KR20110043621A

KR20110043621A - System and methods for in-line monitoring of particles in opaque flows and selective object manipulation in multi-component flow

Info

Publication number: KR20110043621A
Application number: KR1020117001938A
Authority: KR
Inventors: 래쉬드 마블리브; 앤드류 마블리브
Original assignee: 밴티지 테크놀로지 코퍼레이션
Priority date: 2008-07-08
Filing date: 2009-07-08
Publication date: 2011-04-27
Also published as: JP2011527751A; WO2010004516A1

Abstract

Systems and methods are disclosed for monitoring particles, in particular for in-line particle monitoring and selective object manipulation with multicomponent flow. One example of a system may include a detection system for monitoring components such as particles in an opaque flow carrier. The example system defines a flowable sample that is opaque for at least the first wavelength range of the light wave and compresses the flowable sample in the first direction, while the second is parallel to and perpendicular to the flow direction of the flowable sample. Direction, while extending the sample in a third direction orthogonal to the first and second directions. Once the sample is compressed in the first direction, the sample becomes transparent for at least one wavelength in the first wavelength range that enables optical means for particle detection. The system may also include a device such as a valve or actuator for manipulating the detected component from other components in the flow carrier. A controller or other processor may receive and process the detected component data and may distinguish the component of interest from the remaining flowable sample. Once the component is recognized, the controller operates in synchronization with the flow manipulation device and detection system to manipulate the detected component from the flow carrier.

Description

System and methods for in-line monitoring of particles in opaque flows and selective object manipulation in multi-component flow}

The objects disclosed herein generally filter or separate multiple components in flow carriers, such as liquids or gases, as well as techniques for detecting and characterizing particles in concentrated liquid systems such as slurries, emulsions and suspensions. And the field of manipulation, including. More particularly, the present invention relates to the field of operations, including filtering or separating multiple components in flow carriers at industrial flow rates.

Liquid systems with high particulate concentrations are widely used in industry. Examples of such systems are slurries used in the chemical mechanical planarization (CMP) process in the semiconductor industry and emulsions used in the pharmaceutical industry.

Optical methods for detection and characterization have been used to monitor particle parameters in gas and liquid media. United States Patent No. 6,710,874 to Mavliev discloses an apparatus and method for the optical characterization of particles in high concentration systems, the entirety of which is incorporated herein by reference.

Flow-through separators are known, such as filters or other types of mechanical separators. Separation efficiency depends on differences in the characteristics of the components to be separated. In some cases, one of the components to be separated may differ by one or more measurable variables and may have a lower concentration in the flow carrier compared to another component. One such case is the filtration of abrasive slurries from oversized particles. Typical polishing slurries are composed of particle ensembles of high concentration (10 ^ 12 / cc) and the desired size (typically 50-500 nm): These particles are required to carry out the polishing process. In certain situations even larger (large) particles of size 1 to 100 μm may be present in the slurry due to aggregation, malfunction, contamination or other reasons. The presence of large particles causes substrate scratches during polishing, resulting in "killer defects" and reduced production yields. One well adopted solution for removing large particles is filtration. In the context of slurry or other emulsion filtration, other different (useful) components accumulate in the filtration device, resulting in secondary large particle formation, requiring frequent maintenance and replacement of the filtration device.

A method for separating particles is disclosed in US Pat. No. 7,294,249 to Gawad. This method requires the influence and separation of particles by dielectrophoresis, a measurement channel region for characterizing the particles, and a classification region for particle classification identified in the measurement channel region by dielectric migration. The classification includes a switching element, which allows active flow of particles into two or more subchannels corresponding to criteria registered in the measurement channel region. The method allows for the rapid and accurate classification of particles, especially biological cells in suspension, while in particular it cannot be carried out to separate particles in multicomponent fluids such as slurries at industrial flow rates.

The particle separation methods disclosed in U.S. Pat.Nos. 7,318,902 and 7,472,794 to Okay, which are incorporated herein by reference, provide laminar fluid flow in microfluidic flow devices with flow impairments. I use it. External means are used to adjust the flow rate, which makes the invention inapplicable to the patent field. Flow obstruction is not particularly desirable for high particle content flow operations such as slurries and emulsions. US Pat. No. 7,428,971 to Hirano et al. And US Pat. No. 7,366,377 to Gettin et al. And US Pat. No. 7,068,874 to Wang et al. Relate to particle manipulation in flow using optical means. These methods may be useful in the field of cell sorting, but are not useful for manipulating objects, especially at industrial flow rates, in opaque fluids with high particle content (such as slurries and emulsions).

Methods and apparatus for filtration or particle separation from multi-component flows, including in-line monitoring of particles in opaque fluids as well as flows with components (particles) to be preserved and flows with high particle content such as slurries and emulsions, are required It is becoming. Preference is also given to methods that do not depend on flow variables such as optical transparency, viscosity, flow rate or laminarity, and methods and apparatus that can operate in industrial conditions.

summary

The particle monitoring system is located in a cuvette and a cuvette configured to define an opaque flowable sample for at least a first wavelength range of light waves and compresses the flowable sample in a first direction, while compressing the sample in parallel with the flow direction A transparent flow compression element adapted to extend in a second direction orthogonal to the first and second directions while controlling in a second direction orthogonal to the first direction, the sample being compressed in the first direction Is transparent for at least one wavelength in the wavelength range of the light wave.

Particle monitoring methods define an opaque flowable sample at least for a first wavelength range of light waves, measure the transparency of the flowable sample, compress the flowable sample in the first direction, while compressing the sample in the flow direction and parallel to the first direction. Controlling in a second direction orthogonal to and extending the sample in a first direction and a third direction orthogonal to the second direction, and identifying the characteristics of the particles contained in the compressed sample, the sample being in the first direction When it is compressed to be transparent to at least one wavelength in the wavelength range of the light wave.

The system for selective object manipulation in a multicomponent flow includes means for detecting and mapping components in the flow carrier, means for manipulating components in the flow carrier, and means for controlling the manipulation of the detected components; The component manipulation means is adapted to remove or separate the detection component from other components in the flow carrier and the control means is adapted to synchronize the manipulation means with the detection means.

In one embodiment, the detection and mapping means is a cuvette configured to define an opaque fluidic sample that is opaque for at least the first wavelength range of the light wave, located in the cuvette and compressing the fluidic sample in the first direction, while compressing the sample in the flow direction. Using at least one wavelength and a transparent flow compression element adapted to extend in a third direction that is parallel to and perpendicular to the first direction and is orthogonal to the first and second directions. A monitor for monitoring the flowable sample, wherein when the sample is compressed in the first direction, the sample is transparent to at least one wavelength in the wavelength range of the light wave.

Selective object manipulation methods in multicomponent flows include manipulating the detected components in the flow carrier, including detecting and mapping components in the flow carrier and removing or separating them from another component, wherein the operating steps of the detected components It is synchronized with the detection and mapping phase.

In one embodiment, the detecting and mapping step defines an opaque fluid sample for at least the first wavelength range of the light wave, measures the transparency of the fluid sample, compresses the fluid sample in the first direction while compressing the sample into the fluid sample. Particles contained in the compressed sample that confine in a second direction that is parallel to the flow direction of and perpendicular to the first direction and extends in the third direction orthogonal to the first and second directions And identifying a feature of the sample, wherein the sample is transparent to at least one wavelength of the first range of wavelengths when the sample is compressed in the first direction.

As will be realized, different embodiments are possible and the details described herein may be varied in various respects without departing from the scope of the claims. Accordingly, the drawings and detailed description are by way of example only and are not meant to be limiting. Like reference numerals are used to refer to like elements.
1 illustrates an exemplary embodiment of a system with flow separation.
2 illustrates an exemplary embodiment of a system for component manipulation.
3 shows an exemplary embodiment of a system with coordinate conversion.
4 illustrates an example embodiment for selective particle removal in a chemical mechanical polishing (CMP) process.
FIG. 5 shows an example of time delay and diffusion factors in one embodiment of a system in which selective object manipulation is performed in a multicomponent flow, such as a slurry used in a CMP process.
6A shows an overview of the flow of one embodiment of a particle monitoring system;
6B shows an overview of systems and variables for numerical evaluation of a particle monitoring system in one embodiment.
6C shows an overview of an exemplary cuvette according to the first embodiment (two optical elements with Y axis extending and curvature Z);
6D shows an overview of an exemplary cuvette in accordance with a second embodiment (optical element having a flow passage extending in the Y axis and defined in the Z axis).
7A shows an overview of an exemplary particle monitoring system according to the first embodiment.
7B shows a more detailed cross-sectional view of an exemplary particle monitoring system according to the first embodiment.
7C and 7D show cross-sectional views of an exemplary particle monitoring system according to a first embodiment that incorporates ambient flow.
8A shows an overview of an exemplary particle monitoring system according to a second embodiment.
8B shows a more detailed cross-sectional view of an exemplary particle monitoring system according to the second embodiment.
9A shows an overview of an exemplary particle monitoring system according to a third embodiment.
9B shows a more detailed cross-sectional view of an exemplary particle monitoring system according to the third embodiment.
9C shows a more detailed overview of cuvettes in an exemplary particle monitoring system according to the third embodiment.
10 shows an overview of an exemplary optical cuvette in accordance with a fourth embodiment.
11 shows an overview of an exemplary optical cuvette according to the fifth embodiment.
12A, 12B, 12C and 12D show an overview of an exemplary particle monitoring system according to a sixth embodiment using cylindrical double-sided concave lenses as waveguides.

details

1 shows a system 1 comprising means for detection and mapping 2 for localization of a component (“component B”) in a flow carrier, such as a liquid or gas. In one embodiment, the means for detection and mapping is an optical system for in situ and / or in-line or off-line monitoring of particles in a flowable sample such as a slurry, emulsion or suspension, such as the system disclosed in FIGS. Can be.

In one embodiment, the system 1 may comprise a flow separation means 3 such as a mechanical device (eg a valve or actuator), an electrical process (eg a dielectric transfer), a magnetic field or a chemical process. Flow separation means may be used to separate the detected component from other components in the flow carrier.

In one embodiment, the system 1 may be a mechanical device (eg an actuator), an electromechanical device (eg an ultrasonic or megasonic actuator), an electrical process (eg an electrical discharge), an electromagnetic field (eg a laser or X-rays), or flow affecting means such as chemical processes. Flow affecting means can be used to change the detection component from other components in the flow carrier by removing or selectively changing the desired properties.

In one embodiment, the system 1 can comprise control means 4 such that the flow manipulation means for excluding, diverting or removing particles can be synchronized with the detection means. The control means 4 may comprise, for example, a computer, a controller or other processor known in the art. The control means can, for example, receive and process the detected image data and distinguish the components of interest from the remaining suspension. Once the particles have been recognized, the control means 4 can act to cause the flow manipulation means 3 to separate or remove component B 5 from the same flow rate as the suspension comprising component B 5 and component A. Downstream of the flow manipulation means 3 it does not have component B 6.

In the exemplary system 1, input may be received from the detection means 2 monitoring the target area for the component or particle of interest. The target area can be monitored to detect known contributions (or absence thereof) that can be used to distinguish particles from the remaining suspension. For example, a particle monitoring system can be used to capture an image stream that can be used to identify particles by their particular contributions. Alternatively, signatures, fingerprints or indicators, or combinations thereof, such as fluorescent signatures, light scattering signatures, optical fingerprints, X-ray diffraction signatures or refractive indexes, or the like, can be used to distinguish particles from the remaining suspension. The surface charge of a particle can be used to distinguish the particle by observing the particle's response to an applied electric or magnetic field.

2 shows another exemplary embodiment in which the flow separating means 3 can be replaced or supplemented by the component operating means 7. Examples of component manipulation means may include, for example, a laser or other radiation light source to destroy dangerous cells while leaving other components there through. Other examples of component manipulation means may include light sources capable of producing other destructive effects, such as radiation sources or shock waves that disrupt the aggregation of particles.

3 illustrates an example method using coordinate transformation of detected components. Detection can be performed by an example particle monitoring system as illustrated in FIGS. 6-12 and the accompanying detailed description. The sample flow is thinner using the same technique for component B detection and subsequent flow separation or manipulation (minimum thickness flow can be allowed for easier detection and mapping and easier separation or manipulation). Can be molded into threads.

Exemplary techniques for shaping the flow include the use of two prisms with opposing tips, two cylindrical lenses and two optical blocks that overlap at least on the Z axis as shown in FIG. 6, for example. can do. In an embodiment of two prisms having opposing ends as shown in FIG. 6B, the prism compresses the flowable sample in the first direction X, while the sample is parallel to the flow direction and orthogonal to the first direction. While limiting to the second direction Z, the sample may be extended in a third direction Y that is orthogonal to the first and second directions. Once the sample is compressed in the first direction, the sample may be transparent to light sources of at least one wavelength.

The coordinate shift factor may be established between the detection and manipulation system y ^ y 'using the detection system and the second detection system instead of the manipulation system. Similarly, the time delay factor t ⇒ t 'can be determined between the two systems. After detecting component B on the detection system, the coordinates (y, t) of component B 'can be determined. The coordinates (y ', t') of component B 'can be determined by the second detection system. The coordinates of the plurality of components B and B 'may be converted from the operating system transfer function T link (y, t) to (y', t '). The detection of the object by the detection system at coordinate y ₁ and time t ₁ , using the known transfer function T, generalizes coordinate y ₁ ′, at which point a suitable action is applied at a predetermined time t ′ ₁ .

4 shows a non-limiting exemplary embodiment for selective particle removal in a chemical mechanical polishing (CMP) system 12. CMP can be used, for example, in semiconductor wafer fabrication. The CMP may use abrasive and corrosive chemical slurry 16 (usually colloid) in combination with a polishing pad and a retaining ring, typically larger in diameter than the semiconductor wafer 9. CMP process slurries typically consist of SiO ₂ or Al ₂ O ₃ particles suspended in an acid or base solution at a concentration of 4 to 18% solids by weight. CMP slurries can include particles having a wide range of particle sizes, such as diameters from 0.03 microns to 1.0 microns or more. In some cases, the slurry may contain larger size particles due to contamination or agglomeration of the slurry particles. Since a correlation has been identified between the number of large particles and the number of scratch defects on the polished wafer, it is important to control these particles. Due to the small number of large particles and the substantially opaque nature of the slurries, it is difficult to identify the particle size distribution in these slurries.

Particles with dimensions exceeding specified values for a particular application are similar to sandpaper with excessively large grit and are disadvantageous by leaving marks or scratches on the surface to be flattened. Therefore, a quality control process is essential to eliminate the use of slurries with excessively large particles.

The pad and wafer 9 can be compressed together by the dynamic polishing head 8 and held in place by the plastic retaining ring. The dynamic polishing head 8 rotates with different axes of rotation (ie not concentric circles). This tends to remove material and eliminate irregular topography, making the wafer flat or planar. This may be necessary to set up the wafer to form additional circuit elements.

In the non-limiting embodiment shown in FIG. 4, the slurry delivery line 15 of the CMP polishing system includes, as one embodiment, a particle detection system 2 and a three-way valve, which is the particle detection system shown in FIG. 7B. Having a particle separation system 3. In the embodiment of FIG. 4, the detection and mapping can be performed using one or more embodiments as shown in FIGS. 6-12 and described in the accompanying detailed description.

The system for in-line monitoring of particles in an opaque flow, which is one of the embodiments shown in FIGS. 6-12, is preferably a slurry delivery line of the CMP polishing system 12 just in front of a few meters of the slurry distribution nozzle 13. Connected to (11). The inline monitoring system 2 has a predetermined detection limit and means for generating an ALARM signal upon detection of particles having a size exceeding a predetermined limit. The ALARM signal can be an electrical signal with an audible and visible indication. ALARM electrical signals can be used by the main control PC or other device. In one embodiment, the ALARM signal may activate a three-way valve 3 located further downstream to remove particles having a size larger than a predetermined size from the slurry and supply it to the waste container 14. The slurry reaching the wafer does not have these large particles that can cause damage to the wafer. The activation of the valve 3 will be delayed for a predetermined time offset after the detection of particles having a size larger than the predetermined size by the detection means 2. In one embodiment, the predetermined time offset or time delay depends on additional process conditions such as, for example, the flow rate of the slurry through the feed line 11. For higher flow rates, the time offset is shorter because the particles take less time to transfer from the detection means 2 to the valve 3 via the supply line 11. Such conditions can cause particle detection and manipulation to occur during the polishing process when it is essential to eliminate scratches that cause large particles. Particle detection and manipulation can be omitted, for example, during an idle cycle.

In one embodiment, the three-way valve 3 is integrated in a slurry line close to the slurry delivery nozzle 13. Three-way valves typically have an inlet and two outlets-"ON" at any time (1) and "OFF" at any time (2). Slurry line 15 is connected to the inlet of valve 3 and the “always on” outlet of the valve connected to the slurry line to the polishing platen. The "always OFF" outlet of the valve is connected to the waste container 14.

In one embodiment, the three-way valve 3 is a model that is activated by a pneumatic three-way valve of Swagelok's small body type, for example a pneumatic manifold controlled by the main treatment PC. It may be number NXT-DRP41YFCFCFC-S. In this case the particle detection system generates an ALARM signal for the main processing PC, processes the signal, identifies the need for action and activates the 3-way valve for a predetermined duration. Valve activation will lead to the conversion of slurry flow into waste containers, which will be further analyzed to find the cause of the problem if necessary.

In one embodiment, as a test mode, a second in-line monitor (not shown) may be temporarily connected to the three-way valve and the time delay may be approximately ˜1 for a 3 m line at typical flow rates (example values). Minutes). To determine the time delay value, the slurry flow will be monitored for a specific time period and a correlation between these two system readings will be made. The reading of the first particle detection system will correlate with the reading of the second system with the necessary time delay for particles transporting from the first detection point to the second point. Due to flow turbulence and irregularities, the time delay can vary at certain limits that can be introduced as the diffusion factor S. An example of an exercise for determining the time delay and time spreading factor is shown in FIG. 5.

As shown in FIG. 5, a "packet" of particles, such as changing the particle concentration from zero to some specific value for a fixed time period, can be used to determine the time delay. The time delay and “packet” diffusion factor S (due to turbulence and flow nonuniformity) can be determined by comparing the signals obtained from the two in-line monitors.

In the operating mode, after particle detection by the in-line monitor 2, the control unit 4, for example a PC, generates an event alarm to determine the time delay factor t => t 'and And activation of the three-way valve 3 for a time exceeding the "packet" diffusion factor T at a predetermined time t ', affecting a portion of the slurry with the detected components, such as a polishing process and causing wafer scratches. Large particles are delivered to the waste container 14.

As described, exemplary embodiments examine the flow carriers containing the components to be separated, identify the locations of the specific components to be separated in the flow, and selectively remove the flow fractions having the components to be separated, while removing the components to be separated. For the portion of the flow that does not contain it is concerned with minimizing the impact. In an exemplary embodiment, particle conversion or removal can be synchronized with particle detection. Separated components can be concentrated for further analysis or use. Exemplary embodiments can separate live and dead cells that can be distinguished by components that cannot be separated by filtration, such as fluorescence, but that cannot be separated by filtration.

6A, 6B, 6C and 6D are provided as an overview for introduction. In-line particle detection systems can be used to continuously monitor the flow.

In another embodiment, one particle detection system of the embodiment shown in FIGS. 6-12 may be used in an optional object manipulation system such as the system of one of FIGS. 1-4, for example the CMP system shown in FIG. 4. have.

In the example particle monitoring system shown in FIG. 6A, sample flows (indicated by dashed lines) with inclusions or particles to be detected may be converging or diverging into parts. Arrows indicate the light penetration depth, which depends on the optical properties of the sample, such as sample haze. The aim is to provide light penetration down to the narrowest part of the flow 1. In this case, optical techniques such as dynamic light scattering, quenching, light scattering, or a combination of these techniques can be used to detect and characterize impurities (particles, inclusions) present in the flow.

6B shows an overview of an exemplary particle monitoring system and variables for numerical evaluation to be discussed later.

There may be several basic groups that can be classified as example designs for particle monitoring systems. 6C shows an overview of an exemplary cuvette according to the first group. Here, there may be two optical elements with the Y axis extending and the Z axis curvature. An example includes two prisms with opposing tips, two cylindrical lenses and two optical blocks with minimal overlap on the Z axis. 6D shows an overview of an exemplary cuvette according to the second group. There may be optical elements with a flow passage extending in the Y axis and defined in the Z axis. These designs may include, for example, monolithic waveguide structures with slits for flow defined in the Z direction. Other design groups may include combinations of the above features. For example, one optical element may have a substantial curvature in the Z direction and another element may comprise a flat portion.

The transparency of the sample flow can be arranged in the form of a "sheet" flow, which can be relatively thin in the first (X) and second (Z) orthogonal dimensions and long in the third (Y) orthogonal dimensions. Exemplary optimal sample thicknesses can be determined using, for example, two criteria. The first criterion may be based on the absence of significant majority scattering of light by the sample or the presence of relatively high sample transparency, which may determine the thickness at the first dimension.

The second criterion may be based on the desired pressure drop of the optical cuvette at the desired flow rate. The pressure drop inside the optical cuvette can be an important factor for method availability in the industry. There may be an acceptable range of pressure drops that can be introduced into the flow lanes by a device (such as an in-line monitoring device). This range may vary depending on the application and also depends on process parameters. The pressure drop inside the cuvette can be the inverse of the flow thickness in the first and third dimensions and can determine the cross section of the cuvette. Since the flow thickness in the first dimension X can be determined by the optical transparency criteria and does not change freely, the flow width in the third dimension Y can be used to maintain the pressure drop at the desired level. The pressure drop can be directly proportional to the flow dimension in the second direction Z and this can be used to influence the pressure drop in the cuvette in a desired manner.

As an example, a sample fluid flow can be established having a thickness in the range of about X = 5-500 μm, Z = 0.1-5 mm and a width of Y = 5-25 mm in the third dimension. The split angle at the output of the cuvette can affect the pressure drop in the cuvette at a given flow rate and can be selected accordingly. Another criterion for selecting the classification angle may be its influence on the flow structure. For example, high fractionation angles (orthogonal angles in the extreme, ie slits in flat materials) will best produce turbulent movement in the flow. If turbulence is undesirable, it can be prevented by selecting the appropriate fractionation angle of the cuvette.

In an exemplary embodiment, laser quenching and multiple light scattering by the particles can be ignored for the "sheet" of a typical slurry. At the same time, the slurry flow may not require dilution, so the size distribution of particles in the slurry can have minimal distortion.

Numerical evaluation

In one embodiment, referring to FIG. 6B, the flow variable at the measurement point is width Y, thickness X, flow rate Q. The laser beam of Lp (not shown) power has a width Y and a thickness Z. The measuring area Z * Y is projected by a optical system of magnification k to a camera type sensor of Py * Pz pixels (pixel sizes are z _p and y _p ) and signal accumulation time t _c . Optical magnification is chosen for the overall flow observation:

Y = k ^* Py ^* y _p .

The particle velocity at the measurement area is V = Q / (X * Y). The signal registration time is t = Z / V or t = z _p / k / V, which is smaller. Assuming t <t _c (which is reasonable in most cases), the signal amplitude is:

S = Lp ^* F (d) ^* X / Q ^* (z _p / k / Z)

Where F (d) is the light scattering function for particles of size d. For particles in the scattering medium, the detection limit is determined by the signal / noise ratio rather than by the signal value itself. The signal / noise ratio can be influenced by two variables-the volume of the scattering medium illuminating a single pixel and the ratio of signal and noise accumulation time. Multiplying these two factors by the signal / noise ratio gives:

SN = Py / t _c / Q ^* (F (d) / F (d _m ))

Wherein d _m is the median particle size in the scattering medium. SN does not necessarily depend on flow space variables. This allows for a variety of flow thicknesses X to achieve flow transparency without affecting the signal / noise ratio.

Multiple light scattering can be neglected for the underlying sample optical thickness (ie transmittance> exp (-l)). The acceptable sample optical thickness range can be extended up to five times or more at small signal acquisition angles. In this case, the correlation of Beer-Lambert light scattering may be modified.

The parameters of the sensor (eg detection camera) can be as important as the overall flow rate. Some exemplary calculation results for two cameras (1024 and 2048 pixels) and two flow rates are shown in Table 1 below. The detectable particle size d _p is calculated on the assumption that it is a Raleigh scattering and signal to noise ratio 1 (the slurry variables are d = 100 nm and N = 1e12 1 / cc).

From Table 1 it can be seen from the simple assumption that individual particles as small as 600-1000 nm should be able to be detected. It should be mentioned that the detectable particle size can be reduced by operating the S / N ratio below 1 if necessary, which can be technically easy.

7A, 7B, 7C and 7D show an exemplary particle monitoring system 200 according to the first embodiment. In this embodiment, the particle monitoring system 200 includes a cuvette 210, eg, a transparent optical flow cell, that is adapted to define a flowable sample. The flowable sample may be opaque over at least the first wavelength range of the light wave. A transparent flow compression element 220, such as a prism, is located in the cuvette 210 and compresses the flowable sample in the first (X) direction, while the second direction Z is parallel to the flow direction and orthogonal to the first direction. The sample is controlled while extending the sample in the third direction Y perpendicular to the first and second directions. Once the sample is compressed in the first direction, the sample may be transparent to at least one of the wavelengths in the wavelength range of the light wave.

In one embodiment, exemplary dimensions for the X, Z, and Y directions are about 50 μm to 3 mm in the first (X) direction, about 10 μm to 3 mm in the second (Z) direction and 3 (Y) dimensions are from about 5 mm to 25 mm.

In one embodiment, an optical flow cell such as cuvette 210 may be used to form a concentrated flow of sample fluid. The cuvette 210 may include a flow confluence portion, a measurement portion, a sample introduction portion, and a sample discharge portion. The width of the flow channel in the measuring portion of the cuvette 210 can be narrow at the first dimension (eg 0.1 mm ± 10% or less or greater) and wide at the third orthogonal dimension (eg about 10 mm ± 10% or less).

The effective flow dimension in the second orthogonal direction can be measured by the curvature of the flow focusing element and can, for example, range from 10 μm to 3 mm. The flow channel variable may be substantially constant along the entire length of the measurement portion of cuvette 210 (eg, ± 10% flow channel width in any direction). The measurement portion of the cuvette 210 may be optically transparent and may be used for characterizing sample transparency and for optical characterization of particles in concentrated sample fluid.

In one embodiment, as shown in FIGS. 7C and 7D, the sample fluid flow is in operative communication (eg, at least partially) with a clean (ie, relatively particle free) clear liquid (eg, water) or other suitable liquid. Surrounded by). This can be achieved, for example, by introducing and removing the clear transparent liquid through the surrounding flow inlet and outlet. This method can be used to avoid contamination of the optical component or as another method for controlling sample flow thickness and transparency. Exemplary optical cuvettes with symmetrical peripheral flow inlets are shown in FIGS. 7C and 7D. The main sample flow is introduced through the flow inlet and discharged through the sensing area defined by the tip of prism 220. A peripheral flow of clean liquid miscible with the sample liquid variable forms a boundary layer on the prism 220 surface to prevent particle deposition on the optical surface. The ambient flow can be chosen to be miscible with the sample flow and the flow rate can be minimal so as not to affect the sample flow characteristics.

In one embodiment, an exemplary method of compressing a flow is shown in FIG. 7A as two optical elements (eg, prisms 220) having a gap formed between the tips that compress the sample to make the sample transparent to at least one wavelength of light waves. 7b, 7c and 7d. The tip of prism 220 may be designed to provide the required optical quality. As a flow forming optical element the prism can satisfy the above mentioned parameters: extension by the Y axis and short distance by the axis Z. The optical signal can be collected through the flat surface of the prism opposite the sensing volume forming tip. The prism angle from the tip to the flat surface can be chosen differently depending on the requirements of the signal detection system-the angle can be small for light transmission schemes, and a larger angle is used for scattered light collection for light scattering schemes. Can be.

Symmetric or asymmetric prisms may be used depending on the requirements for the confluence and fractionation angle of the flow. One skilled in the art, in addition to one or all of the embodiments described above, as well as variations thereof, the cuvette would use two optical elements, such as two isostriction (or other) prisms, compressing the sample to at least one dimension to compress the sample to a predetermined wavelength. It is possible to create a flow cell to be transparent to the light waves of.

The system may also include a method for identifying the characteristics of the individual particles contained in the compressed sample. In one embodiment, the identification device is shown in FIG. 7B, such as an optical camera or detector 230 (eg, a CCD camera, CMOS, photodiode or other optical sensing device) in optical communication with the cuvette 210. An associated light source 240, such as a laser generating light beam 250, may be in optical communication with the cuvette 210.

Sample transparency can be measured by quenching and the sample fluid thickness in the flat portion of the cuvette 210 can be adjusted to obtain a certain transparency value or sensing volume value. Conventional light scattering and / or quenching techniques can be used to measure parameters of a single particle having a diameter above the detection limit. Charge-coupled devices (CCDs) or CMOS detectors / cameras 230, together with appropriate frame-capture electronics and data-handling software, allow the effect of background scattering on the quantitative detection of signals generated by individual particles through optical sensing volumes. It can be used to suppress.

7C and 7D show further details of an exemplary cuvette 210 according to the first embodiment. The cuvette 210 may include a body assembly for a component, a prism 220 attached to the actuator 260, and two symmetrical holders. Suitable sealing at the holder-prism interface may be provided by an O-ring (eg, Kalrez or Chemrez material). To achieve a change in channel thickness, the cuvette 210 may be adapted to use two symmetrical optical components, such as a prism 220 separated by an elastic spacer formed of, for example, an O-ring cord or other elastic material. have.

Prism 220 (eg, sapphire or glass coated with diamond-like carbon) is attached to actuator 260 to allow displacement of the prism to adjust the sensing area width. Externally controlled pressure may be caused by shrinkage in, for example, screws, hydraulic or pneumatic actuators, electromagnetic actuators or spacers using other ways to control the displacement to varying degrees depending on the applied pressure and the Young's modulus of elasticity to the spacer. It can be applied on these two opposing parts. This may allow control of sample transparency and the concentrated fluid sample thickness may have a known relationship (eg proportional to) the flow channel thickness. Actuator 260 may provide high frequency (ultrasound or megasonic) vibrations of prism 220 to reduce possible particle deposition on optical components.

This exemplary embodiment allows measurement of sample transparency as a function of sample thickness in a single experiment. These measurements can allow the measurement of particle size variables in the sample fluid using the integrated scattering method. At the same time, the maximum particle variable can be determined using a single particle approach. The combination of these two different approaches (ie integration and differential) may allow for improvements in the accuracy and reliability of the measurements.

As a second embodiment, as shown in FIGS. 8A and 8B, sample fluid flow may be introduced into the flat portion of the cuvette 310, which may be formed by two flat optical waveguides 320. As a variant of the above embodiment, an integral waveguide with a slit for the flow defined in the Z direction from the second group of designs mentioned above can be used. The second embodiment may allow a simple mechanical design of the cuvette in some possible embodiments. However, optical measurements can be performed in transmission mode and the flow can have substantial recycling after passing through the measurement region.

The sample fluid in the flat portion of the cuvette 310 may be illuminated with an appropriately shaped light beam 350 from the laser 340 or other suitable light source. The beam shape may be selected using criteria such as wide enough to cover the entire flow width and narrow enough to pass through the optical waveguide 320. The intensity of the transmitted light can be measured and analyzed to determine sample transparency. The width of the concentrated sample fluid flow can be adjusted to reach the desired level of sample transparency. Once the desired level of sample transparency is achieved, the size parameters of the particles in the sample fluid (eg, the particle size distribution exceeds a predetermined critical diameter) can be measured by known optical and electronic methods with relatively high accuracy. Can be.

In a third embodiment, as shown in FIGS. 9A, 9B, and 9C, the sample fluid flow is into a flat portion of the cuvette 410 that may be formed by the flat optical window 470 and the cylindrical lens 480. Can be introduced. This embodiment may allow for greater optical signal collection angles, but may also present challenges in the mechanical design of the cuvette 410. The dimension Z can be determined by the lens diameter and can be substantially larger than in the first or second embodiment.

10 shows an example of a fourth embodiment. As shown, the sample flow may be an annular "thread" of flow having a thickness X. Exemplary light guide and scattered light collection systems can be made of glass, sapphire or quartz. Scattered light can be delivered to a light detection and signal processing system by a fiber optic guide. Such a guide can be used to connect (convert) the annularly distributed signal to a linear optical detector. 11 shows a fifth embodiment similar to the fourth embodiment.

12A, 12B, 12C and 12D show an exemplary particle monitoring system according to the sixth embodiment. In this embodiment, the waveguide can be formed using a cylindrical biconcave lens. The slit can be cut at the center of the lens and polished for light passage. In this embodiment, the slit width can be fixed.

Experimental results show the ease of concept described herein. For example, the experiment was carried out using the optical cuvette (ie formed by the flat window and the cylindrical lens) of the third embodiment. Examples of such optical cuvettes are shown in FIGS. 9A, 9B and 9C. In this exemplary embodiment, the width of the flow was 10 mm and the sample thickness (X, measured by shim) was ˜100 μm. The diameter of the cylindrical lens was 5 mm and the window diameter was 20 mm. Cylindrical lenses were used to partially concentrate the laser beam near the cylinder-window (detection area). The laser beam was magnified before reaching the optical cuvette by another cylindrical lens to provide uniform illumination along the entire sample length in the Y axis.

In an exemplary experimental embodiment, the housing was made of black Delrin material and the window was partially glued or rubber-sealed. The pressure drop measured at these cell parameters was -1.5 psi for a flow rate of 100 ml / min. The pressure, translated to 7.5 psi at 500 ml / min, should be acceptable for most semiconductor applications.

In this embodiment, the sample is irradiated with a laser and subjected to a custom deformation to reduce the pulse length to remove the image “penetration” of the moving particles. The laser beam was stopped at the collecting lens plane and the collecting lens was used to send square scattered light to a video camera (WT-502, manufactured by Watec Corp.). Images were recorded on a PC using Airlink + frame grabber.

In this embodiment, the experimental results showed a medium in which the non-dilution slurry was scattered uniformly in the “milky phase”. The slurry was transparent due to the small thickness. 1588 nm polymer microspheres in DI water prepared by Duke Scientific Corporation were tested for optical system sensitivity and the ability to record particles of this size. The same concentration of 1588 nm globules was placed in the slurry. The results showed that the added particles were clearly detectable in slurry as well as in DI water.

In this embodiment, the experimental data suggests:

The slurry becomes transparent at the reference thickness and optical methods can be used for particle characterization.

The cuvette resistance to flow can be kept low to effect operation at relatively high flow rates, such as 500 ml / min.

The total flow can be investigated and can be examined for the presence of large particles.

Background scattering from the slurry does not prevent the registration of large particles.

Thus, as one embodiment, experimental results suggest that 100% of the slurry flow can be monitored at a flow rate of 500 ml / min or less.

As described, exemplary embodiments relate to non-invasive systems and methods for in-line or off-line monitoring of a single particle over a wide range of sizes and concentrations contained in a system comprising mostly small particles. . Exemplary methods can accommodate mixtures that do not require dilution thereof and mixtures in which the "tail" of the largest particles in the particle size distribution can be accurately measured. Optical characterization of particles over a wide range of sizes and concentrations in a concentration system can be achieved using an example embodiment of an optical flow cell, such as a cuvette, wherein the sample flow is adapted to apply optical techniques for particle characterization. It is made relatively transparent.

In an embodiment, a system for chemical and mechanical polishing of a semiconductor wafer shown in FIG. 4 is a slurry source (17) comprising SiO ₂ or Al ₂ O ₃ particles suspended in an acid or base solution at a 4-18% weight solids concentration. ). The particle size range is, for example, 0.03 micron to 1.0 micron diameter or more. In some cases, some of the slurry 16 may contain particles of large size due to aggregation or contamination of the slurry particles. It is desirable to remove particles or aggregates of particles from the slurry 16 before the slurry 16 reaches the semiconductor wafer 9, where large particles may damage the semiconductor wafer.

The chemical mechanical polishing system 12 includes an inline particle detection monitor 2 capable of detecting the size of particles flowing through the slurry delivery line 15. The in-line particle size detection monitor 2 is provided by the system 200 shown in FIG. 7B, which system includes a cuvette 210, an optical camera or two prisms in optical communication with the cuvette 210. Identify devices that include a detector 230 (eg, CCD camera, CMOS, photodiode or other optical sensing device). An associated light source 240, such as a laser, for example, which generates the light beam 250, may be in optical communication with the cuvette 210.

Sample transparency may be measured by quenching, and the sample fluid thickness may be adjusted in the flat portion of the cuvette 210 to obtain a predetermined transparency value or sensing volume value. Conventional light scattering and / or quenching techniques can be used to measure the parameters of a single particle having a particle size above the detection limit. Charge-coupled devices (CCDs) or CMOS detectors / cameras 230, together with appropriate frame-capturing electronics and data-handling software, provide background scattering upon quantitative detection of signals generated by individual particles passing through the optical sensing volume. It can be used to suppress the effect on.

If particles having a size larger than a predetermined size, such as 1 micron, are detected, the control unit 4 sends a portion of the slurry 16 containing these particles having a size larger than the predetermined size back to the slurry waste container 14. To activate the three-way valve 3 located in the slurry delivery line 15 downstream of the particle detection monitor 2. A portion of the slurry 16 that does not contain particles exceeding a predetermined size is done with the slurry delivery arm 11 so that they are directed onto the wafer 9 and used to chemically polish the surface of the wafer 9.

The actuation timing of the detection system 2 and the 3-way valve 3 is synchronized and when the portion of the slurry reaches the 3-way valve 3 at point D in the slurry line 15, the slurry line ( A part of the slurry detected by the detection means 2 at point C of 15 is sent to the waste container 14. Portions of the slurry containing undesirable large particles may diffuse due to turbulence and flow non-uniformity during migration from point C to point D. The diffusion of this portion or packet of particles may be directed to the waste container 14 by adjusting the time delay and / or prior to actuating the three-way valve 3 as disclosed in connection with FIG. 5. It can be compensated by adjusting the length of time.

In short, systems and methods are disclosed for selective object manipulation in multicomponent flows. Exemplary systems can include detection systems for monitoring components such as particles in the flow carrier. The system may also include an apparatus (eg, a valve or actuator) for manipulating the detected component from other components in the flow carrier. A controller or other processor can receive and process the protected component data and can distinguish the component of interest from the remaining flowable sample. Once the component is recognized, the controller synchronizes the flow manipulation device with the detection system to organize the detected component from the flow carrier.

The description is presented to enable those skilled in the art to make and use the systems and methods described herein well, and is provided with specific applications and requirements thereof. It is well known to those skilled in the art that various modifications to the above embodiments are possible, and the general principles described herein may be applied to other embodiments and applications without departing from the spirit and scope of the claims. Thus, the illustrated embodiments are not intended to provide limitations, but should be accorded the widest scope consistent with the principles and features described herein.

Claims

Means for detecting and mapping components in the flow carrier;
Means for manipulating the flow component; And
Means for controlling the manipulation of the detected component,
The means for manipulating the flow component is adapted to remove or separate the detected component from other components in the flow carrier, and wherein the control means is adapted to synchronize the manipulation means with the detection means. system.

2. The system of claim 1 wherein the object is a particle.

The system of claim 1, wherein the object is an aggregate of particles.

The system of claim 1, wherein the object is a cell.

2. The system of claim 1 wherein the object is part of a multicomponent flow having one or more variables that deviate from a desired value.

2. The system of claim 1 wherein the multicomponent flow comprises a liquid or a mixture of liquids.

The system of claim 1, wherein the multicomponent flow comprises a liquid having particles.

The system of claim 1, wherein the multicomponent flow comprises a bubbled liquid.

The system of claim 1, wherein the multicomponent flow comprises a liquid with dissolved material.

The system of claim 1, wherein the multicomponent flow comprises a liquid with biological material.

The system of claim 1 wherein the multicomponent flow is a slurry.

2. The system of claim 1 wherein the multicomponent flow is an emulsion.

2. The system of claim 1 wherein the multicomponent flow is ink.

2. The system of claim 1 wherein the multicomponent flow is blood.

The system for selective object manipulation in a multicomponent flow according to claim 1, wherein said detection means ignores the presence of other objects (particles) with different characteristics, while detecting the presence of particles or objects with specific characteristics.

The system for selective object manipulation in multicomponent flow according to claim 2, wherein said detecting means comprises an optical method based on irradiation scattering (particularly suitable for particle detection).

The system for selective object manipulation in multicomponent flow according to claim 1, wherein said detecting means comprises an optical method based on polarization or wavelength change.

The system for selective object manipulation in multicomponent flow according to claim 1, wherein said detecting means comprises an ultrasonic or megasonic sensor.

The system of claim 1, wherein the means for detecting comprises X-ray scattering or reflection.

The system for selective object manipulation in multicomponent flow according to claim 1, wherein said detecting means comprises an electrical or electromagnetic sensor (e.g. a capacitance sensor).

The method of claim 16, wherein the detecting means,
A cuvette adapted to define an opaque flowable sample for at least a first wavelength range of light waves;
Compress the flowable sample in a first direction and control the sample in a second direction parallel to the flow direction and orthogonal to the first direction, while positioned in the cuvette, while the sample is controlled in a third direction orthogonal to the first and second directions A transparent flow compression element adapted to extend; And
A monitor for monitoring the flowable sample using at least one wavelength,
And if the sample is compressed in the first direction, the sample becomes transparent for at least one wavelength in the wavelength range of the light wave.

2. The system of claim 1 wherein the detection component mapping means comprises labeling each detection event according to a time stamp.

The system for selective object manipulation in multicomponent flow according to claim 1, wherein said flow manipulation means is adapted to separate the detected components from other components in the flow carrier.

The system of claim 1, wherein the flow manipulation means is adapted to remove or destroy the detected components in the flow carrier.

24. The system of claim 23, wherein the flow separating means comprises a flow splitting device for at least two subflows.

27. The system of claim 25, wherein the flow splitting device for at least two subflows has a valve in each subflow.

27. The system of claim 25, wherein at least one subflow is in a multicomponent flow directed to the main flow line.

26. The system of claim 25, wherein at least one subflow is for multi-component flow in a waste or waste collection system.

24. The system of claim 23 wherein the flow separation means comprises a three-way valve.

30. The system of claim 29 wherein the flow separation three-way valve " ON " outlet is connected to the main flow line.

30. The system of claim 29, wherein the flow separation three-way valve “always OFF” outlet is connected to a waste flow line.

25. The system of claim 24, wherein the flow component removal means comprises a special chemical injector for local change of flow characteristics.

25. The system of claim 24, wherein the flow component removal means comprises a laser or other source of electromagnetic radiation.

The system for selective object manipulation in multicomponent flow according to claim 1, wherein said flow manipulation means comprises means for controlling the manipulation of the detected component, said control means being adapted to synchronize the detection means with the detection means.

35. The system of claim 34 wherein the control means is part of a component detection means.

35. The system of claim 34, wherein the control means is part of a flow component manipulation means.

35. The system according to claim 34, wherein said control means is a computer.

35. The system of claim 34, wherein the control means is a data processing system.

35. The system of claim 34, wherein the synchronization of the operating means and the detecting means comprises a predetermined time delay between the detection and the operation of the component.

40. The method of claim 39, wherein the time delay is a flow velocity function and the time delay function of the flow velocity performs selective object manipulation in a multicomponent flow measured as a flow velocity divided into cross sections of a flow connector line between detection and manipulation systems. System.

35. The system of claim 34, wherein the synchronization of the operating means and the detecting means comprises a predetermined time duration to manipulate the component.

42. The system of claim 41 wherein the predetermined time duration for manipulation of the component is a function of flow rate, activation time for the flow manipulation system, turbulence of the flow and desired waste minimization factor.

42. The system of claim 41, wherein the time duration for manipulation of the components is measured experimentally using a second detection system at the location of the flow manipulation system.

Means for detecting and mapping components in the flow carrier;
Means for manipulating the flow; And
Means for controlling the manipulation of the detected component,
The flow manipulation means is adapted to manipulate the detected components while preserving other components in the flow carrier,
Said control means being adapted to synchronize said operating means with detection and mapping means.

Detecting and mapping components in the flow carrier; And
Manipulating the detected components while preserving the other components in the flow carrier,
And wherein said manipulating the detected components is synchronized with detecting and mapping the components.

46. The method of claim 45 wherein the object is a particle.

46. The method of claim 45, wherein said object is an aggregate of particles.

46. The method of claim 45, wherein said object is a cell.

46. The method of claim 45, wherein the object is part of a multicomponent fluid having one or more variables that deviate from a desired value.

46. The method of claim 45, wherein said multicomponent flow comprises a liquid or a mixture of liquids.

46. The method of claim 45, wherein said multicomponent flow comprises a liquid having particles.

46. The method of claim 45, wherein said multicomponent flow comprises a bubbled liquid.

46. The method of claim 45, wherein said multicomponent flow comprises a liquid having dissolved material.

46. The method of claim 45, wherein said multicomponent flow comprises a liquid having a biological material.

46. The method of claim 45 wherein the multicomponent flow is a slurry.

46. The method of claim 45 wherein the multicomponent flow is an emulsion.

46. The method of claim 45 wherein the multicomponent flow is ink.

46. The method of claim 45, wherein said multicomponent flow is blood.

46. A method according to claim 45, wherein said detection means ignores the presence of other objects (particles) with different characteristics, while detecting the presence of particles or objects with specific characteristics.

46. The method of claim 45, wherein said detecting means comprises an optical method based on irradiation scattering (particularly suitable for particle detection).

46. The method of claim 45, wherein said means for detecting comprises an optical method based on polarization or wavelength change.

46. The method of claim 45, wherein said detecting means comprises an ultrasonic or megasonic sensor.

46. The method of claim 45, wherein said means for detecting manipulates an optional object in a multicomponent flow comprising X-ray scattering or reflection.

46. The method of claim 45, wherein said means for detecting comprises an electrical or electromagnetic sensor (such as a capacitance sensor).

The method of claim 59, wherein the detecting means,
A cuvette adapted to define an opaque flowable sample for at least a first wavelength range of light waves;
Compress the flowable sample in a first direction and control the sample in a second direction parallel to the flow direction and orthogonal to the first direction, while positioned in the cuvette, while the sample is controlled in a third direction orthogonal to the first and second directions A transparent flow compression element adapted to extend; And
A monitor for monitoring the flowable sample using at least one wavelength,
And when the sample is compressed in the first direction, the sample becomes transparent for at least one wavelength in the wavelength range of the light wave.

46. The method of claim 45, wherein said detection component mapping means comprises labeling each detection event according to a time stamp.

46. The method of claim 45, wherein said flow manipulation means is adapted to manipulate the selective object in a multicomponent flow adapted to separate the detected components from other components in the flow carrier.

46. The method of claim 45, wherein said flow manipulation means is adapted to manipulate selective objects in a multicomponent flow adapted to remove or destroy the detected components in the flow carrier.

68. The method of claim 67, wherein said flow separating means comprises a flow splitting device for at least two subflows.

70. The method of claim 69, wherein the flow splitting device for the at least two subflows manipulates an optional object in a multicomponent flow having a valve in each subflow.

70. The method of claim 69, wherein at least one subflow manipulates the selective object in a multicomponent flow towards the main flow line.

70. The method of claim 69, wherein at least one subflow is directed to a waste or waste collection system.

68. The method of claim 67, wherein said flow separation means comprises a three-way valve.

74. The method of claim 73 wherein the flow separation three-way valve “always on” outlet is connected to a main flow line.

74. The method of claim 73 wherein the flow separation three-way valve “always OFF” outlet is connected to a waste flow line.

69. The method of claim 68, wherein said flow component removal means comprises a special chemical injector for local changes in flow properties.

69. The method of claim 68, wherein said flow component removal means includes a laser or other source of electromagnetic radiation.

46. The method of claim 45, wherein said flow manipulation means comprises means for controlling the manipulation of the detected component, said control means for manipulating the selective object in a multicomponent flow in which the manipulation means is adapted to synchronize with the detection means.

79. The method of claim 78, wherein said control means is part of a component detection means.

79. The method of claim 78, wherein said control means is part of a flow component manipulation means.

79. The method of claim 78 wherein the control means is a computer.

79. The method of claim 78 wherein the control means is a data processing system.

79. The method of claim 78, wherein the synchronization of the operating means and the detecting means comprises a predetermined time delay between detection and operation of the component.

84. The selective object manipulation of claim 83, wherein said time delay is a flow velocity function and said flow velocity time delay function is measured as a flow velocity divided into cross sections of a flow connector line between detection and manipulation systems. How to.

46. The method of claim 45, wherein the synchronization of the operating means and the detecting means comprises a predetermined time duration to manipulate the component.

86. The method of claim 85, wherein the predetermined time duration for manipulating the component is a function of flow rate, activation time for the flow manipulation system, turbulence of the flow, and desired waste minimization factor.

86. The method of claim 85, wherein the time duration for manipulation of the component is measured experimentally using a second detection system at the location of the flow manipulation system.

A cuvette adapted to define an opaque flowable sample at least for a first wavelength range of the light waves;
Compress the flowable sample in a first direction and control the sample in a second direction parallel to the flow direction and orthogonal to the first direction, while positioned in the cuvette, while the sample is controlled in a third direction orthogonal to the first and second directions A transparent flow compression element adapted to extend; And
A monitor for monitoring the flowable sample using at least one wavelength,
And when the sample is compressed in the first direction, the sample becomes transparent for at least one wavelength in the wavelength range of the light wave.

89. The particle monitoring system of claim 88, wherein the transparent flow compression element comprises one or more optical elements.

89. The method of claim 88, wherein the at least one optical element comprises two prisms or two waveguides or cylindrical lenses and an optical window or a first light guide and a second light guide,
The particle monitoring system, wherein the second light guide is confined to transmit scattered light, or the optical waveguide has holes through which the flowable sample flows.

90. The particle monitoring system of claim 89, wherein the at least one optical element comprises a protective coating.

89. The particle monitoring system of claim 88, comprising a mechanism operably connected to at least one optical element and defined to adjust a distance between the at least one optical element.

95. The particle monitoring system of claim 92, wherein said mechanism comprises at least one screw, a hydraulic actuator, a pneumatic actuator, and an electromagnetic actuator.

95. The particle monitoring system of claim 92, wherein said mechanism is adapted to vibrate one or more optical elements.

89. The particle monitoring system of claim 88, comprising a light source in optical communication with the cuvette.

95. The particle monitoring system of claim 95, wherein said light source comprises a laser.

89. The particle monitoring system of claim 88, wherein the monitor comprises a detector in optical communication with the cuvette.

97. The particle monitoring system of claim 97, wherein said detector comprises at least one of a line scanner, a CCD camera, a CMOS camera, and a photodiode camera.

Defining an opaque flowable sample for at least the first wavelength range of the light wave;
Measuring the transparency of the flowable sample;
Compressing the flowable sample in a first direction, while defining the sample in a second direction that is parallel to the flow direction and orthogonal to the first direction, while extending the sample in a third direction orthogonal to the first and second directions ; And
Identifying the characteristics of the particles contained in the compressed sample,
And when the sample is compressed in the first direction, the particles become transparent for at least one wavelength in the wavelength range of the light wave.

107. The method of claim 99, wherein said compressing compresses from about 50 microns to 3 millimeters in the first direction, while defining the flowable sample from about 10 microns to 3 millimeters in the second direction and about 5 flow samples in the third direction. A method for monitoring particles comprising extending from millimeters to 25 millimeters.

101. The method of claim 100, wherein the compression comprises using a transparent flow compression element.

102. The method of claim 101, wherein the transparent flow compression element comprises one or more optical elements.

107. The method of claim 99, comprising adjusting a distance between the one or more optical elements using a mechanism operatively coupled to the one or more optical elements.

109. The method of claim 103, wherein the mechanism is adapted to vibrate one or more optical elements.

107. The method of claim 99, wherein the measurement of transparency comprises illuminating the sample using a light source in optical communication with the cuvette used to define the flowable sample.

107. The method of claim 99, wherein the identifying characteristic of the particle comprises detecting an optical signal using a detector in optical communication with the cuvette.

107. The method of claim 106, wherein the optical signal is delivered through the sample.

107. The method of claim 106, wherein the particles reflect the optical signal from the sample.

107. The method of claim 99, wherein the slurry feed to the process wherein the entire slurry utilized by the process is utilized is monitored as a flowable sample.

99. Use of the device according to any of claims 1 to 44 and 88 to 98 for chemical mechanical polishing.

109. Use of the method according to any one of claims 45-87 and 99-109 for chemical mechanical polishing.