный научно-исследовательский и проектный институт сплавов и обработки цветных металлов "Гипроцветметобработка" Foil manufacturing method
US4016310A (en) * 1975-04-23 1977-04-05 Xerox Corporation Coater hardware and method for obtaining uniform photoconductive layers on a xerographic photoreceptor
US4231982A (en) * 1975-05-20 1980-11-04 Ab Volvo Method for the production of tools for deep drawing, moulding, extruding and the like
JPS53780A (en) * 1976-02-23 1978-01-06 Fiat Allis Construct Machine Support pad for momentary bonding container using pallets
US4321087A (en) * 1978-12-21 1982-03-23 Revlon, Inc. Process for making metallic leafing pigments

Also Published As

Publication number Publication date
GB2116214B (en) 1985-09-25
JPS57123940A (en) 1982-08-02
JPH0133539B2 (en) 1989-07-13
US4517027A (en) 1985-05-14
EP0055542A1 (en) 1982-07-07
GB2116214A (en) 1983-09-21

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