US3042550A - Solid delay line improvements - Google Patents

Solid delay line improvements Download PDF

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US3042550A
US3042550A US73738958A US3042550A US 3042550 A US3042550 A US 3042550A US 73738958 A US73738958 A US 73738958A US 3042550 A US3042550 A US 3042550A
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transducer
delay
ceramic
layer
line
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Richard E Allen
George M Deegan
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Corning Inc
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Corning Inc
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G2/00Details of capacitors not covered by a single one of groups H01G4/00-H01G11/00
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    • C04B37/02Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
    • C04B37/023Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used
    • C04B37/026Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles characterised by the interlayer used consisting of metals or metal salts
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    • 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
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    • C23C14/02Pretreatment of the material to be coated
    • C23C14/027Graded interfaces
    • HELECTRICITY
    • H03BASIC ELECTRONIC CIRCUITRY
    • H03HIMPEDANCE NETWORKS, e.g. RESONANT CIRCUITS; RESONATORS
    • H03H9/00Networks comprising electromechanical or electro-acoustic devices; Electromechanical resonators
    • H03H9/02Details
    • H03H9/125Driving means, e.g. electrodes, coils
    • HELECTRICITY
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    • H03HIMPEDANCE NETWORKS, e.g. RESONANT CIRCUITS; RESONATORS
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    • H03H9/13Driving means, e.g. electrodes, coils for networks consisting of piezo-electric or electrostrictive materials
    • H03H9/133Driving means, e.g. electrodes, coils for networks consisting of piezo-electric or electrostrictive materials for electromechanical delay lines or filters
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Description

United States Patent 3,042,550 SOLID DELAY LINE IMPROVEMENTS Richard E. Allen and George M. Deegan, Corning, N.Y., assignors to Corning Glass Works, Corning, N.Y., a corporation of New York Filed May 23, 1953, Ser. No. 737,389 6 Claims. (Cl. 117--217) The present invention relates to solid delay line improvements and particularly to the production of ferroelectric ceramic transducers that may be readily bonded in known manner for operation in the shear mode to a non-crystalline solid delay line medium and to a back electrode, such for example as a delay line composed of glass or fused silica, and a back electrode composed of a tin-lead alloy.

The industry has for some time employed ferroelectric ceramic transducers mounted for longitudinal mode of vibration on delay lines designed for short delay time periods. On longer lines such transducers have been similarly mounted, and in the absence of knowledge as to how to directly mount the ceramic transducers for shear mode vibration, have resorted to the use of mode conversion prisms. In general, for longer lines with many reflection paths only the thickness shear mode of vibration of quartz has been found satisfactory. Some of the advantages gained by use of ferroelectric ceramic transducers operating in the thickness shear mode, however, are low attenuation of the main signal, high attenuation of the unwanted third time spurious signal, and utilization of low cost optical glass for short delay lines instead of the'high cost silica required when quartz transducers are employed. Moreover, ceramic transducer assemblies are thermally stable and more readily reproducible than are quartz transducers. They also have the further advantage of low insertion loss compared to quartz.

The fact that ceramic transducers must not be subjected to temperatures exceeding 200 C. for any appreciable time after their polarization, has heretofore prevented their employment in the shear mode for lack of a low temperature method of applying a solderable coating thereto. Although such a temperature is exceeded by application thereto of a solderable film by conventional methods, this has been no handicap in the production of transducers polarized for the longitudinal mode. Under these circumstances the surface to be united with the delay line and the oppositely disposed surface for connection to a back electrode are simply coated before polarization of the transducer which is thereafter polarized by connecting the respective films to the terminal of a suitable high potential direct current source for' a short time. The transducer can then be bonded to the delay line by a known method. One such method is taught by the French Patent No. 1,140,481 (US. application Serial No. 475,062, filed December 14, 1954), and now Patent No. 2,964,839 but by restricting temperatures to values insufficient to have a deleterious efiect on the polarization of the transducer.

According to the invention a polarized ferroelectric ceramic transducer having a shear mode of vibration is obtained by slicing it from a block of ceramic material previously polarized in a direction parallel to its poling axis. This then presents the remaining problem of soldering the ceramic to the delay line facet with indium and soldering the back electrode to the back of the ceramic with tin-indium solder at temperatures which will not impair its polarity. According to the invention the problem is solved by the low temperature application to both broad surfaces of a ceramic transducer a thin, welladhered, solderable, four-layer coating, comprising a base layer of platinum or of silver, which preferably is baked in at a temperature of approximately 200 C., a second 2 layer of chromium, a layer of an alloy which is approximately 80% Ni and about 20% Cr laid down in a manner that produces a gradient coating in which the Cr content is the highest at the start and lowest at the end of the coating period respectively, and finally depositing a layer of Au thereon.

For a more detailed description of the invention reference is made to the accompanying drawing wherein:

FIG. 1 is a perspective representation of a polarized block of ferroelectric ceramic material.

FIG. 2 is an exploded view, in side elevation, diagrammatically depicting the ceramic transducer and its respective coatings arranged between a back electrode and the coating of a facet of a delay line; the bonding materials for effecting union of the transducer with the back electrode and with the facet coating also being shown.

Referring to the drawing in detail, the block of material 11 has conductive coatings 12 and 13 on its upper and lower surfaces respectively which have previously been connected to the terminals of a high volt-age direct current source to impart to it a poling axis transversely therethrough, as indicated by the arrows A, so that when a slice such as 15 is removed therefrom for use as a transducer and one of its broad sides mated with a delay line surface, it will be in shear mode relation thereto.

Specifically, the first or base layer of about 300 angstroms of platinum or silver is deposited on both sides of the slice 15 of the ceramic by vacuum evaporation at room temperature. This coating is preferably baked in an open atmosphere at a temperature of approximately 200 C. for from one to eighteen hours to provide good. adherence.

The second layer of about 500 angstroms of chromium is then deposited by vacuum evaporation at room temperature. The purpose of this metal, which is insoluble in solder, is to serve as a barrier between the solder and the platinum, which is soluble.

The third layer of about 500 angstroms of a nickelchrome alloy containing approximately Ni and 20% Cr is also applied at room temperature by the evaporation process in the vacuum maintained during application of the second layer.

The fourth or final layer of about 500 angstroms of gold is applied in the vacuum maintained during application of the third layer to preserve the nickel-chromes metallic surface.

In effecting unions with the delay line medium and with the back electrode respectively, the final layers of gold are almost instantly dissolvable by the solders employed. During such a soldering operation the solder penetrates the multi-layer coatings until it is stopped either at the high Cr part of the nickel-chrome layer or at the nickel-chrome Cr interface.

As indicated in FIG. 2, the delay line bears a layer of platinum on its transducer mating facet 20. Fusion of its surface to the gold surface of 15 is effected by directing heat into the mating surfaces until they reach a temperature of 200 C. or thereabout and puddling pure indium thereon. Such surfaces are then swabbed with a vibrating fibre glass brush, tinned with pure indium from an auxiliary molten puddle thereof and the indium slowly spread over the respective mating surfaces substantially as described in the French patent. The respective surfaces are then permitted to cool down to a stabilized temperature of between 165 175 C. and after a final skin removal from such surfaces they are brought together into aligned contact and subjected to gradually increased pressure until cooled to approximately C.

At this point, the mating surface of the transducer and the back electrode are swabbed with a fibre glass brush tinned with 65% In35% Sn solder, mated, and then 3 allowed to cool. The back electrode preferably is a preformed block of 60% tin-% lead, as in the referred-to patent and application.

Surplus solder is removed from the finished assembly with a sharp knife or razor blade. Any of the evaporated coating material on the external surfaces is readily removed by dental sand blasting equipment.

Although union between applicants ferroelectric transducer with a delay line and a tin-lead back electrode is substantially in accordance with the teaching of the referred-to French patent, as briefly described above, quite obviously similar unions may be'effected by use of any solder having a high indium content. The ferroelectric ceramic material employed by applicants is approximately PbT-iO PbZrO but it is believed applicants techniques are equally applicable to other ferroelectric ceramic compositions.

What is claimed is: v

1. The method of preparing surfaces of a transducer for solder-able union with a solid delay line and its back electrode which comprises application to each of its two broad surfaces a base coat of a noble metal by vacuum deposition, depositing a layer of chromium on said base coat, overlaying the chromium with a gradient coating containing approximately Ni and 20% Cr with the content of Cr being highest at the chromium interface and lowest at the exposed surface, and finally overlaying the...

gradient coating with a layer of gold.

2. The method of coating a transducer with a material solderable at a temperature of approximately 200 C., which comprises applying by vapor deposition in a vacuum successively and at temperatures under 200 C., films of the followin gmctallic materials: a ndble metal, chroa nickel-chromium alloy containing approximately 80% Ni and 20% Cr laid down in graded composition in which the Cr content is highest at the start and lowest at the completion of evaporation and gold.

3. A method such as defined by the preceding claim which includes baking the noble metal coating at a temperature of approximately 200 C. for a substantial time period. I

4. In a ferroelectric ceramic transducer ,having on a surface thereof parallel to its poling axis a coating through the medium of which it is solder-able to an indiumized mating facet of a delay line and a back electrode at a temperature below that at which the polarization of such transducer would be adversely affected said coating comprising layers of a noble metal, chromium, nickelch'rome and gold arranged thereon in the order named.

5. A ferroelectric ceramic transducer such as defined by claim 4 wherein the noble metal comprises silver.

6. A ferroelectric ceramic transducer such as defined by claim 4 wherein the noble metal comprises platinum.

References Cited in the file of this patent UNITED STATES PATENTS 2,672,590 McSkimin Mar. 16, 1954 2,702,427 Roberts Feb. 22, 1955 2,731,573 Hansen et al Ian. 17, 1956 2,767,336 Arenberg Oct. 16, 1956 2,777,997 Arenberg et a1 Ian. 15, 1957 2,787,520 Meincrs et al Apr. 2, 1957 2,859,415 Fagen Nov. 4, 1958 OTHER REFERENCES Belser: Review of Scientific Instruments," vol. 25, No. 2, February 1954, pages 180-183.

Claims (1)

1. THE METHOD OF PREPARING SURFACES OF A TRANSDUCER FOR SOLDERABLE UNION WITH A SOLID DELAY LINE AND ITS BACK ELECTRODE WHICH COMPRISES APPLICATION TO EACH OF ITS TWO BROAD SURFACES A BASE COAT OF A NOBLE METAL BY VACUUM DEPOSITION, DEPOSITING A LAYER OF CHREMIUM ON SAID BASE COAT, OVERLAYING THE CHROMIUM WITH A GRADIENT COATING CONTAINING APPROXIMATELY 80% NI AND 20% CR WITH THE CONTENT OF CR HIGHEST AT THE CHROMIUM INTERFACE AND LOWEST OF THE EXPOSED SURFACE, AND FINALLY OVERLAYING THE GRADIENT COATING WITH A LAYER OF GOLD.
US3042550A 1958-05-23 1958-05-23 Solid delay line improvements Expired - Lifetime US3042550A (en)

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US3042550A US3042550A (en) 1958-05-23 1958-05-23 Solid delay line improvements
US3111741A US3111741A (en) 1958-05-23 1960-10-27 Solid delay line improvements
US3206698A US3206698A (en) 1958-05-23 1961-01-11 Electro-mechanical delay line having ferroelectric transducer bonded to solid delay medium

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US3042550A US3042550A (en) 1958-05-23 1958-05-23 Solid delay line improvements
GB1719959A GB890813A (en) 1958-05-23 1959-05-20 Ultrasonic delay line improvements
NL239431A NL124189C (en) 1958-05-23 1959-05-22
DE19591416028 DE1416028B2 (en) 1958-05-23 1959-05-22
BE578941A BE578941A (en) 1958-05-23 1959-05-22 Improvements in solid delay lines.
FR795267A FR1224785A (en) 1958-05-23 1959-05-22 Improvements in solid delay lines
US3111741A US3111741A (en) 1958-05-23 1960-10-27 Solid delay line improvements
US3206698A US3206698A (en) 1958-05-23 1961-01-11 Electro-mechanical delay line having ferroelectric transducer bonded to solid delay medium

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US3131459A (en) * 1959-11-09 1964-05-05 Corning Glass Works Method of bonding absorbing material to a delay line
US3173201A (en) * 1961-08-23 1965-03-16 James F Motson Method of sealing a glass element within a metal member
US3178271A (en) * 1960-02-26 1965-04-13 Philco Corp High temperature ohmic joint for silicon semiconductor devices and method of forming same
US3206698A (en) * 1958-05-23 1965-09-14 Corning Glass Works Electro-mechanical delay line having ferroelectric transducer bonded to solid delay medium
US3247473A (en) * 1959-11-09 1966-04-19 Corning Glass Works Cold diffusion bond between acoustic delay line and back electrode or acoustic absorber
US3252722A (en) * 1959-11-09 1966-05-24 Corning Glass Works Delay line bond
US3276097A (en) * 1963-12-19 1966-10-04 Bell Telephone Labor Inc Semiconductor device and method of making
US3590467A (en) * 1968-11-15 1971-07-06 Corning Glass Works Method for bonding a crystal to a solid delay medium
US3599123A (en) * 1969-09-24 1971-08-10 Bell Telephone Labor Inc High temperature ultrasonic device
US3857161A (en) * 1973-02-09 1974-12-31 T Hutchins Method of making a ductile hermetic indium seal
US3999263A (en) * 1974-11-14 1976-12-28 Litton Systems, Inc. Method of forming a micro-array multibeam grid assembly for a cathode ray tube
US4726507A (en) * 1984-08-29 1988-02-23 The United States Of America As Represented By The Secretary Of The Air Force Cryogenic glass-to-metal seal
DE3638342A1 (en) * 1986-11-10 1988-05-19 Siemens Ag Electrical component, made of ceramic and having multilayer metallisation, and a method for its production
US4837928A (en) * 1986-10-17 1989-06-13 Cominco Ltd. Method of producing a jumper chip for semiconductor devices
US6188162B1 (en) * 1999-08-27 2001-02-13 Product Systems Incorporated High power megasonic transducer
US6222305B1 (en) 1999-08-27 2001-04-24 Product Systems Incorporated Chemically inert megasonic transducer system
US20020190608A1 (en) * 2001-04-23 2002-12-19 Product Systems Incorporated Indium or tin bonded megasonic transducer systems

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US3367755A (en) * 1965-02-26 1968-02-06 Gen Dynamics Corp Laminar conductive material having coats of gold and indium
US3846649A (en) * 1973-06-18 1974-11-05 Rca Corp Piezoelectric transducer comprising oriented zinc oxide film and method of manufacture
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US4033503A (en) * 1976-08-27 1977-07-05 Nasa Method for attaching a fused-quartz mirror to a conductive metal substrate
US4077558A (en) * 1976-12-06 1978-03-07 International Business Machines Corporation Diffusion bonding of crystals
WO1983003266A1 (en) * 1982-03-15 1983-09-29 Gsp Metals Chemicals Corp Chelating metals
US4582240A (en) * 1984-02-08 1986-04-15 Gould Inc. Method for low temperature, low pressure metallic diffusion bonding of piezoelectric components
US5076486A (en) * 1989-02-28 1991-12-31 Rockwell International Corporation Barrier disk
US5476726A (en) * 1992-01-22 1995-12-19 Hitachi, Ltd. Circuit board with metal layer for solder bonding and electronic circuit device employing the same
WO1998024296A3 (en) * 1996-11-20 1998-10-01 Univ California Multilaminate piezoelectric high voltage stack

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US2672590A (en) * 1950-03-22 1954-03-16 Bell Telephone Labor Inc Delay line
US2767336A (en) * 1951-05-22 1956-10-16 David L Arenberg Cement for bonding elements of a delay line with low transmission losses using mixtures of inorganic salts
US2777997A (en) * 1951-11-06 1957-01-15 David L Arenberg Ultrasonic delay lines
US2787520A (en) * 1952-03-07 1957-04-02 California Research Corp Process for producing piezoelectric transducers
US2859415A (en) * 1952-09-03 1958-11-04 Bell Telephone Labor Inc Ultrasonic acoustic wave transmission delay lines
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Publication number Priority date Publication date Assignee Title
US3206698A (en) * 1958-05-23 1965-09-14 Corning Glass Works Electro-mechanical delay line having ferroelectric transducer bonded to solid delay medium
US3131459A (en) * 1959-11-09 1964-05-05 Corning Glass Works Method of bonding absorbing material to a delay line
US3247473A (en) * 1959-11-09 1966-04-19 Corning Glass Works Cold diffusion bond between acoustic delay line and back electrode or acoustic absorber
US3252722A (en) * 1959-11-09 1966-05-24 Corning Glass Works Delay line bond
US3178271A (en) * 1960-02-26 1965-04-13 Philco Corp High temperature ohmic joint for silicon semiconductor devices and method of forming same
US3173201A (en) * 1961-08-23 1965-03-16 James F Motson Method of sealing a glass element within a metal member
US3276097A (en) * 1963-12-19 1966-10-04 Bell Telephone Labor Inc Semiconductor device and method of making
US3590467A (en) * 1968-11-15 1971-07-06 Corning Glass Works Method for bonding a crystal to a solid delay medium
US3599123A (en) * 1969-09-24 1971-08-10 Bell Telephone Labor Inc High temperature ultrasonic device
US3857161A (en) * 1973-02-09 1974-12-31 T Hutchins Method of making a ductile hermetic indium seal
US3999263A (en) * 1974-11-14 1976-12-28 Litton Systems, Inc. Method of forming a micro-array multibeam grid assembly for a cathode ray tube
US4726507A (en) * 1984-08-29 1988-02-23 The United States Of America As Represented By The Secretary Of The Air Force Cryogenic glass-to-metal seal
US4837928A (en) * 1986-10-17 1989-06-13 Cominco Ltd. Method of producing a jumper chip for semiconductor devices
DE3638342A1 (en) * 1986-11-10 1988-05-19 Siemens Ag Electrical component, made of ceramic and having multilayer metallisation, and a method for its production
US6188162B1 (en) * 1999-08-27 2001-02-13 Product Systems Incorporated High power megasonic transducer
US6222305B1 (en) 1999-08-27 2001-04-24 Product Systems Incorporated Chemically inert megasonic transducer system
US6722379B2 (en) 1999-08-27 2004-04-20 Product Systems Incorporated One-piece cleaning tank with indium bonded megasonic transducer
US20020190608A1 (en) * 2001-04-23 2002-12-19 Product Systems Incorporated Indium or tin bonded megasonic transducer systems
US6904921B2 (en) 2001-04-23 2005-06-14 Product Systems Incorporated Indium or tin bonded megasonic transducer systems

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FR1224785A (en) 1960-06-27 grant
NL124189C (en) 1968-05-15 grant
DE1416028B2 (en) 1970-08-13 application
US3111741A (en) 1963-11-26 grant
GB890813A (en) 1962-03-07 application
BE578941A (en) 1959-11-23 grant
BE578941A1 (en) grant
DE1416028A1 (en) 1970-01-22 application
US3206698A (en) 1965-09-14 grant

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