US3600575A - Crystal mount and goniometer for taking laue patterns and for orientation of large single crystals - Google Patents

Crystal mount and goniometer for taking laue patterns and for orientation of large single crystals Download PDF

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US3600575A
US3600575A US821595A US3600575DA US3600575A US 3600575 A US3600575 A US 3600575A US 821595 A US821595 A US 821595A US 3600575D A US3600575D A US 3600575DA US 3600575 A US3600575 A US 3600575A
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crystal
goniometer
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specimen
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/205Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials using diffraction cameras

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  • Parker ABSTRACT A combined, portable crystal mount and goniometer apparatus having built-in vertical and horizontal goniometer members, and an adjustably mounted crystal holder member adapted to be rigidly positioned on the camera track of a standard type of X-ray diffraction apparatus and thereby extend the latters inherent ability in taking Laue patterns of small types of crystalline structures to the further capability of taking X-ray diffraction pictures of the relatively large or macro-type crystal.
  • the present invention relates generally to the taking of X- ray diffraction pictures of crystal structures and in particular, to an improved combined crystal holder and goniometer device for assisting in the production of Laue patterns of the macro-type of crystals.
  • the present invention consists of a combined crystal mount and goniometer mechanism which includes basically a vertical goniometer element, a main frame member supported in posi tion by the vertical goniometer, an adjustable crystal holder element mounted to the main frame member, and a horizontal goniometer element having base support means for supporting the vertical goniometer.
  • the vertical goniometer further includes a dial portion having a main scale inscribed thereon and a vernier scale portion which is the element that specifically supports the main frame member. This vernier scale portion is rotatably supported relative to the dial portion and is adjustable to various positions of adjustment to thereby simultaneously adjust the main frame member and the crystal holder element supported thereby to various positions of orientation about a horizontal axis.
  • the horizontal goniometer also includes a main dial portion which is shaped to interfit with the camera track of the X-ray diffraction apparatus with which it is combined, and a vernier scale portion.
  • the latter constitutes one element of the base support means, and it is movable in rotation relative to the last-named, main dial portion. Since the base support means is rigidly interconnected with the vertical goniometer, any movement of the said horizontal goniometer-vernier scale portion also moves or adjusts the main frame member and crystal holder element about a vertical axis, the collective adjustment of the crystal holder element about both vertical and horizontal axes thereby providing for the determination of the crystal orientation.
  • FIG. 1 is a top assembly view of the crystal mount and goniometer arrangement of the present invention shown positioned on the camera track of an existing mechanism;
  • FIG. 2 is a front view of the assembly of FIG. 1, illustrating further details of the crystal mount and goniometer arrangement of the present invention
  • FIG. 3 is a right side view of the invention of FIGS. 1 and 2,
  • FIG. 4 is another front view, illustrating further details of the novel crystal alignment device shown in FIG. 3;
  • FIGS. 5 and 6 represent top views of the lower and upper base plate members, respectively, that are utilized as an integral part of the inventive crystal mount;
  • FIG. 7 represents a front view of one type of spacer element which may be placed between the film cassette support means of an X-ray diffraction camera apparatus and the crystal mount of the present invention for thereby determining the correct distance between the plane of the crystal specimen under investigation and the film being exposed to the X-rays 'thereof;
  • FIG. 8 illustrates a quartz crystal specimen shown mounted on a plate-form of crystal holder which, in turn, may be positioned on an extensiblearm element of the main crystal mount of the present invention
  • FIG. 9 represents another form of crystal holder which is utilizable with the present crystal mount, and which further shows a representative example of one type of clamp device utilizable for holding irregular-shaped, macrocrystals on the inventive crystal mount;
  • FIGS. 10, 11 and 12 respectively represent plan views of various forms of screen elements adapted to be used with the crystal holder of the present invention for uniquely providing for multiple exposure of the film in examining the crystal structure of the specimen under investigation.
  • the improved crystal mount assembly of the present invention is indicated generally at 30 as being mounted in position on a relatively enlarged, supporting member at 6 representing the camera track of an X-ray diffraction camera apparatus.
  • the film cassette of this camera is shown at I.
  • Said X-ray diffraction camera apparatus may include an X-ray generator (not shown) which provides the source of X-rays to be used in the investigation of one or more types of crystal specimens in the new and improved manner to be described in more detail hereinafter.
  • X-rays produced by such an X-ray generator are indicated in the present description by means of an arrow marked A" in FIG. 1.
  • the relatively elongated and shielded X-ray transmitting member at In may be utilized.
  • An X-ray shielding shutter element may be provided in one portion of said X-ray transmitting member, as is indicated at the reference numeral 1c, which shielding shutter element 10 may be utilized to open or close the end of an X-ray transmitting passage (not shown) in the member la and thereby control the transmission of X- rays from the X-ray source.
  • Said relatively elongated member 1a is shown supported within a relatively enlarged base support 1b which is, in turn, supported to one side of the film cassette 1.
  • a screw adjustment device is utilized at 1d to releasably retain the member 1a interconnected with the support 1b.
  • support 1b and said film cassette 1 may likewise be shielded and incorporate communicating and centrally located X-ray transmitting passages to thereby provide for the transmission of, and therefore the exposure to X-rays of any crystal specimen, such as that depicted at 4. Such rays are thereafter difiracted to the film negative in the film cassette 1 to form thereon the previously mentioned Laue patterns.
  • the aforementioned crystal specimen 4 which may consist of a relatively enlarged crystal sample of substantially rectangular or other regular shape, is shown as being mounted in close proximity to the film in the said film cassette 1 by means of a metallic specimen-plate holder element 5.
  • the latter which is also made into a rectangular configuration, is in turn mounted on a second, metallic plate of similar configuration.
  • This second plate consists of the head portion 16a of a relatively elongated arm member 16 which, together therewith, constitutes one form of a crystal holding means utilized with, and forming an integral part of, the overall crystal mount assembly 30 of the present invention.
  • Said arm member 16 is releasably or extensibly held within, and thus is supported by an enlarged, hollow, and relatively long and preferably tubular-shaped arm-support member 18.
  • The'latter member 18 is, in turn, releasably retained in close-fitting relation within a relatively enlarged opening 17a (Note FIG. 2) provided adjacent one end portion of the main, rectangular-shaped, frame member 17 of the present crystal mount assembly 30.
  • the said arm-support member 18 is made hollow in form, as indicated hereinbefore, and is designed with an inside diameter surface portion so dimensioned as to snugly fit the outside diameter surface of said arm member 16, as is indicated in the aforementioned FIGS. 1 and 2.
  • the said main frame member 17 is provided adjacent to the end thereof containing the aforesaid opening 170 with a narrow cutout, or groove at 17b which groove 17b provides an opening in the top surface of the frame member 17 and further extends downwardly therefrom to communicate with the aforesaid enlarged opening 17a.
  • the said arm-support member 18 may be releasably retained at a selected position within the opening 17a and, in this manner, ease of assembly and/or repair of the inventive arrangement may be facilitated.
  • an adjustment screw member at 19 may be utilized to adjustably position the arm member 16 in a selected position of adjustment so that the crystal specimen 4, mounted on the specimen-plate holder element 5, which is in turn positioned on the head portion 16a, is retained at an appropriate distance from the film in the film cassette 1.
  • the previously described specimen-plate holder element is actually releasably mounted on the aforesaid head portion 16a by means of a pair of adjustment screws provided at 16b and 16c, respectively, on the said head portion. These screws 16b, 16c are engageable within aligned and threaded openings (not shown) provided in both the head portion 16a and the specimen-plate holder element 5.
  • the use of such adjustment screws, as at 16b and 16c, which facilitate the removal and attachment of crystal specimens to the said head portion 160, constitutes a key feature of the present invention, in that a number of different types of regular-shaped crystal specimens, such as the alternate form indicated at 4a in FIG.
  • FIG. 8 may be each individually mounted on a separate specimen-plate holder element, such as that at 5a, in the aforesaid FIG. 8, and thereafter each combined plate holder element and crystal specimen mounted in the order of their intended examination on the said head portion 161: and then successively and quickly X-rayed through the simple manipulation of the said screws 16b, 16c.
  • the specimen shown in FIG. 8 may, for example, represent a quartz crystal.
  • the aforementioned specimen-plate holder elements such as that indicated at 5 in FIG. 1, or that at 5a in FIG. 8, are of generally rectangular configuration and, as previously indicated, are utilized with macro-crystal specimens of generally regular shape.
  • another unique feature and advantage of the present invention is that, with the simplified hollow support member 18, which has been previously described as being positioned within the enlarged opening 17a formed in the main frame member 17, any number of different types of alternate forms of crystal holders may be utilized with, and as part of the present crystal mount assembly 30.
  • the alternate crystal holder disclosed in FIG. 9 may be easily mounted to the said main frame member 17.
  • the modified rod element shown at 24, to which the clamp device 25 may be interconnected in an opening provided therein as indicated may be easily mounted or installed within the previously described hollow support member 18 and then quickly rigidly adjusted in position through appropriate manipulation of the aforementioned adjustment screw member 19, after of course, first removing the previously installed extensible arm member 16 and head portion 16a.
  • irregularshaped, macro-crystals may be easily and quickly clamped into correct position in close proximity to the film in the film cassette 1 by means of the operation of the clamp jaws at 25a and 25b comprising the said clamp device 25.
  • the latter elements may be easily actuated between their crystal-holding and releasing positions by operation of the clamp adjustment and threaded device means at 26.
  • the previously mentioned head portion 16a may be rigidly fonned on, or affixed to one end of, a first, relatively short shaft, or rod portion 16d, as for example by means of a plurality of screw elements (not shown), or bolted or otherwise affixed thereto in any suitable manner.
  • a relatively short shaft, or rod portion 16d may be adjustably or pivotally attached one end portion of a relatively long shaft or rod portion 16f, the shaft portions 16d and 16f collectively constituting the previously described crystal holding means are member 16, and being pivotally mounted to each other at the pivot 16e.
  • This pivotal interconnection provides for tiltable or adjustable movement of the head portion 16a to permit the latter element to follow, or conform with the contour of the plane of the crystal to be examined.
  • the complete crystal mount assembly 30 further includes, in addition to the previously described crystal holding means, comprising arm member 16 and head portion 16a and main frame member 17, a baseplate portion indicated generally at 20 in FIGS. 1 and 2 and in more detail in FIGS. 5 and 6.
  • baseplate portion 20 includes a lower plate 21 (FIG. 5) and an upper plate 22 (FIG. 6).
  • lower plate 21 is specifically curved on one end portion thereof, as indicated generally at 21a, to thereby precisely interfit with a corresponding curvature on the surface of the appropriate face of, and thereby provide support for, the base support portion 23a (Note FIG.
  • a vertical goniometer at 23 which forms an important and integral part of the present crystal mount assembly 30 and which may be further appropriately bolted in an upright position to the upper plate 22, as for example by means of a screw element at 27 (FIG. 1) that engages in one appropriate opening provided therefor at 1 1 in upper plate 22 (FIG. 6). Additional rigid interconnection is provided therebetween by means of the screw element at 28 (FIG. 1) engaging within a threaded opening at 10 (FIG. 6).
  • a horizontal goniometer is illustrated at 29 as being rigidly supported in depending relation beneath said lower plate 21.
  • Said horizontal goniometer is further uniquely designed with a dial portion having a main scale inscribed thereon, as indicated at 29a, and with the bottom thereof having a centrally disposed, fiat recessed surface portion, indicated generally at 29c, and opposite side edge surfaces integrally formed thereon and disposed in downwardly depending relation therefrom, as is indicated at the reference numerals 29d and 29e, respectively.
  • the said flat recessed surface portion 290 and side edge surfaces 29d, 29:; are specifically dimensioned to exactly interfit in snug-fit, sliding relation on top of the previously described camera track 6.
  • the crystal mount assembly 30 of the present invention is both supported in a stabilized manner and is easily adjustable to the correct position relative to the film cassette 1.
  • a pair of adjustment screws are provided at 34 (Note FIG. 3) for releasably retaining the main dial portion 29a of said horizontal goniometer 29 in an adjusted position thereon.
  • the aforementioned lower and upper plates 21 and 22 are affixed to each other, as by means of screw elements interconnected therebetween, as is respectively indicated for example at the reference numerals 12 and 12a, and at 13 and 13a in the aforesaid FIGS. 5 and 6.
  • Horizontal goniometer 29 further includes a vernier scale portion at 29b which is actually inscribed on the aforementioned lower plate 21 and is revolvable or adjustable in rotation along therewith about the screw adjustable-pivot means at 48 (See FIG. 2).
  • the screw adjustment deviceat 47 is utilized to releasably retain said vernier scale portion 29b in an adjusted position relative to said main dial portion 29a.
  • the vertical goniometer 23 is affixed to the plates 21, 22 and therefore any adjustment of vernier scale portion 29b automatically rotates said vertical goniometer, and the main frame member 17 and crystal holding means 16, 16a interconnected therewith.
  • the said vertical goniometer 23 likewise incorporates a main scale-inscribed dial portion at 9 and a vernier scale portion at 23b.
  • the vertical goniometer main dial portion 9 is fixedly mounted, whereas the said vernier scale portion 23b is revolvably or rotatably mounted relative to said dial portion 9 about the pivot-stub shaft, shown at 45 as being interconnected therebetween.
  • This fixed mount for the said main dial portion 9 is, of course, ensured by the previously described rigid interconnection between its base support portion 23a and the baseplate portion 20.
  • a screw adjuster element shown at 8 as mounted on the outer end of the shaft 45, is used to releasably retain the previously noted dial portion 9 in close, adjacent proximity to the vernier scale portion 23b.
  • a second, screw adjuster element is used at 7 for releasably retaining said movably mounted vernier scale portion 23b in an adjusted position relative to said fixedly positioned dial portion 9.
  • screw adjuster element 7 extends through and is slidably engaged within an arcuate-shaped slot at 9a (Note FIG. '3) forming a track or guide means, and which is integrally formed in the surface of the said main dial portion 9.
  • the main, frame-supporting bracket member at 46 which bracket member rigidly supports the intermediate, preferably tubular-shaped frame supporting member 49, which in turn, is rigidly engaged within the relatively enlarged frame opening 49a formed adjacent the end portion of the main frame member 17 opposite the previously described enlarged frame opening 17a.
  • the said frame member 17,.and the previously described crystal specimen mounted on the plate holder element 5 is positioned in one or the other positions of adjustment by the movement of the said vernier scale portion 23b relative to said main dial portion 9.
  • the inventive system further includes a novel crystal-centering and alignment device, indicated generally at 31 in FIG. 3.
  • said device 31 is shown assembled in position with the aforesaid crystal mount assembly 30, whereas in FIG. 4, further details thereof are illustrated with the said device 31 shown disassembled from the inventive crystal mount assembly.
  • the device 31 is indicated as consisting principally of a main upright block-supporting and centering portion at 32, and one or more spacer-crystal alignment blocks at 33.
  • the above-described upright, main block-supporting and centering portion 32 may incorporate on one end thereof; namely its bottom end, a unique configuration specifically adapted to engage with, and be supported on the camera track 6.
  • the said bottom end of said centering portion 32 is made with a centrally disposed, flat recessed bottom surface portion at 35 (Note FIG. 4), which forms the oppositely disposed, depending side edge portions at 36 and 37.
  • the latter are designed to overlap opposite side edges of the camera track 6 in a substantially snug-fit, and sliding relation thereto similar to the previously described, overlapping and downwardly depending opposite side edges 29d and 29e formed on the bottom of the horizontal goniometer 29.
  • Mounted in the right side (as viewed in FIG.
  • the screwadjustment device at 38 which is used to actuate the spacer element 39 for its adjustable movement to the right or left and thereby either rigidly interconnect the crystal-centering and alignment device 31 in overlapping relation to the said camera track 6, or when appropriate, to release the same from the said track.
  • the former device may be, first, mounted in position, as shown in FIG. 3, on the camera track 6 and thereafter clamped in place by the correct adjustment of the spacer element 39 (FIG. 4) through manipulation of the screw-adjustment device 38. Thereafter, the crystal mount assembly 30 may be positioned on the same camera track 6 by mounting the horizontal goniometer 29 with its depending opposite side edges 29d and 29a in overlapping and snug-fit relation on the said track in substantially adjacent relation to the film cassette 1.
  • the said crystal mount assembly 30 is them slidably moved on the said track 6 towards the alignment device 31, which has already been mounted on the track 6, until a specifically designed cutout or recessed surface portion, indicated at 40a, in the rear supporting structure 40 provided for the main dial portion 29a of the horizontal goniometer 29, and which further supports the previously mentioned adjustment screws 34, exactly meshes with a correspondingly designed projectinglike surface formed, as indicated generally at 36a, on the previously noted depending side edge portion 36 (Note FIG. 3).
  • the said blocks 33 and the remainder of the said alignment device 31 is so dimensioned that the desired distance between the film and the crystal plane is attained, after the above-described centering operation has taken place, and the alignment device 31 thereafter removed and the crystal mount assembly 30 readjusted on the camera track 6 until it is brought into contact with the base support means (not shown) for the film cassette 1.
  • the effective distance between the plane of the crystal specimen 4 and the film in the said film cassette 1 has now been set at a predetermined distance appropriate to the present investigation, as for example, 3 cm.
  • an appropriately dimensioned spacer element such as that depicted at 41 in FIG. 7, be interposed between the centering and alignment device 31 and the face of the horizontal goniometer 29 during the previously described crystal-centering and alignment operation.
  • Another unique and novel feature of the present assembly resides in its ability to use the same film in the film cassette 1 for multiple exposures before the final development thereof occurs.
  • a number of masking elements as for example those illustrated respectively at 42, 43 and 44 in FIGS. l0, l1 and'12, may be utilized.
  • each masking element 42, 43, 44 affords an inherent or built-in capability of providing the X-ray exposure of a different crystalline plane or planes of a particular test specimen, as at 4 in FIGS. 1 and 2, by the incorporation of a cutout or X-ray-transmitting opening at a different orientation in the surface thereof.
  • FIGS. 1 and 2 one of these masking elements, namely that of FIG. 10, is depicted at 3 as being mounted in place over, and between the film cassette I and the crystal specimen 4. Said masking element 3 is retained in its position by means of the clamp device 2.
  • the same film negative may be used for several exposures of the crystal specimen 4, and thus the correct orientation thereof more quickly determined.
  • the aforementioned crystal specimen 4 after being mounted on the face of the specimen-plate holder element 5 is exposed to X-ray radiation from an appropriate X- ray generator and the X-rays generated thereby are directed in the direction of the arrow A" through an aperture or opening in the previously noted X-ray transmitting member la, from whence they are thereafter directed through appropriately aligned openings in the film cassette 1 to the crystal specimen 4. From the latter, the X-rays are diffracted back to the negative film in the film cassette 1.
  • the abovedescribed masking elements such as at 42, 43 or 44 in FIGS. 10, 11 and 12, may be utilized, in respective turn, to thereby provide for the previously noted multiple exposure of the same negative film in the said film cassette.
  • Additional exposures may be made with a particular masking element, as at 42, 43, or 44, installed with the crystal specimen 4 rotated at various angular positions of orientation by the relative adjustment respectively between the main scale-inscribed dial portions 9 and 29a, respectively, of the vertical and horizontal goniometers 23 and 29, with respect to their corresponding vemier scale-inscribed portions 23b and 29b.
  • the said relative adjustments may be made until Laue patterns of uniform distribution and thereby representing the correct crystal plane orientation have been recorded and observed on the film in the film cassette 1. Thereafter, the combined crystal holding means 16, 16a and crystal specimen 4 may be removed as a unit and transferred intact to a diamond cutter and cut to the specifications indicated by the previously determined Laue patterns.
  • an X-ray diffraction camera apparatus for taking Laue patterns and for determining the orientation of crystalline structures, and further having a camera track, film-cassette means containing a dry development type of film, and an X- ray transmitting member mounted to one side of, and having a shielded X-ray transmitting passage communicating with a central opening in the film for transmitting X-rays therethrough to the other side of said film-cassette means; a crystal mount assembly positioned in spaced relation to, and on the said other side of said film-cassette means and mounted on said camera track; said crystal mount assembly comprising; a first, direct, flat and regular-shaped, crystal specimen plateholder element mounting, and thereby retaining the crystalline structure to be X-rayed on the front surface thereof and thus in close proximity to, and on the side of, said film-cassette means and the film contained therewithin opposite from said X-ray transmitting member and in direct alignment with the X-ray path therefrom; an adjustable, indirect, and intermediate
  • said adjustable, indirect, and intermediately positioned arm support comprises a rodlike member releasably and adjustably retained at one end portion thereof in telescopic, mounted relation within the said hollow support member incorporated in one side of said main, crystal specimen-frame support element; and said indirect, plate-holder element comprises an enlarged head portion assembled to the opposite end of said arm support and being further interconnected with a macro-crystal specimen of substantially regular configuration; said head portion being pivotally and adjustably mounted on l of said main, crystal specimen-frame support element, and further projecting outwardly therefrom towards said film-cassette means and film and terminating in a second end portion in close proximity to said film and incorporating a pair of jawlike elements adjustable relative to each other for thereby releasably retaining macro-crystal specimens of different sizes and irregular configurations.

Abstract

A combined, portable crystal mount and goniometer apparatus having built-in vertical and horizontal goniometer members, and an adjustably mounted crystal holder member adapted to be rigidly positioned on the camera track of a standard type of X-ray diffraction apparatus and thereby extend the latter''s inherent ability in taking Laue patterns of small types of crystalline structures to the further capability of taking X-ray diffraction pictures of the relatively large or macro-type crystal.

Description

ilnited States Patent [72] Inventor Frank L. Chan 3228 Ravenwood Road, Fairborn, Ohio 45324 [211 App]. No. 821,595
[22] Filed May 5, 1969 [45] Patented Aug. 17, 1971 [54] CRYSTAL MOUNT AND GONIOMETER FOR TAKING LAUE PATTERNS AND FOR ORIENTATION OF LARGE SINGLE CRYSTALS 3 Claims, 12 Drawing Figs.
[52] U.S. Cl 250/51,5, 250/65 R [51] lnt.-Cl G0ln 23/20 [50] Field of Search 250/5 1 .5
[56] References Cited UNITED STATES PATENTS 2,820,904 1/1958 Lowitzsch 250/51.5
2,904,688 9/1959 Miller 250/51.5 3,384,748 5/1968 Rioux eta1.... 250/51.5 3,443,091 5/1969 Bartlett et a1. 250/51.5 2,545,899 3/1951 Soba 250/66 Primary ExaminerJames W. Lawrence Assistant Examiner-C. E. Church Attorneysl-larry A. Herbert, Jr. and Arthur R. Parker ABSTRACT: A combined, portable crystal mount and goniometer apparatus having built-in vertical and horizontal goniometer members, and an adjustably mounted crystal holder member adapted to be rigidly positioned on the camera track of a standard type of X-ray diffraction apparatus and thereby extend the latters inherent ability in taking Laue patterns of small types of crystalline structures to the further capability of taking X-ray diffraction pictures of the relatively large or macro-type crystal.
PATENTED mm 1 ISYI v 3500575 sum-u BF 4 I! I5 INVENTOR.
Arm/4' 1- an? CRYSTAL MOUNT AND GONIOMETER FOR TAKING LAUE PATTERNS AND FOR ORIENTATION OF LARGE SINGLE CRYSTALS BACKGROUND OF THE INVENTION The present invention relates generally to the taking of X- ray diffraction pictures of crystal structures and in particular, to an improved combined crystal holder and goniometer device for assisting in the production of Laue patterns of the macro-type of crystals. i I
In the present investigation of various crystalline structures, certain natural crystals have been collected from North Dakota, Colorado, the Far East, and more recently, from South America, and in particular, from Brazil. Crystalline structures have been utilized to good effect in various fields of interest to the research community, such as in communications. This interest has encouraged the development of different techniques in the study of crystals and, in particular, X- ray diffraction cameras have been utilized for some time to obtain Laue patterns, and thereby identify the particular structure of certain crystals. Previously developed cameras of this type have used the wet development process in order to develop the film exposed to the X-ray of theparticular crystal under examination. Because of the considerable extended time periods required in the wet process development, the use of a dry development process involving the Polaroid flat film cassette for obtaining the aforementioned Laue pattern has been under recent consideration. With the latter method, the so-called back reflection type of X-ray pictures are produced.
Since'the aforementioned dry development process offers obvious and significant advantage in the X-ray diffraction picture study of crystalline structures due to i s speed of development, further study thereof has continued; however one apparent disadvantage has been that with presently existing crystal mounting means, only the smaller type of'crystals can be satisfactorily X-rayed. The crystal mounting means resulting from the present study is considered unique in that it may be combined with previously-developed X'ray diffraction apparatus and thereby ensure the investigation of the larger, or macro-type specimens to determine their particular crystalline structure. The present system for examining the macro-type crystal, which may be taken as meaning crystals of a size in excess of 1 inch X 3 inch X inch, accomplishes its function in the novel manner to be hereinafter summarized and explained in detail.
SUMMARY OF THE INVENTION The present invention consists of a combined crystal mount and goniometer mechanism which includes basically a vertical goniometer element, a main frame member supported in posi tion by the vertical goniometer, an adjustable crystal holder element mounted to the main frame member, and a horizontal goniometer element having base support means for supporting the vertical goniometer. The vertical goniometer further includes a dial portion having a main scale inscribed thereon and a vernier scale portion which is the element that specifically supports the main frame member. This vernier scale portion is rotatably supported relative to the dial portion and is adjustable to various positions of adjustment to thereby simultaneously adjust the main frame member and the crystal holder element supported thereby to various positions of orientation about a horizontal axis.
The horizontal goniometer also includes a main dial portion which is shaped to interfit with the camera track of the X-ray diffraction apparatus with which it is combined, and a vernier scale portion. The latter constitutes one element of the base support means, and it is movable in rotation relative to the last-named, main dial portion. Since the base support means is rigidly interconnected with the vertical goniometer, any movement of the said horizontal goniometer-vernier scale portion also moves or adjusts the main frame member and crystal holder element about a vertical axis, the collective adjustment of the crystal holder element about both vertical and horizontal axes thereby providing for the determination of the crystal orientation.
Other advantages, as well as objects, of the present invention will become readily apparent from the following detailed description of the invention, taken in connection with the accompanying drawings, in which:
SUMMARY OF THE DRAWINGS FIG. 1 is a top assembly view of the crystal mount and goniometer arrangement of the present invention shown positioned on the camera track of an existing mechanism;
FIG. 2 is a front view of the assembly of FIG. 1, illustrating further details of the crystal mount and goniometer arrangement of the present invention;
FIG. 3 is a right side view of the invention of FIGS. 1 and 2,
illustrating still further details of the crystal mount and goniometer arrangement, and in particular, illustrating the unique crystal alignment device used with the inventive crystal mount assembly;
FIG. 4 is another front view, illustrating further details of the novel crystal alignment device shown in FIG. 3;
FIGS. 5 and 6 represent top views of the lower and upper base plate members, respectively, that are utilized as an integral part of the inventive crystal mount;
FIG. 7 represents a front view of one type of spacer element which may be placed between the film cassette support means of an X-ray diffraction camera apparatus and the crystal mount of the present invention for thereby determining the correct distance between the plane of the crystal specimen under investigation and the film being exposed to the X-rays 'thereof;
FIG. 8 illustrates a quartz crystal specimen shown mounted on a plate-form of crystal holder which, in turn, may be positioned on an extensiblearm element of the main crystal mount of the present invention;
FIG. 9 represents another form of crystal holder which is utilizable with the present crystal mount, and which further shows a representative example of one type of clamp device utilizable for holding irregular-shaped, macrocrystals on the inventive crystal mount; and
FIGS. 10, 11 and 12 respectively represent plan views of various forms of screen elements adapted to be used with the crystal holder of the present invention for uniquely providing for multiple exposure of the film in examining the crystal structure of the specimen under investigation.
DESCRIPTION OF THE PREFERRED EMBODIMENT Referring generally to the drawings and, in particular, to FIGS. 1 and 2 thereof, the improved crystal mount assembly of the present invention is indicated generally at 30 as being mounted in position on a relatively enlarged, supporting member at 6 representing the camera track of an X-ray diffraction camera apparatus. The film cassette of this camera is shown at I. Said X-ray diffraction camera apparatus may include an X-ray generator (not shown) which provides the source of X-rays to be used in the investigation of one or more types of crystal specimens in the new and improved manner to be described in more detail hereinafter. In this regard, X-rays produced by such an X-ray generator are indicated in the present description by means of an arrow marked A" in FIG. 1. For the purpose of transmitting and directing the X-rays so produced, the relatively elongated and shielded X-ray transmitting member at In may be utilized. An X-ray shielding shutter element may be provided in one portion of said X-ray transmitting member, as is indicated at the reference numeral 1c, which shielding shutter element 10 may be utilized to open or close the end of an X-ray transmitting passage (not shown) in the member la and thereby control the transmission of X- rays from the X-ray source. Said relatively elongated member 1a is shown supported within a relatively enlarged base support 1b which is, in turn, supported to one side of the film cassette 1. A screw adjustment device is utilized at 1d to releasably retain the member 1a interconnected with the support 1b. Of course, support 1b and said film cassette 1 may likewise be shielded and incorporate communicating and centrally located X-ray transmitting passages to thereby provide for the transmission of, and therefore the exposure to X-rays of any crystal specimen, such as that depicted at 4. Such rays are thereafter difiracted to the film negative in the film cassette 1 to form thereon the previously mentioned Laue patterns.
The aforementioned crystal specimen 4, which may consist of a relatively enlarged crystal sample of substantially rectangular or other regular shape, is shown as being mounted in close proximity to the film in the said film cassette 1 by means of a metallic specimen-plate holder element 5. The latter, which is also made into a rectangular configuration, is in turn mounted on a second, metallic plate of similar configuration. This second plate consists of the head portion 16a of a relatively elongated arm member 16 which, together therewith, constitutes one form of a crystal holding means utilized with, and forming an integral part of, the overall crystal mount assembly 30 of the present invention. Said arm member 16 is releasably or extensibly held within, and thus is supported by an enlarged, hollow, and relatively long and preferably tubular-shaped arm-support member 18. The'latter member 18 is, in turn, releasably retained in close-fitting relation within a relatively enlarged opening 17a (Note FIG. 2) provided adjacent one end portion of the main, rectangular-shaped, frame member 17 of the present crystal mount assembly 30. The said arm-support member 18 is made hollow in form, as indicated hereinbefore, and is designed with an inside diameter surface portion so dimensioned as to snugly fit the outside diameter surface of said arm member 16, as is indicated in the aforementioned FIGS. 1 and 2. The said main frame member 17 is provided adjacent to the end thereof containing the aforesaid opening 170 with a narrow cutout, or groove at 17b which groove 17b provides an opening in the top surface of the frame member 17 and further extends downwardly therefrom to communicate with the aforesaid enlarged opening 17a. With this arrangement, and with the use of an adjustment screw (not shown) built into the side edge portion of said frame member 17 at a point substantially adjacent the top surface thereof and adapted to extend inwardly a sufiicient distance, the said arm-support member 18 may be releasably retained at a selected position within the opening 17a and, in this manner, ease of assembly and/or repair of the inventive arrangement may be facilitated. In the same manner, an adjustment screw member at 19 (Note FIGS. 1 and 2) may be utilized to adjustably position the arm member 16 in a selected position of adjustment so that the crystal specimen 4, mounted on the specimen-plate holder element 5, which is in turn positioned on the head portion 16a, is retained at an appropriate distance from the film in the film cassette 1.
The previously described specimen-plate holder element is actually releasably mounted on the aforesaid head portion 16a by means of a pair of adjustment screws provided at 16b and 16c, respectively, on the said head portion. These screws 16b, 16c are engageable within aligned and threaded openings (not shown) provided in both the head portion 16a and the specimen-plate holder element 5. The use of such adjustment screws, as at 16b and 16c, which facilitate the removal and attachment of crystal specimens to the said head portion 160, constitutes a key feature of the present invention, in that a number of different types of regular-shaped crystal specimens, such as the alternate form indicated at 4a in FIG. 8, may be each individually mounted on a separate specimen-plate holder element, such as that at 5a, in the aforesaid FIG. 8, and thereafter each combined plate holder element and crystal specimen mounted in the order of their intended examination on the said head portion 161: and then successively and quickly X-rayed through the simple manipulation of the said screws 16b, 16c. The specimen shown in FIG. 8 may, for example, represent a quartz crystal.
The aforementioned specimen-plate holder elements, such as that indicated at 5 in FIG. 1, or that at 5a in FIG. 8, are of generally rectangular configuration and, as previously indicated, are utilized with macro-crystal specimens of generally regular shape. However, in the event it is desired to subject macro-crystals of irregular shape to X-ray diffraction examination, another unique feature and advantage of the present invention is that, with the simplified hollow support member 18, which has been previously described as being positioned within the enlarged opening 17a formed in the main frame member 17, any number of different types of alternate forms of crystal holders may be utilized with, and as part of the present crystal mount assembly 30. For instance, to properly support crystal specimens of irregular configuration, the alternate crystal holder disclosed in FIG. 9 may be easily mounted to the said main frame member 17. Thus, the modified rod element shown at 24, to which the clamp device 25 may be interconnected in an opening provided therein as indicated, may be easily mounted or installed within the previously described hollow support member 18 and then quickly rigidly adjusted in position through appropriate manipulation of the aforementioned adjustment screw member 19, after of course, first removing the previously installed extensible arm member 16 and head portion 16a. In this manner, irregularshaped, macro-crystals may be easily and quickly clamped into correct position in close proximity to the film in the film cassette 1 by means of the operation of the clamp jaws at 25a and 25b comprising the said clamp device 25. The latter elements may be easily actuated between their crystal-holding and releasing positions by operation of the clamp adjustment and threaded device means at 26.
Again referring to FIG. 1, it is seen that the previously mentioned head portion 16a may be rigidly fonned on, or affixed to one end of, a first, relatively short shaft, or rod portion 16d, as for example by means of a plurality of screw elements (not shown), or bolted or otherwise affixed thereto in any suitable manner. To the other end of said relatively short shaft, or rod portion 16d may be adjustably or pivotally attached one end portion of a relatively long shaft or rod portion 16f, the shaft portions 16d and 16f collectively constituting the previously described crystal holding means are member 16, and being pivotally mounted to each other at the pivot 16e. This pivotal interconnection provides for tiltable or adjustable movement of the head portion 16a to permit the latter element to follow, or conform with the contour of the plane of the crystal to be examined.
The complete crystal mount assembly 30 further includes, in addition to the previously described crystal holding means, comprising arm member 16 and head portion 16a and main frame member 17, a baseplate portion indicated generally at 20 in FIGS. 1 and 2 and in more detail in FIGS. 5 and 6. As particularly viewed in the latter figures, baseplate portion 20 includes a lower plate 21 (FIG. 5) and an upper plate 22 (FIG. 6). As noted in FIG. 5, lower plate 21 is specifically curved on one end portion thereof, as indicated generally at 21a, to thereby precisely interfit with a corresponding curvature on the surface of the appropriate face of, and thereby provide support for, the base support portion 23a (Note FIG. 2) of a vertical goniometer at 23, which forms an important and integral part of the present crystal mount assembly 30 and which may be further appropriately bolted in an upright position to the upper plate 22, as for example by means of a screw element at 27 (FIG. 1) that engages in one appropriate opening provided therefor at 1 1 in upper plate 22 (FIG. 6). Additional rigid interconnection is provided therebetween by means of the screw element at 28 (FIG. 1) engaging within a threaded opening at 10 (FIG. 6). In this connection, a horizontal goniometer is illustrated at 29 as being rigidly supported in depending relation beneath said lower plate 21. Said horizontal goniometer is further uniquely designed with a dial portion having a main scale inscribed thereon, as indicated at 29a, and with the bottom thereof having a centrally disposed, fiat recessed surface portion, indicated generally at 29c, and opposite side edge surfaces integrally formed thereon and disposed in downwardly depending relation therefrom, as is indicated at the reference numerals 29d and 29e, respectively. With such an arrangement, the said flat recessed surface portion 290 and side edge surfaces 29d, 29:; are specifically dimensioned to exactly interfit in snug-fit, sliding relation on top of the previously described camera track 6. In this manner, the crystal mount assembly 30 of the present invention is both supported in a stabilized manner and is easily adjustable to the correct position relative to the film cassette 1. For this purpose, a pair of adjustment screws are provided at 34 (Note FIG. 3) for releasably retaining the main dial portion 29a of said horizontal goniometer 29 in an adjusted position thereon. The aforementioned lower and upper plates 21 and 22 are affixed to each other, as by means of screw elements interconnected therebetween, as is respectively indicated for example at the reference numerals 12 and 12a, and at 13 and 13a in the aforesaid FIGS. 5 and 6.
Horizontal goniometer 29 further includes a vernier scale portion at 29b which is actually inscribed on the aforementioned lower plate 21 and is revolvable or adjustable in rotation along therewith about the screw adjustable-pivot means at 48 (See FIG. 2). Naturally, since, lower plate 21 is affixed to the upper plate 22, the latter element is also adjusted along with the said vernier scale portion. To releasably retain said vernier scale portion 29b in an adjusted position relative to said main dial portion 29a, the screw adjustment deviceat 47 is utilized. Of course, the vertical goniometer 23 is affixed to the plates 21, 22 and therefore any adjustment of vernier scale portion 29b automatically rotates said vertical goniometer, and the main frame member 17 and crystal holding means 16, 16a interconnected therewith. The said vertical goniometer 23 likewise incorporates a main scale-inscribed dial portion at 9 and a vernier scale portion at 23b. As in the case of the previously described horizontal goniometer 29, the vertical goniometer main dial portion 9 is fixedly mounted, whereas the said vernier scale portion 23b is revolvably or rotatably mounted relative to said dial portion 9 about the pivot-stub shaft, shown at 45 as being interconnected therebetween. This fixed mount for the said main dial portion 9 is, of course, ensured by the previously described rigid interconnection between its base support portion 23a and the baseplate portion 20. A screw adjuster element shown at 8 as mounted on the outer end of the shaft 45, is used to releasably retain the previously noted dial portion 9 in close, adjacent proximity to the vernier scale portion 23b. A second, screw adjuster element is used at 7 for releasably retaining said movably mounted vernier scale portion 23b in an adjusted position relative to said fixedly positioned dial portion 9. For this purpose, screw adjuster element 7 extends through and is slidably engaged within an arcuate-shaped slot at 9a (Note FIG. '3) forming a track or guide means, and which is integrally formed in the surface of the said main dial portion 9.
integrally formed with, and as an extension to the aforesaid vernier scale portion 23b of the said vertical goniometer 23 is the main, frame-supporting bracket member at 46, which bracket member rigidly supports the intermediate, preferably tubular-shaped frame supporting member 49, which in turn, is rigidly engaged within the relatively enlarged frame opening 49a formed adjacent the end portion of the main frame member 17 opposite the previously described enlarged frame opening 17a. Thus, the said frame member 17,.and the previously described crystal specimen mounted on the plate holder element 5 is positioned in one or the other positions of adjustment by the movement of the said vernier scale portion 23b relative to said main dial portion 9. b
In addition to the above-described crystal mount assembly 30, the inventive system further includes a novel crystal-centering and alignment device, indicated generally at 31 in FIG. 3. In the latter FIG. 3, said device 31 is shown assembled in position with the aforesaid crystal mount assembly 30, whereas in FIG. 4, further details thereof are illustrated with the said device 31 shown disassembled from the inventive crystal mount assembly. The device 31 is indicated as consisting principally of a main upright block-supporting and centering portion at 32, and one or more spacer-crystal alignment blocks at 33.
The above-described upright, main block-supporting and centering portion 32 may incorporate on one end thereof; namely its bottom end, a unique configuration specifically adapted to engage with, and be supported on the camera track 6. For this purpose, the said bottom end of said centering portion 32 is made with a centrally disposed, flat recessed bottom surface portion at 35 (Note FIG. 4), which forms the oppositely disposed, depending side edge portions at 36 and 37. The latter are designed to overlap opposite side edges of the camera track 6 in a substantially snug-fit, and sliding relation thereto similar to the previously described, overlapping and downwardly depending opposite side edges 29d and 29e formed on the bottom of the horizontal goniometer 29. Mounted in the right side (as viewed in FIG. 4) of the said main upright block-supporting and centering portion 32, adjacent to the said depending side edge portion 36 is the screwadjustment device at 38, which is used to actuate the spacer element 39 for its adjustable movement to the right or left and thereby either rigidly interconnect the crystal-centering and alignment device 31 in overlapping relation to the said camera track 6, or when appropriate, to release the same from the said track.
In utilizing the above-described alignment device 31 with the inventive crystal mount assembly 30 in order to properly center and position the crystal specimen 4 at the correct distance relative to the film in the film cassette 1, the former device may be, first, mounted in position, as shown in FIG. 3, on the camera track 6 and thereafter clamped in place by the correct adjustment of the spacer element 39 (FIG. 4) through manipulation of the screw-adjustment device 38. Thereafter, the crystal mount assembly 30 may be positioned on the same camera track 6 by mounting the horizontal goniometer 29 with its depending opposite side edges 29d and 29a in overlapping and snug-fit relation on the said track in substantially adjacent relation to the film cassette 1. The said crystal mount assembly 30 is them slidably moved on the said track 6 towards the alignment device 31, which has already been mounted on the track 6, until a specifically designed cutout or recessed surface portion, indicated at 40a, in the rear supporting structure 40 provided for the main dial portion 29a of the horizontal goniometer 29, and which further supports the previously mentioned adjustment screws 34, exactly meshes with a correspondingly designed projectinglike surface formed, as indicated generally at 36a, on the previously noted depending side edge portion 36 (Note FIG. 3). Once the surfaces 36a and 40a having fully intermeshed and the said adjustrnent screws 34 clamped in position, then it is only necessary to adjust the position of the crystal specimen 4 by the slidable manipulation of the previously described crystal holding means arm member 16 (Note FIGS. 1 and 2) within its hollow support member 18 until the plane of the said crystal specimen 4 and the previously noted blocks 33 are brought into contact with each other. Of course, the said blocks 33 and the remainder of the said alignment device 31 is so dimensioned that the desired distance between the film and the crystal plane is attained, after the above-described centering operation has taken place, and the alignment device 31 thereafter removed and the crystal mount assembly 30 readjusted on the camera track 6 until it is brought into contact with the base support means (not shown) for the film cassette 1. At this time, the effective distance between the plane of the crystal specimen 4 and the film in the said film cassette 1 has now been set at a predetermined distance appropriate to the present investigation, as for example, 3 cm. Should a different distance, such as 5 cm., be desired, it is only required that an appropriately dimensioned spacer element, such as that depicted at 41 in FIG. 7, be interposed between the centering and alignment device 31 and the face of the horizontal goniometer 29 during the previously described crystal-centering and alignment operation. Another unique and novel feature of the present assembly resides in its ability to use the same film in the film cassette 1 for multiple exposures before the final development thereof occurs. To this end, a number of masking elements, as for example those illustrated respectively at 42, 43 and 44 in FIGS. l0, l1 and'12, may be utilized. As seen clearly in the said figures, each masking element 42, 43, 44 affords an inherent or built-in capability of providing the X-ray exposure of a different crystalline plane or planes of a particular test specimen, as at 4 in FIGS. 1 and 2, by the incorporation of a cutout or X-ray-transmitting opening at a different orientation in the surface thereof. In FIGS. 1 and 2, one of these masking elements, namely that of FIG. 10, is depicted at 3 as being mounted in place over, and between the film cassette I and the crystal specimen 4. Said masking element 3 is retained in its position by means of the clamp device 2. In this way, by the alternate and/or successive use of different masking elements, as at 42, 43, 44, the same film negative may be used for several exposures of the crystal specimen 4, and thus the correct orientation thereof more quickly determined.
In operation, the aforementioned crystal specimen 4, after being mounted on the face of the specimen-plate holder element 5 is exposed to X-ray radiation from an appropriate X- ray generator and the X-rays generated thereby are directed in the direction of the arrow A" through an aperture or opening in the previously noted X-ray transmitting member la, from whence they are thereafter directed through appropriately aligned openings in the film cassette 1 to the crystal specimen 4. From the latter, the X-rays are diffracted back to the negative film in the film cassette 1. During this process, the abovedescribed masking elements such as at 42, 43 or 44 in FIGS. 10, 11 and 12, may be utilized, in respective turn, to thereby provide for the previously noted multiple exposure of the same negative film in the said film cassette. Additional exposures may be made with a particular masking element, as at 42, 43, or 44, installed with the crystal specimen 4 rotated at various angular positions of orientation by the relative adjustment respectively between the main scale-inscribed dial portions 9 and 29a, respectively, of the vertical and horizontal goniometers 23 and 29, with respect to their corresponding vemier scale-inscribed portions 23b and 29b. The said relative adjustments may be made until Laue patterns of uniform distribution and thereby representing the correct crystal plane orientation have been recorded and observed on the film in the film cassette 1. Thereafter, the combined crystal holding means 16, 16a and crystal specimen 4 may be removed as a unit and transferred intact to a diamond cutter and cut to the specifications indicated by the previously determined Laue patterns.
I claim:
1. In an X-ray diffraction camera apparatus for taking Laue patterns and for determining the orientation of crystalline structures, and further having a camera track, film-cassette means containing a dry development type of film, and an X- ray transmitting member mounted to one side of, and having a shielded X-ray transmitting passage communicating with a central opening in the film for transmitting X-rays therethrough to the other side of said film-cassette means; a crystal mount assembly positioned in spaced relation to, and on the said other side of said film-cassette means and mounted on said camera track; said crystal mount assembly comprising; a first, direct, flat and regular-shaped, crystal specimen plateholder element mounting, and thereby retaining the crystalline structure to be X-rayed on the front surface thereof and thus in close proximity to, and on the side of, said film-cassette means and the film contained therewithin opposite from said X-ray transmitting member and in direct alignment with the X-ray path therefrom; an adjustable, indirect, and intermediately positioned, arm support extending towards and at right angles to the plane of said film-cassette means when in one position of adjustment, and having one end portion incorporating a second, indirect, flat and regular-shaped, plateholder element arranged in releasable mounting relation to the rear surface of said first, direct-crystal specimen plateholder element; and a combined crystal specimen-andgoniometer-adjustable support means comprising; a main, crystal specimen-frame support element having a hollow support member mounted in one side thereof and adjustably supporting therein in snug-fit and telescopically arranged relation to said intermediately positioned and crystal specimen-indirect mounting, arm support for thereby maintaining the position of the said crystal specimen indirectly supported to the second, indirect plate-holder element thereof in the apparatus X-ray path and at various predetermined adjustable distances from, and to the rear of said film-cassette means and film; and goniometer-base support means interconnected with, and thereby retaining said main, crystal specimen-frame support element in upright relation on, and relative thereto, and further incorporating a pair of goniometer devices oriented at right angles to each other for selectively adjusting said frame support element and the crystal specimen supported thereby about two axes disposed normal to each other; said pair of goniometer devices including a combined vertical goniometer device and vertical support means for adjustably supporting said main, crystal specimen-frame support element in its upright relation comprising a fixed, main, vertical goniometer-scale-inscribed dial portion, a vertical goniometer-vemier scale portion revolvable on, and movable relative to, said main, vertical goniometer-seale-inscribed dial portion about a supporting pivot shaft extending therebetween for adjusting the position of said main, frame support element and the crystal specimen carried thereby about a first, horizontal axis, and means interconnecting said vertical goniometer device to said main, frame support element comprising a supporting bracket member fixed at one end thereof to the said pivot shaft of said vertical goniometer-vemier scale portion, and a tubular-shaped, interconnecting member fixed at one end thereof to the other end of said bracket member and attached to, and thereby supporting in fixed relation at the other end thereof the side of said main, crystal specimen-frame support element remote from the attachment of its hollow support member with said intermediately positioned arm support; and a combined horizontal goniometer device and horizontal support means comprising a first, main, horizontal base support plate portion rigidly affixed at one side thereof to the bottom of, and thereby supporting said fixed, main, vertical goniometer-scale-inscribed dial portion in upright rigid relation thereon, a second, horizontal goniometer-vemier scale plate portion rigidly supported in depending relation from, and rigidly interconnected with, said first, main horizontal base support plate portion, and a third, fixed, main, horizontal goniometer-scale-inscribed dial plate portion supported in depending relation from said second, horizontal goniometervernier scale plate portion and further incorporating a centrally disposed recessed portion on the bottom surface thereof in slidable adjusting and snug-fit relation on said camera track, said rigidly interconnected horizontal goniometer-vemier scale and base support plate portions being collectively revolvably mounted to the upper surface of said fixed, main horizontal goniometer-scale-inscribed dial plate portion for simultaneously adjusting the said main, vertical goniometerscale-inscribed dial portion, and said main, frame support element and crystal specimen interconnected therewith about a second axis oriented in transverse relation to the adjustment of said vertical goniometer-vemier scale portion about said first-named axis.
2. In an X-ray diffraction camera apparatus as in claim 1, wherein said adjustable, indirect, and intermediately positioned arm support comprises a rodlike member releasably and adjustably retained at one end portion thereof in telescopic, mounted relation within the said hollow support member incorporated in one side of said main, crystal specimen-frame support element; and said indirect, plate-holder element comprises an enlarged head portion assembled to the opposite end of said arm support and being further interconnected with a macro-crystal specimen of substantially regular configuration; said head portion being pivotally and adjustably mounted on l of said main, crystal specimen-frame support element, and further projecting outwardly therefrom towards said film-cassette means and film and terminating in a second end portion in close proximity to said film and incorporating a pair of jawlike elements adjustable relative to each other for thereby releasably retaining macro-crystal specimens of different sizes and irregular configurations.

Claims (2)

  1. 2. In an X-ray diffraction camera apparatus as in claim 1, wherein said adjustable, indirect, and intermediately positioned arm support comprises a rodlike member releasably and adjustably retained at one end portion thereof in telescopic, mounted relation within the said hollow support member incorporated in one side of said main, crystal specimen-frame support element; and said indirect, plate-holder element comprises an enlarged head portion assembled to the opposite end of said arm support and being further interconnected with a macro-crystal specimen of substantially regular configuration; said head portion being pivotally and adjustably mounted on said rodlike member to enable its independent movement and adjustment relative thereto and thus follow or conform with the contour of the crystal specimen mounted thereon.
  2. 3. In an X-ray diffraction camera apparatus as in claim 1, wherein said adjustable, indirect, and intermediately positioned arm support comprises a clamp device having a main support incorporating one end porTion releasably and adjustably interfitting in an enlarged opening formed in one side of said main, crystal specimen-frame support element, and further projecting outwardly therefrom towards said film-cassette means and film and terminating in a second end portion in close proximity to said film and incorporating a pair of jawlike elements adjustable relative to each other for thereby releasably retaining macro-crystal specimens of different sizes and irregular configurations.
US821595A 1969-05-05 1969-05-05 Crystal mount and goniometer for taking laue patterns and for orientation of large single crystals Expired - Lifetime US3600575A (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
FR2596154A1 (en) * 1986-03-18 1987-09-25 Labo Electronique Physique DEVICE FOR MEASURING THE ORIENTATION OF MONOCRYSTALLINE MASSIVE MATERIALS BY THE LAUNE METHOD
US5870832A (en) * 1996-03-18 1999-02-16 Slocum; Barclay Frame for gravity-related measurement device
USD433641S (en) * 1996-03-04 2000-11-14 D. Barclay Slocum Goniometer frame

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US2545899A (en) * 1949-01-26 1951-03-20 Jose G Soba Multiple x-ray picture seriating device
US2820904A (en) * 1952-10-25 1958-01-21 Philips Corp Crystal holder
US2904688A (en) * 1958-06-06 1959-09-15 Super Cut Cassette and holder therefor for back reflection cameras
US3384748A (en) * 1964-04-03 1968-05-21 Centre Nat Rech Scient Goniometric supports for supporting crystal during crystal analysis and subsequent cutting
US3443091A (en) * 1966-05-02 1969-05-06 Polaroid Corp Single apparatus with means to perform a back-reflection or transmission diffraction method of x-ray photography

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Publication number Priority date Publication date Assignee Title
US2545899A (en) * 1949-01-26 1951-03-20 Jose G Soba Multiple x-ray picture seriating device
US2820904A (en) * 1952-10-25 1958-01-21 Philips Corp Crystal holder
US2904688A (en) * 1958-06-06 1959-09-15 Super Cut Cassette and holder therefor for back reflection cameras
US3384748A (en) * 1964-04-03 1968-05-21 Centre Nat Rech Scient Goniometric supports for supporting crystal during crystal analysis and subsequent cutting
US3443091A (en) * 1966-05-02 1969-05-06 Polaroid Corp Single apparatus with means to perform a back-reflection or transmission diffraction method of x-ray photography

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2596154A1 (en) * 1986-03-18 1987-09-25 Labo Electronique Physique DEVICE FOR MEASURING THE ORIENTATION OF MONOCRYSTALLINE MASSIVE MATERIALS BY THE LAUNE METHOD
EP0241061A2 (en) * 1986-03-18 1987-10-14 Laboratoires D'electronique Philips Device for the measurement of the orientation of bulky monocrystalline materials using the Laue method
EP0241061A3 (en) * 1986-03-18 1990-03-07 Laboratoires D'electronique Philips Device for the measurement of the orientation of bulky monocrystalline materials using the laue method
USD433641S (en) * 1996-03-04 2000-11-14 D. Barclay Slocum Goniometer frame
US5870832A (en) * 1996-03-18 1999-02-16 Slocum; Barclay Frame for gravity-related measurement device

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