WO2007028345A1 - Procede de detection a haut debit destine aux echantillons solides et systeme correspondant - Google Patents

Procede de detection a haut debit destine aux echantillons solides et systeme correspondant Download PDF

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Publication number
WO2007028345A1
WO2007028345A1 PCT/CN2006/002351 CN2006002351W WO2007028345A1 WO 2007028345 A1 WO2007028345 A1 WO 2007028345A1 CN 2006002351 W CN2006002351 W CN 2006002351W WO 2007028345 A1 WO2007028345 A1 WO 2007028345A1
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tested
sample
temperature
measuring
optical
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PCT/CN2006/002351
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English (en)
Chinese (zh)
Inventor
Peijun Cong
Zhifu Liu
Wenhui Wang
Youqi Wang
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Accelergy Shanghai R & D Center Co., Ltd
Accelergy Corporation
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Publication of WO2007028345A1 publication Critical patent/WO2007028345A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/16—Measuring arrangements characterised by the use of optical techniques for measuring the deformation in a solid, e.g. optical strain gauge
    • G01B11/161—Measuring arrangements characterised by the use of optical techniques for measuring the deformation in a solid, e.g. optical strain gauge by interferometric means

Definitions

  • the present invention relates to a high throughput measurement method and system for simultaneously measuring changes in length of a plurality of samples to be tested under continuous temperature changes. Background technique
  • Coeff icient of Thermal Expansion is an important physical parameter of materials and has an important influence on the engineering application of materials.
  • the coefficient of thermal expansion is primarily measured by measuring the structural parameters of the material: the length varies with temperature and is calculated from the definition of the coefficient of thermal expansion. In the field of high-throughput material characterization and screening, the measurement of thermal expansion coefficient has the following characteristics: 1. The amount of sample is relatively small and there are many types. 2. The measurement range of the sample is wide. For the purpose of material development, it is desirable that the parameters of the material properties obtained are as complete as possible, and therefore it is desirable to obtain a coefficient of thermal expansion over the widest possible temperature range. Sometimes, the temperature is measured over a range of 1200 degrees Celsius. 3.
  • the optical measurement method is a commonly used measurement method in the industry, which can directly or indirectly measure the basic parameters such as temperature, displacement, volume, area, and height of the target.
  • measurement methods used in the industry include Michelson interferometry, Fabry-peort interferometry, and the like. These methods accurately measure the length of a single sample, The coefficient of thermal expansion can be obtained after the second measurement.
  • these methods can only measure the thermal expansion coefficient of one sample per test, which cannot meet the research and development needs of the industry.
  • the industry needs a way to test the coefficient of thermal expansion of several different samples at once. Summary of the invention
  • One aspect of the present invention is to provide a high-throughput measurement method for simultaneously measuring changes in length of a plurality of samples under continuous temperature changes, the technical solution of which is: a continuous temperature change,
  • a high-flux measurement method for measuring the length change of a plurality of samples to be tested is characterized in that: in the first step, an optical interferometry device and a plurality of samples to be tested are provided; and a plurality of samples to be tested are placed on a carrier member And causing at least two samples to be tested to be within the detection region of the optical interferometric device, wherein each sample to be tested defines a surface to be tested perpendicular to the direction of propagation of the light emitted by the optical interferometry device; a surface to be tested of the sample to be tested, providing a reference surface; in the second step, the optical interferometric measuring device activates the light to be measured and the reference surface defined by each sample to be tested, and the light reflected back is optically The reference light within the interfer
  • the third step is to analyze the interferogram i-ridge data obtained by the optical interferometry device, and calculate the value of the length change of each sample to be tested at different temperatures. Further, the operator can select a predetermined temperature during the heat treatment of the sample to be tested, and measure the sample to be measured by using an optical interferometry device.
  • the optical interferometric measuring device used in the present invention has the measuring principle of: Referring to FIG. 1, the light emitted by the light source 10 passes through the beam splitter 11 and then passes through the reference plane 12 and the sample, respectively. After the surface reflection of 13 is entered into the optical interferometry device 14, it is known from the interference properties of the light that the two beams reaching the photodetector have coherence and thus an interference pattern will be generated and recorded by the optical interference measuring device. If the position of the reference plane is changed, that is, the known small distance is moved back and forth along the direction of the light, a certain phase change will be introduced in the reference light, and the output of the optical interferometric measuring device will also change accordingly.
  • the topography of the sample surface can be reversed. Further, it may also be a method of generating a phase shift, that is, without using a reference plane, but using two orthogonal polarization states of light as reference light and measurement light, respectively, for example, by inserting a waveplate to change the reference light.
  • the phase Fast and accurate measurement of the surface appearance of the sample surface can be achieved by phase shifting interference technology.
  • the specific phase-shifting interferometer used has been launched by a number of companies on the market. The specific companies include Vecco and 4D technology.
  • the thermal expansion is omnidirectional, and the thermal expansion in a certain direction is linear and extends to both ends.
  • the extension data of only one end in one direction is not comprehensive, and a reference plane is needed to jointly determine the direction, and the length of the sample to be tested changes at different temperatures.
  • the reference surface provided may be a second surface to be tested defined by each sample to be tested, which is parallel to the surface to be tested, or may be a sample to be tested.
  • the defined plane for example, may be the support surface defined by the support. Since different reference planes are selected, they will be different in the specific implementation manner. Therefore, the two methods will be further explained below.
  • the manner of measuring the two surfaces to be tested by using the phase shifting interferometer is: Outside the parallel surfaces to be tested, an optical interferometric measuring device is placed, and each optical interferometric measuring device is only used to measure and record the length change data of one of the surfaces to be tested at different temperatures.
  • the two surfaces to be tested selected for the sample to be tested may be any two planes that are relatively parallel and perpendicular to the light emitted by the optical interferometer, for example, taking the sample to be tested as a regular cube, and two parallel surfaces to be tested. It can be the upper and lower surfaces, or the left and right surfaces, or the front and back surfaces.
  • the reference surface of the sample to be tested is defined by the sample to be tested, as shown in FIG. 2, a plurality of samples 21 and 22 to be tested are placed on the carrier substrate 20, and each sample 21, 22 to be tested is defined.
  • the direction of propagation of the light emitted by 24; the first and second optical interference devices 23, 24 are respectively placed outside the two surfaces to be tested 21, 22, and the light emitted by each of the optical interference devices 23, 24 (shown in dashed lines in the figure) are perpendicularly incident on the respective tested surfaces 210, 211, 220, 221, and then reflected back into the optical interferometric measuring device, forming an interference pattern with the reference light and recorded, and then, at different predetermined temperatures Applying an optical interferometry device to measure and record the interferogram data,
  • the reference surface is defined by the non-test sample itself
  • the change and wavelength of the interference pattern are known, and the reference surface is not moved, and the measurement surface can also be judged. Relative displacement. Therefore, instead of directly measuring the height change of the sample, it is By measuring the relevant reference surface, it is also possible to obtain the amount of change in the length of the sample to be tested at different temperatures. For example, the amount of change in position of the upper surface of the sample and its supporting surface after the temperature change is directly measured, and the change in the length of the sample supporting surface is subtracted from the calculation, and the change in the length of the sample to be tested is also known.
  • the reference surface of the sample to be tested is defined by the non-test sample itself, as shown in FIG. 3, a plurality of samples to be tested 31, 32 are placed on the support substrate 30, and the optical interferometry device is disposed on Above the support substrate 30, in order to obtain a change in the length of the sample to be tested in the vertical direction, instead of measuring the upper and lower surfaces to be tested parallel to each other, the upper surface of the sample to be tested and the parallel thereto may be measured.
  • the upper surface of the support substrate 30 may be directly incident on the upper surface 301 of the support substrate 30 and the side to be tested 310, 320 and the side of the support substrate 30 of the sample to be tested 31, 32, and the light emitted by the optical interferometer (shown by a broken line in the figure) may be perpendicularly incident.
  • the interferogram data at a predetermined temperature, the length of the surface to be tested 310, 320 defined by the sample to be tested includes the support substrate
  • the length change value is subtracted from the length change values of the upper surfaces 301, 302 of the support substrate, which are each as reference surfaces, to obtain absolute values of their respective length changes.
  • the interference pattern of the optical interferometric device will periodically change. When the distance change is equal to a half wavelength distance, the interference pattern will complete one cycle. Variety. Therefore, during the temperature-programming process of the sample, the sampling interval of the optical measuring device should be small enough to avoid the information lost due to the above periodic changes, resulting in incorrect measurement. Generally, it is preferable to have 4 or more measurement data within a range of half wavelength. For comparison and calculation. The above is the measurement without changing the wavelength of the light wave. In other embodiments, the corresponding measurement data can also be obtained by changing the wavelength of the light wave. Since the wavelengths of the light waves are known, the amount of change in the length of the sample to be tested can also be obtained by a calculation method known in the art.
  • the sample to be tested may be any sample, and is not limited. Wherein, if the sample to be tested is transparent, a film with increased reflectivity may be plated on the upper surface of the sample before measurement to obtain a better measurement effect.
  • the coating may be in any manner known in the art, such as evaporating or sputtering a layer of high temperature resistant metal such as Al, Au, and the like.
  • the flatness of any plane is only a relative "Plat", in the microscopic state, the surface will have different degrees of depressions or protrusions. Therefore, the two parallel surfaces to be tested are only relatively parallel, and their vertical perpendicular to the measured light is only perpendicular. Not absolute vertical. Further, in order to obtain Better test results, the opposite surfaces of the sample to be tested (such as the upper and lower surfaces, or the left and right surfaces, or the front and back surfaces), can be surface treated before testing , that is, polishing treatment.
  • the degree of treatment of the surface of the sample to be tested is related to the selected optical interferometric measuring device, and specifically may be within a wavelength range of one wavelength to two tenths of the light emitted by the optical interferometric measuring device used. Further, in some cases, to ensure accuracy, the thickness of the sample should not be too small.
  • the obtained length data is an example for calculating the thermal expansion coefficient of the l Oppb level. If the height measurement accuracy is 0.5 nm, the height of the sample is preferably about 1 cm.
  • the support surface of the sample support for supporting the sample may also be subjected to surface treatment, on the one hand, to facilitate good contact with the sample to be tested, and on the other hand, to ensure good measurement if it is used as a measurement surface. As a result, the degree of polishing treatment is similar to that of the sample surface, as long as the selected optical measuring instrument can form interference fringes thereon.
  • a batch of the sample to be tested may be ground and polished together. Due to the diffraction effect of the sample edge at a certain height, the sample area and the sample spacing must be large enough to effectively observe the interference patterns of the upper and lower surfaces. After the sample is placed, as long as the different relative displacements of the surface of each sample and the surface of the adjacent sample table are measured at different temperatures, and then subtracted, the change of the height of the sample to be tested is obtained.
  • the positional relationship between the sample to be tested and its support may be varied, depending on actual needs, for example, all of the samples may be on one support surface or may be on different support surfaces.
  • the support substrate 40 is provided with a plurality of support surfaces 41, 42 each of which is provided with a sample to be tested 43, 44, optical
  • the interference device is located above the support substrate 40, and the upper surfaces 430, 440 to be tested of the samples to be tested 43, and their support surfaces 41, 42 as reference planes adjacent to the lower surface are measured.
  • the number of samples to be tested it is related to the selected specific optical interferometric measuring device. Since the selected optical interferometric measuring device has a certain detection area, subject to this limitation, the samples to be tested must all be in the detection area, and thus The number of samples to be tested will be limited.
  • the heat treatment of several samples it may be performed directly, for example, directly heating the sample to be tested; or indirectly, for example, heating the support, thereby indirectly making the sample disposed thereon The temperature rises.
  • the heating method of the sample to be tested or the support thereof may be a heating method known in the art, such as electric heating, microwave heating, infrared heating, laser heating, or the like. Since the speed of the optical measurement is fast, the heating rate can be accelerated accordingly, as long as the period information of 2 ⁇ is not lost during the measurement.
  • the change of the temperature of the sample to be tested it may be a process of rising up, or may be heated to a certain temperature first, and then in the process of cooling, which may be adjusted according to actual needs.
  • the temperature of the sample to be tested can be firstly raised or lowered at a suitable speed after being cooled or heated to a certain temperature by the cooling system, so that the entire measurement process can be completed.
  • the sample and its support are preferably placed in a relative adiabatic system with controlled heat exchange.
  • the heat treatment is carried out in a vacuum environment, since the sample to be tested can only lose heat by heat radiation and heat conduction, temperature control can be performed well.
  • the optical interferometric measuring device can perform a numerical measurement of several sample length changes in a short time, for example, some mature commercial phase shifting interferometers, Complete a measurement in milliseconds.
  • the measurement of the sample temperature should be synchronized with the measurement of the change of its length, and the speed of temperature rise and fall should be controlled within the acceptable range of the two measurements.
  • the measurement of the temperature and the change of the length of several samples is completed within several tens of seconds, and thus, the selected temperature measurement method needs to be a method for rapid temperature measurement known in the industry. For example, infrared thermometer rapid scanning measurement method, infrared camera parallel measurement method, temperature sensor array parallel measurement method, and the like.
  • thermometer rapid scanning measurement method
  • the response time of the general infrared thermometer is on the order of milliseconds. Therefore, if there are not many samples, such as less than 200, you can use the high-speed measurement method and dynamic trimming, such as the temperature measurement history and measurement speed, the sequence, the measured time or the measured temperature. Corrected. Make the temperature measurement and displacement measurement synchronized.
  • the surface temperature of the sample is measured in parallel by the same principle, so that it has the advantages of high speed, accuracy, and convenience in synchronizing with the displacement measurement result.
  • thermocouples and thermistors can be fabricated on the sample stage or on the sample.
  • temperature measurement can also be achieved.
  • a thermistor is formed on the surface of the silicon wafer, so that the silicon wafer on which the temperature sensor is fabricated can be used as the sample stage.
  • the temperature can be measured independently or the temperature of each sample can be fitted, so heating of the entire sample stage can be performed without uniformity. It is very high, but it should be ensured that it is sufficiently uniform in at least one sample to be tested, otherwise it will affect the accuracy of the measurement.
  • the temperature of the surrounding air is also changed due to heating/cooling of the sample;
  • the refractive index of air is related to temperature.
  • air acts as a medium for light transmission its refractive index change also introduces a change in phase.
  • measurement inaccuracies are caused, introducing a systematic error that is the same for each sample.
  • the heat convection ratio t of the air is strong, the temperature of the air on different measurement paths may be different, thus introducing different random errors between the samples.
  • the temperature variation range is large and the propagation path of the affected light is long, the influence of the propagation medium must be considered or removed.
  • the requirements for measurement error are not too high, these problems may be disregarded; if the requirements are higher, the measurement may be performed in a vacuum environment, for example, in a vacuum chamber. Avoid these errors caused by air. It can be determined by the operator.
  • a plurality of samples 51, 52 polished on the upper and lower surfaces are placed on the same polished sample stage 50, and heated.
  • the device 53 is below the sample stage 50 to heat the sample stage, and then heat-treats the sample; the optical interferometry device 55 and its mirror device 54 are placed over the sample to be tested to measure the upper surface 511, 521 of the sample to be tested and its opposite lower surface.
  • the amount of change in length of the supporting upper surfaces 501, 502 under continuous temperature changes.
  • the upper surface of the sample to be tested is polished to obtain a good optical surface.
  • the lower surface of the sample and the sample stage are polished to make full contact with the sample stage, so as to avoid additional displacement changes on the upper surface of the sample to be tested when temperature changes.
  • the specific degree of polishing can be determined according to actual needs.
  • the optical measuring instrument used is an optical interferometric measuring device known in the art, such as a phase shifting interferometer, it only needs to follow the operation of the measuring device. Just do it.
  • the obtained measurement data can be processed according to a processing method known in the industry to obtain data of the length change of the sample to be tested. Further, for the processing of the optical interferometry device data, it may be performed as a whole or separately.
  • the overall processing refers to taking 100 samples of the phase shifting interferometer as an example, and performing overall processing on the interference spectrum data of a certain temperature. Using the mature processing method of the industry, 100 data can be obtained on one map.
  • Separate processing refers to taking 100 sample measurements by phase shifting interferometer as an example, segmenting the interferogram data of a certain temperature, and dividing the interference map according to different positions of different samples in the test area, each The sample to be tested corresponds to the interference pattern of a region, and is thus arranged to obtain test data of each sample to be tested, and then calculate the thermal expansion coefficient of each sample to be tested.
  • the data processing of the optical interferometer is taken as an example, which is a mature field in the industry, and will not be described here.
  • the obtained value of the length change amount of several samples under continuous temperature change can be combined with the length data and temperature data of the sample to be tested, and the thermal expansion coefficient of the sample to be tested is calculated according to a known calculation formula.
  • the coefficient of thermal expansion at different temperatures of the sample to be tested is obtained by applying the measuring method of the present invention, which can also be used for other applications.
  • the coefficient of thermal expansion should also be changed correspondingly at these stages.
  • the softening point and conversion point of such materials can be found by analyzing the relationship between the coefficient of thermal expansion and temperature. See Figure 7 for the temperature profile of one of the glass materials.
  • the measuring method according to the present invention can also be applied to compare and screen the thermal expansion coefficients of a plurality of samples to be tested, as long as at least one reference sample of a known thermal expansion coefficient is added to a plurality of samples to be tested. Wherein, since the thermal expansion coefficient of at least one sample is known, the thermal expansion coefficient of other samples to be tested can also be derived by calculation.
  • a high-throughput measurement method according to the present invention is applied to perform screening of thermal expansion coefficients of a plurality of samples to be tested, as shown in FIG. 8, a plurality of samples to be tested 81, 82, 83, 84, 85, 86, 87, 88 arranged in a center-symmetric shape, placed on a circular sample disk 80 having a high thermal conductivity, by adding a central portion 89 of the sample disk 80 to raise the temperature to an upper temperature limit, and naturally cooling after maintaining a certain period of time, During the cooling process, the phase change of the upper surface of the sample and the surface of the adjacent sample disk is observed by a phase shifting interferometer (not shown), that is, the difference in thermal expansion coefficient between the sample to be tested and the reference sample can be compared. Among them, the more uniform the temperature distribution of the sample to be tested during the test, the more accurate the test results.
  • the composition of the sample to be tested which is generally screened is different, and therefore the heat capacity of each sample is also different.
  • a slight difference in sample temperature is bound to occur.
  • the effect of temperature non-uniformity on the accuracy of the thermal expansion coefficient is much less than the effect of the sample length change rate.
  • all samples will eventually cool to the same temperature, so the speed of the cooling rate has no effect over the entire temperature range, only affecting a certain part of the temperature range.
  • a plurality of samples to be tested are set as shown in FIG.
  • the samples to be tested 91, 92, 93, 94, 95, 96, 97, 98 are arranged in a center-symmetric distribution and placed on a circular sample disk 90, wherein the inner and outer sides of the circumference of the sample to be tested are arranged
  • the annular regions 901 and 902 having a large thermal resistance can reduce the cooling rate of the sample region.
  • different embodiments of the thermal resistance ring may be one or more concentric deep grooves made on the high thermal conductivity sample plate 90, or may be arranged in a concentric circle by a plurality of minute deep pits. The shape can vary with different needs.
  • the test tray may be placed in a closed cavity, and the cooling rate is adjusted by adjusting the pressure of the charged gas (in vacuum) In the state, the sample to be tested can only lose heat through heat radiation and heat conduction. After charging a large amount of gas, heat convection will play an important role, that is, accelerate the loss of heat, and if necessary, add forced convection to further increase the cooling rate due to It is a comparison, not an accurate measurement, and the effect of the refractive index change of the gas on each sample can be offset.
  • the above-disclosed application of the comparison of the thermal expansion coefficients of a plurality of samples to be tested is also fully applicable to the measurement of the thermal expansion coefficient.
  • the adjustment of the parameters during the test for example, the adjustment of the test environment, can be adjusted according to the content disclosed in this law and the specific needs.
  • another aspect of the present invention relates to a screening method for a thermal expansion coefficient of a thousand samples, which is a method of making a material to be tested and a base material together, and changing the degree of bending of the beam after the temperature is changed, and also comparing and screening.
  • the coefficient of thermal expansion of the material may be planarly connected, or may be a rectangular cross-connection as shown in FIGS. 10 and 11 to improve the adhesion strength.
  • the samples 101, 102, 103 and the substrate 100 pass through the protrusions 106 and the concave portion.
  • the matching of the grooves 107 forms a rectangular cross-connection.
  • the materials of different thermal expansion coefficients and the double-layer beams composed of the same size substrate have the same temperature change, and the degree of change in the degree of bending is also Differently, as shown in FIG. 12, since the coefficient of thermal expansion of the sample in one of the silent beam is known, the degree of bending of the layered beam relative to the known coefficient of thermal expansion is changed by comparing the respective double-layered beams. The amount, the relative relationship of the coefficient of thermal expansion of the sample can be obtained.
  • a high-flux measuring system capable of simultaneously measuring the change in length of two or more samples to be tested under continuous temperature change.
  • the technical solution adopted by the utility model is: a high-flux measuring system comprising a support body, a heat treatment device, a temperature measuring device and one or more optical interference measuring devices, wherein the support body is used for placing the sample to be tested, The heat treatment device is used for heat treatment of the sample, the temperature measurement device is used for recording the temperature data of the sample to be tested, and the optical interference measurement device is used for measuring and recording the length data of the sample to be tested under continuous temperature change.
  • the components used in the measurement system of the present invention may be known in the industry.
  • the device having this function may also be the device disclosed above.
  • the carrier member may be a carrier substrate composed of a high temperature resistant ceramic material or the like.
  • the measurement of the length change of several samples under continuous temperature change can be completed in one time, and the value of the change in length can be obtained.
  • These data can be used for the calculation of the coefficient of thermal expansion of the sample to be tested. Due to the measurement of the coefficient of thermal expansion of the sample to be tested, it mainly measures three main parameters: temperature and its amount of change; length of the sample; amount of change in length before and after the temperature change.
  • the measurement of the length and temperature of the sample is relatively simple, and various length measuring tools and temperature measuring tools are available in the industry, such as known temperature measuring devices: infrared thermometers, infrared cameras, temperature sensors, etc.; Known length measuring devices: vernier calipers, micrometers, etc.
  • the measurement accuracy of the sample length change is on the order of micrometers, even nanometers, which is the key to measuring the coefficient of thermal expansion.
  • the invention adopts an optical interferometric measuring device for length measurement, which can obtain a plurality of samples at one time, and the length change amount of the sample under continuous temperature change, thereby satisfying the industry's measurement of the thermal expansion coefficient of the high-throughput sample to be tested. need.
  • the unknown measurement may be obtained according to the obtained measurement data.
  • the interference spectrum of the sample to be tested is compared with the interference pattern of the known sample.
  • the thermal expansion coefficient of other samples to be tested can be inferred. This method has a great effect on the preliminary screening of materials that meet the thermal expansion coefficient of a certain standard. Save time and increase efficiency.
  • FIG. 1 is a schematic diagram of a measurement principle of a high-throughput measurement method according to the present invention
  • FIG. 2 is a schematic diagram of a measurement implementation manner of a high-throughput measurement method according to the present invention
  • FIG. 3 is a schematic diagram of still another measurement implementation method of the high-throughput measurement method according to the present invention
  • FIG. 5 is a schematic diagram of an embodiment of a high-throughput measurement method according to the present invention
  • FIG. Schematic diagram of an embodiment Figure ⁇ is a graph of the temperature and coefficient of thermal expansion of a certain glass sample drawn by using the data obtained by the measurement method of the present invention
  • FIG. 8 is a schematic diagram of an embodiment of screening a plurality of samples for thermal expansion coefficient by applying the high-throughput measuring method of the present invention, wherein only the setting mode and heating mode of the sample are illustrated;
  • Figure 11 is a partial enlarged view of Figure 10;
  • Fig. 12 is a view showing a state in which a combination of different sample materials and a base material shown in Fig. 10 is subjected to heat treatment. detailed description
  • the first stage the preparation of the glass sample block and the sample tray and the completion of the sample library
  • the first step 13 upper and lower surfaces of the glass sample to be tested are ground and surface-polished (a batch of samples to be tested are ground and polished together), and the polishing precision is about 0. 05 um; the upper surface is splashed in a vacuum after polishing and polishing. A layer of high temperature resistant gold film is formed into a cylindrical glass sample block, and the sample diameter is 4 awake.
  • a sample plate made of stainless steel is used as a supporting member of the sample, and the upper and lower surfaces are treated with 05 ⁇ The measured sample of the same batch of grinding and polishing, polishing accuracy of about 0. 05 legs.
  • the sample tray has a diameter of 50 mm and a thickness of 2 mm;
  • 13 samples to be tested are arranged on the sample tray along a predetermined circumference to complete the preparation of the sample library.
  • the thermal expansion coefficient of the glass sample is calculated by phase shifting interferometer.
  • the sample library is placed in a vacuum chamber
  • the sample stage is heated at a certain speed by electric heating. Heat to 350.
  • C begins to measure the temperature of each sample using an infrared temperature measuring instrument and uses a phase shifting interferometer to measure the surface of the sample at this time and the surface of the sample surface of the sample edge, and then stabilize the temperature rise every 10 degrees.
  • C measures a set of data until the temperature reaches 800 ° C;
  • the height difference of the sample is obtained by subtracting the independent relative displacements of the upper surface of each sample and the surface of the side sample table at each two temperatures. Then, a set of data of the height of the sample as a function of temperature is obtained. The obtained data are averaged to obtain ⁇ ⁇ ⁇ ;
  • the obtained data is brought into the calculation formula of the linear expansion coefficient of the glass:
  • 16 samples to be measured are polished on the upper and lower surfaces, and the thickness of the sample after polishing is 1 cm, and then placed on the same polished sample stage;
  • sample stage is placed in a space, sealed and evacuated to 10- 6 bar;
  • an infrared heating device is used, and the sample is subjected to l.
  • the speed of the C/rain is heated, and at the same time, the change in the height of the sample (the height change of the step on the upper surface and the surface of the sample stage) is accurately measured by the phase shifting interferometer to obtain the rate of change of the sample length.
  • the fourth step is to heat up to 700. Stop heating after C, stop measurement, and naturally cool down;
  • the two-dimensional map is drawn by using the measured length change and temperature data, and the temperature (range) of the softening point of each sample material can be found in the drawn two-dimensional map, and 16 samples are compared and screened.

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Abstract

Un procédé pour mesurer un changement de durée pour un débit élevé comprend les stades suivants: au premier stade, on fournit un dispositif d'interférométrie optique et plusieurs échantillons testés; au deuxième stade, les échantillons testés sont mis à la portée de détection du dispositif d'interférométrie optique, un traitement thermique est appliqué aux échantillons testés et, en même temps, le dispositif d'interférométrie optique est utilisé pour mesurer les échantillons alors que les données de température correspondantes sont enregistrées; au troisième stade, les données provenant d'un dispositif d'interférométrie optique sont analysées, puis la quantité de changement de durée pour chacun des échantillons testés à de différente température est calculée.
PCT/CN2006/002351 2005-09-09 2006-09-11 Procede de detection a haut debit destine aux echantillons solides et systeme correspondant WO2007028345A1 (fr)

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