# US 5,703,366 A · Optical sensing with crystal assembly sensing tip > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,703,366 A - Document ID: US5703366A - Status: Granted - Kind: A - Application number: 08/706,169 - Filed: 1996-08-30 - Granted: 1997-12-30 - Earliest claimed: 1994-05-13 - Assignees: ASI Applied Systems, L.L.C. - Inventors: Donald W. Sting; Milan Milosevic - Web page: https://patentgrep.com/patent/US5703366A ## CPC - G01N 21/474: {Details of optical heads therefor, e.g. using optical fibres} - G01N 21/552: Attenuated total reflection - G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q) ## Abstract A crystal assembly for optical analyzation of samples includes a first crystal member and a second crystal member, the latter of which is preferably a diamond. The first and second crystal members, which have substantially the same index of refraction for infrared energy, are coupled together at an optically transmitting interface. This interface may be formed by crystal surfaces in intimate contact with one another or by a third crystal member positioned therebetween. The first crystal member has at least one circumferential sidewall focusing surface for redirecting infrared energy within the first crystal member to and from a focal ring or focal plane at or near the optical interface. The focused infrared energy transmitted from the first crystal member is internally reflected within the second crystal member to obtain encoding specific to a sample in contact with a surface of the second crystal member. The encoded infrared energy is then reflected back into the first crystal member for ultimate transmission to a detector. ## Claims ### Claim 1 An optical analytical system having a source of infrared energy, an infrared detector system, and a crystal assembly comprising a first crystal member having at least one circumferential focusing surface, and a crystal disc, an optically transmitting interface between at least a portion of one surface of the first crystal member and at least a portion of an adjacent surface of the crystal disc, said crystal disc having a sample contacting surface which is opposite said optically transmitting interface, said source energy being redirected by a circumferential focusing surface, transmitted through said optical interface, and totally internally reflected in the second crystal at least once at the sample contacting surface, whereby said source energy obtains sample specific encoding; and said encoded source energy being transmitted from the crystal disc through the optically transmitting interface into said first crystal member and redirected by a circumferential focusing surface to the infrared detector system for sample analyzation. ### Claim 2 (depends on 1) The analytical system of claim 1 wherein the crystal disc is a diamond and the material of the first crystal member is selected to have an index of refraction for infrared energy substantially similar to the index of refraction for infrared energy of the diamond. ### Claim 3 (depends on 1) The analytical system of claim 1 wherein said source energy is totally internally reflected two or more times at the sample contacting surface. ### Claim 4 (depends on 3) The analytical system of claim 3 wherein the first crystal member has a cavity symmetrically formed therein adjacent the optically transmitting interface and sized to let infrared energy in and out of the crystal disc while permitting total internal reflection within the crystal disc between entry and exist. ### Claim 5 (depends on 3) The analytical system of claim 3 wherein at least a portion of the surface of said crystal disc adjacent to said optically transmitting interface is reflectively coated to optimize the energy reflected at that surface. ### Claim 6 (depends on 1) The analytical system of claim 1 wherein the optically transmitting interface comprises a third crystal member positioned between the first crystal member and crystal disc in intimate optically transmitting contact therewith. ### Claim 7 (depends on 6) The analytical system of claim 6 wherein the third crystal member is at least one thin layer deposited between the first crystal member and crystal disc. ### Claim 8 (depends on 6) The analytical system of claim 6 wherein the crystal disc is diamond, the first and third crystal members have an index of refraction substantially similar to the diamond and the third crystal member has one surface thereof adjacent the first crystal member at least partly reflectively coated to permit internal reflection of the infrared energy within the diamond and the third crystal member. ### Claim 9 (depends on 1) The analytical system of claim 1 wherein the first crystal member has a transmission surface through which infrared energy enters and leaves the first crystal member, and wherein said analytical system includes an energy waveguide containing a transmissive medium through which infrared energy passes before entering and after leaving the first crystal member, the first crystal member having a higher index of refraction than the transmissive medium to reduce infrared energy divergence angles in the first crystal member as compared to that present in the transmissive medium. ### Claim 10 (depends on 9) The analytical system of claim 9 wherein the transmission medium is divided by a partition extending at or near to the transmission surface of the first crystal member to define separate infrared energy entry and exit paths. ### Claim 11 (depends on 10) The analytical system of claim 10 wherein the crystal assembly is mounted on the end of a tube to form a sensing probe and the partition has mirrored surfaces on both sides and extends down the tube at or near its center. ### Claim 12 (depends on 9) The crystal assembly of claim 9 wherein the first crystal member includes a substantially cylindrical portion between the transmission surface and the circumferential focusing surface. ### Claim 13 (depends on 1) The analytical of claim 1 wherein two circumferential focusing surfaces are diametrically opposed to one another and have symmetrical arcuate surfaces in elevation. ### Claim 14 (depends on 1) The analytical system of claim 1 wherein the first crystal member has, in elevation, multiple circumferential focusing surfaces for sequentially redirecting infrared energy within the first crystal member. ### Claim 15 (depends on 14) The analytical system of claim 14 wherein the first crystal member has, in elevation, at least one curved circumferential focusing surface and at least one straight circumferential focusing surface for sequentially redirecting infrared energy within the first crystal member. ### Claim 16 (depends on 1) The analytical system of claim 1 wherein the first crystal member is formed by two symmetrical crystal hemi-cylindrical sections, which are coated with reflective material along their respective abutting and coupled surfaces cooperatively to form an infrared partition in the first crystal member. ### Claim 17 (depends on 1) The analytical system of claim 1 wherein said crystal assembly further comprises a first fiber optic bundle, in optical contact with said first crystal member, that acts as an energy waveguide to said first crystal member, and a second fiber optic member, in optical contact with said first crystal member, that collects encoded infrared energy from the first crystal member for return to a detector. ### Claim 18 (depends on 17) The analytical system of claim 17 wherein said first fiber optic bundle comprises a hemi-cylindrical array, and said second optic fiber bundle comprises a second hemi-cylindrical array. ### Claim 19 (depends on 1) The analytical system of claim 1 wherein the optically transmitting interface comprises two flat interface surfaces on the first crystal member and crystal disc in intimate optical contact with one another. ### Claim 20 (depends on 19) The analytical system of claim 19 wherein a tube is coupled to a probe tip body which houses the crystal assembly cooperatively to form a probe for the analytical system. ### Claim 21 (depends on 20) The analytical system of claim 20 wherein the diamond is positioned to at least partially extend beyond the probe tip body. ### Claim 22 An optical analytical system having a source of infrared energy, an infrared detector system, and a crystal assembly comprising a first crystal member having at least one circumferential focusing surface, and a crystal disc, said crystal assembly further comprising a first rolled sheet of silver chloride that acts as an energy waveguide to said first crystal member and a second rolled sheet of silver chloride that acts as an energy waveguide from said first crystal member, an optically transmitting interface between at least a portion of one surface of the first crystal member and at least a portion of an adjacent surface of the crystal disc, said crystal disc having a sample contacting surface which is opposite said optically transmitting interface, said source energy being redirected by at least one of said circumferential focusing surfaces, transmitted through said optical interface, and totally internally reflected in the second crystal at least once at the sample contacting surface, whereby said source energy obtains sample specific encoding; and said encoded source energy being transmitted from the crystal disc through the optically transmitting interface into said first crystal member and redirected by at least one of said circumferential focusing surfaces to the infrared detector system for sample analyzation. ### Claim 23 (depends on 22) The analytical system of claim 22 wherein the opposed end surfaces of said first and second rolled sheets are coated with reflective material and brought into or nearly into abutment with one another. ### Claim 24 Apparatus for optical analyzation of a sample with infrared energy, comprising a source of infrared energy, a detector and a crystal body having a circumferential focusing surface and one or more sample contacting surfaces wherein at least one of said sample contacting surfaces is curved to focus infrared energy focused by a first portion of the circumferential focusing surface back upon a second portion of said circumferential focusing surface so that infrared energy passing into and out of said crystal body is directed to and from diametrically opposed positions on said first and second portions of the circumferential focusing surface and the infrared energy is encoded with sample specific information at the sample contacting surface to permit analyzation of the sample at the detector. ### Claim 25 (depends on 24) The apparatus of claim 24 wherein said curved sample contacting surface comprises one end of a cylindrical extension from said crystal body. ### Claim 26 (depends on 24) The apparatus of claim 24, further comprising an energy waveguide associated with said crystal body and containing a transmissive medium through which infrared energy passes to and from said crystal body, the index of refraction of the crystal body being greater than the index of refraction for said transmissive medium. ### Claim 27 (depends on 24) The apparatus of claim 24 wherein said energy waveguide contains a transmissive medium through which infrared energy passes to and from said crystal body, the index of refraction of the crystal body being greater than the index of refraction for said transmissive medium. ### Claim 28 A crystal assembly in an optical system to analyze a sample with infrared energy comprising: a diamond disc having a sample contacting surface on one side of said disc and a first interface surface on another side of said disc opposite said sample contacting surface; a first crystal member having a second interface surface positioned to form an .optically transmitting interface with said first interface surface on said disc; said first crystal member having at least one circumferential focusing surface for redirecting infrared energy through said optically transmitting interface to permit the infrared energy to be internally reflected within said diamond disc to obtain sample specific encoding. ### Claim 29 (depends on 28) The crystal assembly of claim 28 wherein the material of the first crystal member is selected to have an index of refraction for infrared energy substantially similar to the index of refraction for infrared energy of the diamond disc. ### Claim 30 (depends on 29) The crystal assembly of claim 29 wherein the first crystal member has a transmission surface through which infrared energy enters and leaves the first crystal member, the infrared energy passing through a transmissive medium before entering and after leaving the crystal member, the crystal member having a higher index of refraction than the transmission medium to reduce infrared energy divergence angles in the first crystal member as compared to that present in the transmissive medium. ### Claim 31 (depends on 28) The crystal assembly of claim 28 wherein the optically transmitting interface comprises two substantially flat interface surfaces on said crystal member and diamond disc, in intimate optical contact with one another. ### Claim 32 (depends on 28) The crystal assembly of claim 28 wherein the optically transmitting interface comprises a third crystal member positioned between said first crystal member and diamond disc in intimate optically transmitting contact therewith. ### Claim 33 (depends on 32) The crystal assembly of claim 32 wherein the third crystal member is at least one layer deposited between the first crystal member and diamond disc. ### Claim 34 (depends on 33) The crystal assembly of claim 33 wherein the first and third crystal members have an index of fearaction substantially similar to the diamond disc and the third crystal member has one surface thereof adjacent the first crystal member at least partly reflectively coated to permit internal reflection of the infrared energy within the diamond disc and the third crystal member. ### Claim 35 (depends on 28) The crystal assembly of claim 28 wherein the first crystal member includes a substantially cylindrical portion between the transmission surface and the circumferential focusing surface. ### Claim 36 (depends on 28) The crystal assembly of claim 28 wherein a tube is coupled to a probe tip body which houses the crystal assembly cooperatively to form a probe for the optical system. ### Claim 37 (depends on 36) The crystal assembly of claim 36 wherein the diamond is positioned to at least partially extend beyond the probe tip body. ### Claim 38 (depends on 28) The crystal assembly of claim 28 wherein the first crystal member has a cavity symmetrically formed therein adjacent the optically transmitting interface and sized to let infrared energy in and out of the diamond disc member while permitting total internal reflection within the diamond disc between entry and exist. ### Claim 39 (depends on 28) The crystal assembly of claim 28 wherein the infrared energy passing within the diamond disc has a path length under going multiple internal reflections. ### Claim 40 (depends on 28) The crystal assembly of claim 28 wherein two circumferential focusing surfaces are diametrically opposed to one another and have symmetrical arcuate surface's in elevation. ### Claim 41 (depends on 28) The crystal assembly of claim 28 wherein the first crystal member has, in elevation, at least one curved circumferential focusing surface and at least one straight circumferential focusing surface for sequentially redirecting infrared energy within the first crystal member to the focal ring. ### Claim 42 A crystal assembly for a radiant energy analytical system, comprising: a first crystal member and a crystal disc, with an optically transmitting interface between said first crystal member and one face of said crystal disc, said crystal disc having a sample contacting surface on the opposite side of said disc from said interface; and said first crystal member having a circumferential focusing surface that redirects said radiant energy through said optically transmitting interface into said crystal disc so that said radiant energy is totally internally reflected within said crystal disc to obtain sample specific encoding. ### Claim 43 (depends on 42) The crystal assembly of claim 42 wherein said circumferential focusing surface comprises a portion of an outer surface of said first crystal member. ### Claim 44 (depends on 43) The crystal assembly of claim 43 wherein said circumferential focusing surface comprises frusto-conical section. ### Claim 45 (depends on 43) The crystal assembly of claim 43 wherein said circumferential focusing surface is curved in elevation. ### Claim 46 (depends on 42) The crystal assembly of claim 42 for an optical system to analyze a sample with infrared energy, wherein said crystal disc is a diamond and the material of said first crystal member is selected to an index of refraction for infrared energies substantially similar to the index of refraction for infrared energy of the diamond. ### Claim 47 A crystal assembly in an optical system to analyze a sample with energy comprising: a first crystal member having an optically transmitting interface a second crystal member; said second crystal member having a sample contacting surface a side of said second crystal member opposite said interface; the first crystal member having: a circumferential focusing surface for redirecting infarred energy through said optically transmitting interface; and a cavity adjacent the optically transmitting interface, said cavity being sized to permit said circumferential focusing surface to direct infrared energy through a first portion of said interface adjacent to said cavity so that said infrared energy is totally internally reflected within the second crystal member to obtain sample specific encoding and passes back through a second portion of the interface symmetrically opposed to said first portion of the interface. ### Claim 48 (depends on 47) The crystal assembly of claim 47 wherein said second crystal is a disc, said optically transmitting interface is on one side of said disc and the sample contacting surface is on the other side of said disc. ### Claim 49 (depends on 48) The crystal assembly of claim 48 wherein said optically transmitting interface comprises an annular ring around said cavity. ### Claim 50 (depends on 49) The crystal assembly of claim 49 wherein said cavity is symmetrically Formed about an optical center line of said first crystal member. ### Claim 51 (depends on 47) The crystal assembly of claim 47 wherein the second crystal member is a diamond and the material of the first crystal member is selected to have an index of refraction for infrared energy substantially similar to the index of refraction for infrared of the diamond. ### Claim 52 A crystal for optical analyzation of a sample comprising at least one crystal body having a sample contacting surface and at least one circumferential curved focusing surface adapted to direct infrared energy to said sample contacting surface, said sample contacting surface being curved to redirect said infrared energy back upon a circumferential curved focusing surface so that infrared energy passing into and out of said crystal body is directed in substantially opposite directions to and from diametrically opposed positions on said circumferential curved focusing surface or surfaces. ### Claim 53 An optical analytical system having a source of infrared energy, an infrared detector system, and an optical assembly comprising a first crystal member, one or more circumferential focusing surfaces, and a crystal disc, an optically transmitting interface between at least a portion of one surface of the first crystal member and at least a portion of an adjacent surface of the crystal disc, said crystal disc having a sample contacting surface which is opposite said optically transmitting interface, said source energy being redirected by one or more of said circumferential focusing surfaces, transmitted through said optical interface, and totally internally reflected in the second crystal at least once at the sample contacting surface, whereby said source energy obtains sample specific encoding; and said encoded source energy being transmitted from the crystal disc through the optically transmitting interface into said first crystal member and redirected by one or more of said circumferential focusing surfaces to the infrared detector system for sample analyzation. ### Claim 54 (depends on 53) The analytical system of claim 53 wherein two circumferential focusing surfaces are diametrically opposed to one another and have symmetrical arcuate surfaces in elevation. ### Claim 55 (depends on 53) The analytical system of claim 53 wherein the crystal disc is a diamond and the material of the first crystal member is selected to have an index of refraction for infrared energy substantially similar to the index of refraction for infrared energy of the diamond.