Slurry monitor coupling bulk size distribution and single particle detection

{
  "publication_number": "US10908059B2",
  "country": "US",
  "kind": "B2",
  "title": "Slurry monitor coupling bulk size distribution and single particle detection",
  "abstract": "Provided herein are particle detection systems, and related methods configured to characterize a liquid sample, comprising: a first probe configured to determine a first parameter set of a plurality of first particles in a liquid sample, the first particles characterized by a size characteristic selected from a first size range; wherein the first parameter set comprises a first size distribution and a first concentration; and a second probe configured to determine a second parameter set of one or more second particles in the liquid sample, the second particles being characterized by a size characteristic selected from a second size range; wherein the second parameter set comprises a second size distribution and a second concentration.",
  "claims": [
    "1. A particle detection system configured to characterize a liquid sample, said particle detection system comprising: a first probe configured to determine a first parameter set of a plurality of first particles in said liquid sample, said first particles being characterized by a size characteristic selected from a first size range; wherein said first parameter set comprises a first size distribution and a first concentration; and a second probe configured to determine a second parameter set of one or more second particles in said liquid sample, said second particles being characterized by a size characteristic selected from a second size range; wherein said second parameter set comprises a second size distribution and a second concentration; and wherein the first size range includes particles having sizes less than or equal to 200 nm and the second size range includes particles having sizes greater than 200 nm.",
    "2. The system of claim 1, wherein the first size range and the second size range overlap.",
    "3. The system of claim 1 further comprising a third probe, said third probe configured to determine a third parameter set of a plurality of third particles in said liquid sample, wherein said third particles are characterized by a size characteristic selected from a third size range.",
    "4. The system of claim 3, wherein said first size range, said second size range, and said third size range do not overlap with each other.",
    "5. The system of claim 3, wherein said third size range includes particles having sizes greater than or equal to 100 nm and less than or equal to 500 nm.",
    "6. The system of claim 5, wherein said first size range includes particles having sizes selected from the range of 2 nm to 100 nm and wherein said second size range includes particles having sizes greater than 500 nm.",
    "7. The system of claim 3, wherein each of said first, second, and third probes are independently selected from the group consisting of a light scattering probe, a light side scattering probe, a highly parallel light scattering probe, a near forward light scattering probe, a dynamic light scattering probe, a light diffraction probe, a laser diffraction probe, a laser scattering probe, an electroresistance probe, an electrostatic probe, a magnetic probe, a magnetoresistance probe, a pressure probe, flowrate probe, an acoustic probe, an ultrasonic probe, a pulsed Doppler acoustic probe, a structured laser beam probe, a light obscuration probe, an interferometry probe, an aerosolized condensation particle counter, a Coulter counter, an electrophoresis-based particle counter, a photoacoustic probe, a laser induced breakdown detection probe, an inductively coupled plasma mass spectrometry (ICP/MS) probe, and any combination thereof.",
    "8. The system of claim 1, wherein said first probe is configured to have a concentration detection range selected from the range of 10 3 particles/m L to 10 15 particles/m L.",
    "9. The system of claim 1, wherein said second probe is configured to have a concentration detection range selected from the range of 0.01 particle/mL to 10 5 particles/mL.",
    "10. The system of claim 1, wherein said first probe and said second probe are configured to determine said first and said second parameter sets simultaneously.",
    "11. The system of claim 1, wherein said system is configured to continuously monitor said first parameter set and said second parameter set.",
    "12. The system of claim 1, wherein said system further comprises a sample chamber configured to receive said liquid sample continuously or discretely.",
    "13. The system of claim 1, wherein a flow rate of said liquid sample in said system is changeable.",
    "14. The system of claim 1, wherein said first probe is configured to measure said first parameter set in a first liquid fraction of said liquid sample, said first liquid fraction having a volume less than a volume of said liquid sample; and wherein said second probe is configured to measure said second parameter set in a second liquid fraction of said liquid sample, said second liquid fraction having a volume less than a volume of said liquid sample.",
    "15. The system of claim 14, wherein a flow rate of said second liquid fraction is greater than a flow rate of said first liquid fraction.",
    "16. The system of claim 14, further comprising a first sample chamber having said first liquid fraction and a second sample chamber having said second liquid fraction.",
    "17. The system of claim 1, wherein said liquid sample is a slurry.",
    "18. The system of claim 17, wherein said liquid sample is a chemical mechanical planarization (CMP) slurry or a diluted slurry.",
    "19. The system of claim 18, wherein said liquid sample is a non-diluted chemical mechanical planarization (CMP) slurry.",
    "20. A method for characterizing a liquid sample, said method comprising steps of: feeding said liquid sample into a particle detection system comprising a first probe and a second probe; measuring a first parameter set in said liquid sample with said first probe; wherein said first parameter set comprises a first size distribution and a first concentration of a plurality of first particles, said first particles are characterized by a size characteristic selected from a first size range; measuring a second parameter set in said liquid sample with said second probe; wherein said second parameter set comprises a second size distribution and a second concentration of one or more second particles, said second particles are characterized by a size characteristic selected from a second size range; and wherein the first size range includes particles having sizes less than or equal to 200 nm and the second size range includes particles having sizes greater than 200 nm.",
    "21. The method of claim 20, wherein the particle detection system further comprises a third probe; wherein the method further comprises a step of measuring a third parameter set in said liquid sample via said third probe; and wherein said third parameter set comprises a third size distribution and a third concentration of a plurality of third particles, said third particles characterized by a size characteristic selected from a third size range.",
    "22. The method of claim 20, wherein said first probe is configure to have a concentration detection range selected from the range of 10 3 particles/mL to 10 15 particles/mL and said second probe is configured to have a concentration detection range selected from the range of 0.01 particle/mL to 10 5 particles/m L.",
    "23. The method of claim 20, wherein said step of feeding is performed continuously or discretely, and said steps of measuring are performed continuously or discretely.",
    "24. The method of claim 20, wherein said steps of measuring are performed simultaneously or are performed sequentially in any order.",
    "25. The method of claim 20, further comprising changing a flow rate of said liquid sample in a sample chamber of said system.",
    "26. The method of claim 20, wherein each of said steps of measuring is independently characterized by a measurement time selected from the range of 1 microsecond to 60 minutes.",
    "27. The method of claim 20, wherein said step of feeding comprises flushing a sample chamber of said system with a reference liquid sample or with a blank liquid sample.",
    "28. The method of claim 20, further comprising a step of splitting said liquid sample into a first liquid fraction and a second liquid fraction, wherein said step of measuring said first parameter set is performed on said first liquid fraction and said step of measuring said second parameter set is performed on said second liquid fraction.",
    "29. The method of claim 28, wherein said step of feeding comprises changing a flow rate of said first liquid fraction or said second liquid fraction independently of said second liquid fraction or said first liquid fraction, respectively.",
    "30. The method of claim 20, wherein said liquid sample is a slurry.",
    "31. The method of claim 20, wherein said plurality of first particles includes particles having sizes selected from the range of 1 nm to 200 nm and wherein said one or more second particles includes particles having sizes greater than 200 nm and less than 100 μm.",
    "32. A particle detection system configured to characterize a liquid sample, said particle detection system comprising: a first probe configured to determine a first parameter set of a plurality of first particles in said liquid sample, said first particles being characterized by a size characteristic selected from a first size range; wherein said first parameter set comprises a first size distribution and a first concentration; and a second probe configured to determine a second parameter set of one or more second particles in said liquid sample, said second particles being characterized by a size characteristic selected from a second size range; wherein said second parameter set comprises a second size distribution and a second concentration; wherein said first probe is configured to measure said first parameter set in a first liquid fraction of said liquid sample, said first liquid fraction having a volume less than a volume of said liquid sample; and wherein said second probe is configured to measure said second parameter set in a second liquid fraction of said liquid sample, said second liquid fraction having a volume less than a volume of said liquid sample; and wherein a flow rate of said second liquid fraction is greater than a flow rate of said first liquid fraction.",
    "33. The system of claim 1, wherein said first probe and said second probe are different.",
    "34. The system of claim 1, wherein the first probe is physically separated from said second probe.",
    "35. The system of claim 1, wherein the first probe is a different probe type than said second probe.",
    "36. The system of claim 1, wherein the first probe is selected from the group consisting of: a light scattering probe, an electronic or resistivity based probe; an electrostatic based probe; a structured laser beam particle sensing probe; an interferometric characterization based probe; an ultrasonic probe, an acoustic probe; an aerosolized condensation particle counter (CPC); a dynamic light scattering (DLS) based probe; a photoacoustic detection based probe; a laser induced breakdown detection based probe; an inductively coupled plasma mass spectrometry (ICP/MS) based probe and any combinations of these.",
    "37. The system of claim 1, wherein the first probe is a light scattering probe, an ultrasonic probe, a dark beam probe or a dynamic light scattering probe.",
    "38. The system of claim 1, wherein the second probe is selected from the group consisting of: a light obscuration probe; a near forward light scattering probe; a structured laser beam particle sensing probe; an ultrasonic probe, an acoustic probe, an interferometric characterization based probe; an electronic or resistivity based probe; an electrostatic based probe; a photoacoustic detection based probe; a laser induced breakdown detection based probe; an inductively coupled plasma mass spectrometry (ICP/MS) based probe and any combinations of these.",
    "39. The system of claim 1, wherein the second probe is a light scattering probe, an ultrasonic probe, a dynamic light scattering probe or a light obscuration probe.",
    "40. The system of claim 1, wherein: i. the first probe is an ultrasonic probe and the second probe is a light scattering probe; or ii. the first probe is a dark beam probe and the second probe is a light obscuration probe; or iii. the first probe is a dynamic light scattering probe and the second probe is a light obscuration probe."
  ],
  "description_excerpt": "Chemical Mechanical Planarization (CMP) is a process by which chemical and mechanical forces are combined to polish a surface. CMP plays an important role in semiconductor-device industries, for example. Prior to deposition or fabrication of complex and precisely controlled micro- and nano-scale semiconductor components, a working surface (e.g., a 300 mm wafer) should meet stringent tolerances for flatness and smoothness to maximize quality and reproducibility. The polishing is achieved, at least in part, via a CMP slurry, which includes a large concentration (e.g., 10 7 to 10 15 particles/mL) of small abrasive particulates suspended and/or dispersed in a pH controlled chemical solution.\n\nThe tight tolerances for quality and reproducibility in turn require precise and accurate control of all variables, including the CMP slurry itself, during the planarization. One problematic issue is variation in the concentration and distribution of the abrasive particulates, which influences the rate of planarization. An increase in the number of large particulates can cause scratch and dig defects on the surface of the wafer. As a result, it is important to monitor the size distribution and concentration of the particulates in the CMP slurry.\n\nConventional technologies for determining the particulate size distribution and concentration in slurries include traditional optical particle counters that may require ex-situ processing of the liquid sample, such as dilution, prior to a measurement.",
  "cpc": [
    "G01N 15/0211",
    "G01N 15/02",
    "G01N 15/0266",
    "G01N 15/06",
    "G01N 2015/0053",
    "G01N 2015/0222",
    "G01N 2015/0283"
  ],
  "ipc": [
    "G01N 15/02",
    "G01N 15/06"
  ],
  "assignees": [
    "Particle Measuring Systems Inc"
  ],
  "inventors": [
    "Brian A. Knollenberg",
    "Daniel Rodier"
  ],
  "filing_date": "2019-11-13",
  "publication_date": "2021-02-02",
  "grant_date": "2021-02-02",
  "priority_date": "2018-11-16",
  "application_number": "US-201916682314-A",
  "family_id": "70727463",
  "cited_by_count": 20,
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