WO2007028344A1 - 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
WO2007028344A1
WO2007028344A1 PCT/CN2006/002350 CN2006002350W WO2007028344A1 WO 2007028344 A1 WO2007028344 A1 WO 2007028344A1 CN 2006002350 W CN2006002350 W CN 2006002350W WO 2007028344 A1 WO2007028344 A1 WO 2007028344A1
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WIPO (PCT)
Prior art keywords
samples
tested
sample
temperature
different
Prior art date
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PCT/CN2006/002350
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English (en)
Chinese (zh)
Inventor
Peijun Cong
Zhifu Liu
Wenhui Wang
Youqi Wang
Original Assignee
Accelergy Shanghai R & D Center Co., Ltd
Accelergy Corporation
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Application filed by Accelergy Shanghai R & D Center Co., Ltd, Accelergy Corporation filed Critical Accelergy Shanghai R & D Center Co., Ltd
Publication of WO2007028344A1 publication Critical patent/WO2007028344A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
    • G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
    • G01N25/4846—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a motionless, e.g. solid sample
    • G01N25/4853—Details
    • G01N25/486—Sample holders
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
    • G01N25/04—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of melting point; of freezing point; of softening point

Definitions

  • the present invention relates to a high throughput testing method and system for testing a plurality of solid samples simultaneously. Background technique
  • the commonly used test methods are Different ial Scanning calorimeters (DSC) and gradient furnace methods, but it takes several hours to measure a temperature-time point using these conventional methods, and an experiment Only one point can be measured. It takes many experiments and a long time to complete a TTT chart.
  • DSC Different ial Scanning calorimeters
  • gradient furnace methods it takes several hours to measure a temperature-time point using these conventional methods, and an experiment Only one point can be measured. It takes many experiments and a long time to complete a TTT chart.
  • combinatorial chemistry With the wide application of combinatorial chemistry in materials research, researchers can simultaneously prepare many material samples and test the performance of these samples in a short period of time and screen these materials. The application of combinatorial chemistry methods has greatly improved the efficiency of new material discovery. In just a few years, material researchers have used combinatorial chemistry methods in high-temperature superconducting materials, magnetic materials, luminescent materials, polymer materials and catalysts. The field has made important discoveries. Compared with traditional methods, combined material research methods can systematically study more material systems in a shorter period of time.
  • the method is to superimpose the constituent element metals of the alloy to be studied and heat-treat at a high temperature, thereby forming a region having a compositional gradient composed of alloy constituent elements at the boundary of the superimposed element metal.
  • a phase diagram of the alloy can be obtained by analyzing the elemental and phase composition of this region. This method can determine the phase diagram of a binary or ternary alloy.
  • a method of determining the T. T. T. diagram of a slab material using a combinatorial chemistry concept is to first melt the glass material at a high temperature, then suck the molten glass into the capillary tube with a capillary tube, and rapidly cool down to solidify the glass in the capillary tube. Placing a capillary with glass in a furnace with a temperature gradient
  • the capillary tube with the glass sample was taken out for a while, and the crystallization in the glass sample was observed. By measuring the crystallization of the glass sample under different holding times, the glass material can be obtained.
  • T. T. T. map Multiple experimental points can be obtained at a time using this method, but multiple experiments are still required to obtain a complete ⁇ . T. T. map.
  • One aspect of the present invention is to provide a method of testing a high throughput solid sample.
  • the technical solution adopted includes the following steps: placing a plurality of samples to be tested on the provided carrying device; and secondly, heat treating at least two samples to be tested, and ensuring that at least two samples are always at Different temperatures;
  • the third step is to monitor the state of the sample to be tested, obtain monitoring data and record.
  • a plurality of samples to be tested are provided, which may include two forms: 1) a discontinuous form of a plurality of samples to be tested, that is, a plurality of samples to be tested, each to be tested The sample is spatially independent of the other samples to be tested; 1) a continuous form of several samples to be tested, ie a plurality of samples to be tested are combined. Further descriptions of the discontinuous and continuous forms of the samples to be tested are provided below.
  • discontinuous form of several samples to be tested it may include the following implementations: 1) These discontinuous samples to be tested are composed of the same material; for example, several discrete samples to be tested are It is composed of glass materials of the same composition; 2) the constituent materials of the discontinuous samples to be tested are different, that is, each sample to be tested is distinguished from other samples on the constituent materials; 3) the combination of the above two methods, That is, these discontinuous samples to be tested can be divided into several groups, and the samples to be tested in each group are composed of the same material, and the groups are composed of different materials, the number of groups and each group included.
  • the number of samples to be tested may be further determined by specific needs. In the above three cases, the specific number of samples is not limited, and may be set by the operator as needed.
  • another aspect of the present invention is to provide a method for preparing a sample of a sample to be tested in a discontinuous form.
  • the technical solution is as follows: the solid sample material is placed in the first receiving cavity, and the first receiving cavity is provided with a The hole is connected to the second receiving cavity; the solid sample material is heated to be melted, and the heating temperature is controlled, so that the sample material enters the second receiving cavity dripping through the opening of the first receiving cavity, and is in the second receiving cavity Cool to a spherical sample.
  • the quantity of the sample material and the material consistency of the plurality of sample materials can be set as needed.
  • the first receiving cavity and the second receiving cavity may be any known structure having a receiving function.
  • the first receiving cavity and the second receiving cavity may be respectively a melting groove, a receiving tube and the like.
  • the manner in which the sample material is converted into a molten state may be any known method.
  • the sample material is directly heated to be in a molten state; or by heating the first receiving chamber that carries it, thereby increasing its temperature to a molten state, and the like.
  • how to enter the second receiving chamber may be any manner known in the art, such as using its own gravity or the like.
  • the above method for preparing a plurality of discontinuous forms of the sample to be tested can be used to prepare a plurality of discrete samples to be tested.
  • a plurality of block sample materials 01, 102, 103, 104, 105 are placed in respective sample melting tanks 111, 112, respectively. , 11 3, 114, 115, there is a small hole at the bottom of each sample tank, and a thin tube 121, 122, 123, 124, 125 is connected under the hole; the sample tank is heated to melt the sample, and the heating temperature is controlled to make the molten glass A small hole along the bottom of the groove is dropped into the lower capillary tube, and solidified in a thin tube to form a spherical sample 131, 132, 1 33, 134, 135 of uniform size.
  • the respective constituent materials of the plurality of block sample materials 101, 102, 103, 104, 105 may be the same or different, depending on the needs.
  • each of the divided sub-regions may be directly connected to the adjacent sub-regions, or may be provided with a connector for connection therebetween.
  • each divided sub-area can be equivalent to a discontinuous sample monomer; if it is not the same, if each divided sub-area is large enough, it can be equivalent to a discontinuous waiting
  • the sample can also be divided into a number of sub-sub-regions that can correspond to a discontinuous sample monomer, which is equivalent to a set of discrete samples to be tested.
  • a plurality of samples 20 to be tested include a plurality of sub-regions 201, 202, 203, 204 that are usable for detection, and pass between the sub-regions.
  • the connectors 205 are joined together to form a continuous form of a plurality of samples to be tested.
  • each area that can be used for detection is equivalent to a discontinuous sample to be tested.
  • the form and constituent material of the connecting body 205 may be arbitrary as long as the sub-regions 201, 202, 203, 204 usable for detection can be connected together. There is no strict limit to the size and number of each area that can be used for detection, depending on the specific needs.
  • a plurality of samples 20 to be tested defining opposite first end regions 21 and second end regions 22, including W
  • the content of the 21nd direction to the second end region 22 is gradually decreasing, and the Z element is gradually decreasing from the second end region 22 to the first end region.
  • each sub-area is composed of different substances, or it may be composed of the same plurality of substances, but the percentages are different; for example, each sub-area includes two substances.
  • the sub-regions that are divided may also be longitudinally divided into a plurality of sub-sub-regions (as indicated by a vertical dashed line in the figure).
  • the sub-regions 2311 may be divided into four consecutive sub-regions 2311. , 2312, 2313, 2314, each of the divided sub-sub-regions is equivalent to one sample to be tested, and it can be said that each sub-region 231, 232, 233, 234, 235 is equivalent to a group including a plurality of samples to be tested.
  • Samples to be tested including a number of identically distributed Samples to be tested (eg, sub-sub-regions 2311, 2312, 2313, 2314). Further, the above embodiment may also evolve into the following manner. Among the sub-regions 231, 232, 233, 234, and 235, only a partial region is equivalent to one sample to be tested. For example, in one embodiment, as shown in FIG. 2D, in each sub-sub-region (shown by a vertical broken line in the figure), the partial regions 2351, 2352, 2353, and 2354 included therein are equivalent to one discontinuity. Sample to be tested. Further, in other alternative different embodiments, the composition of the material included in each sub-region may be any form known in the art, and is not limited to the embodiment of the two materials constructed in the above examples.
  • the continuous form of preparing a plurality of samples to be tested it may be any method known in the art, such as a well-established elemental/structural deposition method and the like.
  • sample to be tested may be composed of a known solid material such as glass, ceramic, refractory material, steel material, alloy or polymer material or the like.
  • the carrying device used may be any device known in the art to carry the carrying function.
  • a carrier device it can be a carrier substrate that can be used to carry a number of samples to be tested.
  • a plurality of regions having a receiving function may be disposed on the carrier substrate, for example, a recessed or protruding receiving cavity, a receiving groove, and the like.
  • the carrying device it may be connected by a number of components having a carrying function; for example, referring to Figure 3, the carrying device comprises several independent carrying elements?
  • the carrying member/accommodating cavity/accommodating groove or the like having the accommodating function in the carrying device may be regularly distributed, such as a matrix arrangement, a circumferential arrangement, etc.; Regular arrangement.
  • the carrier device or some specific region thereof, such as the region for carrying the sample is subjected to a higher temperature in the next step, the carrier itself is preferably capable of withstanding higher temperatures, or At least some of its specific areas can withstand higher temperatures.
  • the temperature range that can be tolerated it is between 100 °C and 3000. Between C, for example 800. C, 1000. C, 1200. C, 1400 ° C, 1600 ° C, 1800. C, 2000 ° C, 2200 ° C, 2400. C and so on, the specific adjustments are made according to different needs.
  • the carrying device itself may be subjected to a temperature gradient, that is, different temperatures of the different regions of the carrying device are different, so that the selected constituent materials for the carrying device preferably satisfy the two requirements.
  • the material that can be used for the carrier device may be various materials known in the art that can withstand high temperatures, such as precious metals, ceramics, steel materials, etc., specifically, it may be platinum, A1 2 0 3 , stainless steel, etc. .
  • a plurality of samples to be tested may be any manner known in the art or in the manner disclosed in the following.
  • a plurality of samples to be tested which may be in a continuous form or in a discontinuous form, are placed in a predetermined area of the carrier.
  • a predetermined area it may be an area having a carrying function for carrying a sample.
  • a containment function it may also have a containment function. Since a plurality of samples to be tested include a discontinuous form and a continuous form, the different placement embodiments will be further described below.
  • the manner in which they are placed on a predetermined area on the carrying device may be any manner known in the art, for example, directly seeing each of the samples to be tested placed on the carrying device. region.
  • the predetermined area preferably has a certain accommodating function to prevent a large change of the position of the sample to be tested on the carrying device, so as to avoid the change of the position may affect the other waiting in the subsequent procedure. Test the sample.
  • the predetermined area may be an area having a receiving function disposed on the carrying device; for example, the carrying substrate may be a regularly distributed/irregularly distributed receiving formed on the carrying substrate. Cavity.
  • the predetermined area may be a receiving area of each of the carrying members, such as a carrying device that is joined together by a plurality of turns, the predetermined area of which may be a receiving cavity of the weir.
  • the carrier substrate 40 is provided with a row of regularly arranged concave receiving cavities 41, 42, 43, 44 for the sample to be tested 45. They are respectively placed in corresponding receiving cavities, wherein each sample to be tested is the same as the constituent materials of other samples to be tested.
  • the carrying device is a carrying substrate 500, and a plurality of receiving cavities arranged in a matrix of 6 ⁇ 8 are disposed thereon.
  • the same sample to be tested is accommodated in the receiving chambers of a horizontal row 501, 502, 503, 504, 505, 506, but the sample to be tested in each horizontal row of the receiving cavity and the other horizontal row of the receiving cavity are to be tested.
  • the samples are different; for example, the first horizontal row 501 contains 8 identical first samples to be tested 511, and the sixth horizontal row 506 contains 8 identical sixth samples to be tested 516, the first type to be tested Sample 511 is different from sixth sample to be tested 516.
  • the manner and amount of placement of predetermined areas on the carrier device is arbitrary, as desired.
  • it can be arranged in a regular pattern, for example, a regular arrangement of a single row, a matrix arrangement of multiple rows (for example, a matrix arrangement of 3 ⁇ 10, a matrix arrangement of 5 ⁇ 10, a matrix arrangement of 10 ⁇ 10, etc., the specific number It can be arranged as needed, or it can be arranged in a circular arrangement; it can also be arranged randomly and irregularly.
  • the plurality of samples to be tested may be composed of the same material or different materials.
  • the carrier device is a carrier substrate, which may be attached to a predetermined area of the carrier substrate, for example, disposed on the carrier substrate; or may be directly formed on a predetermined area of the carrier substrate, such that a predetermined area of the carrier substrate is It is the area where the sample is set as a whole.
  • the predetermined area on the carrying device for carrying a plurality of samples to be tested does not necessarily need to have a containment function.
  • the manner of heat treatment of at least two samples to be tested may be in various ways known in the art, or may be the manner disclosed in the present disclosure. .
  • a heat treatment embodiment it may be to heat at least two samples to be tested (wherein, for a discontinuous form of several samples to be tested, which are two separate samples to be tested; and for a continuous form of several samples to be tested) , which is a partial area of the two sub-areas/sub-areas that are divided, controls its heating process so that its temperature is always different.
  • the temperature of each sample to be tested is different from other samples to be tested; or a plurality of samples to be tested are grouped, and the temperature of the sample to be tested in each group is the same, different groups
  • the temperature of the sample to be tested is different.
  • the specific value of the temperature can be set according to specific needs.
  • the heat treatment embodiment may be a heat treatment of the carrier device, and indirect heat treatment of a plurality of samples to be tested carried thereon (the sample to be tested comprises a continuous form and a discontinuous form).
  • the sample to be tested comprises a continuous form and a discontinuous form.
  • the heat carrying device forms a temperature gradient on or over a certain area, and causes at least two samples to be tested to be at different temperature values in the temperature gradient, so that the temperatures of at least two samples to be tested are always different.
  • the temperature gradient is realized in the carrying device or a certain region thereof, and the number of samples to be tested set in the region occupied by each temperature value in the temperature gradient may be one or several, depending on the specific Need to be determined.
  • the numerical range of the 3 ⁇ 4 degree gradient disclosed above is not limited, because in the actual application process, as the number of samples to be tested increases, the size of the carrying device increases, and the temperature difference between the highest point and the lowest point may be large.
  • the temperature difference can be between 0-1000 ° C, or between 0-2000 ° C, etc., and may be 20. C, 50 o C, 100 ° C, 300 ° C, 500 ° C, 600. C, 700 ° C, 800 o C, 900 ° C, 1200 ° C, 1500 ° C, 1800 ° C and so on.
  • the user can decide how to set the temperature gradient region according to the actual needs, and the size and distribution of the sub-regions with the same temperature value are determined according to actual needs.
  • the manner of heat treatment may be any one known in the art, such as one or more of heating methods such as infrared lamp heating, resistance wire heating, laser heating, and induction heating.
  • the temperature value is monitored to determine that the temperature is under control; wherein the temperature monitoring method can be any manner known in the art, such as using a thermocouple, an infrared thermometer, Thermal camera and other means of temperature measurement.
  • the heating environment can also be varied, for example, by heating the sample to be tested in air, various filling gases, or a vacuum environment.
  • discontinuous form of several samples to be tested and the heat treatment mode of the continuous form are separately described.
  • the carrier substrate 60 is provided with a plurality of receiving grooves 61, 62, 63 arranged in a row, each of the receiving grooves.
  • Each of the discontinuous samples to be tested 64, 65, 66 is accommodated, and the opposite end regions 601, 602 of the heat carrying substrate 6Q are heated to control the heating process so that the temperature difference between the end regions 601, 602 is present, and thus, through the substrate 60 itself.
  • the heat conduction forms a linearly distributed temperature gradient T1 - T5 on the substrate 60, and the receiving grooves 61, 62, 63 are respectively in different numerical regions T2, ⁇ 3, ⁇ 4 of the temperature gradient due to the positional relationship, so that the content thereof is discontinuous.
  • the samples to be tested 64, 65, 66 are at different temperatures.
  • the plurality of discontinuous samples to be tested used in this embodiment may be made of the same material, or may be made of different materials in other alternative embodiments.
  • the heating method of the carrier substrate it may also be uniform heating of the multi-segment region. To form temperature gradients of various values.
  • the carrier substrate 70 is provided with three rows of 721, 722, and 723 (shown by broken lines) in a circumferentially distributed arrangement.
  • each row includes a plurality of receiving holes 701, 702, 703, 704, 705, 706, 707, 708, 709, each of the receiving holes correspondingly contains a discontinuous sample to be tested 711, 712, 713, 714, 715, 716, 717, 718, 719, heating the central region 710 of the carrier substrate 70, through the substrate 70 itself
  • the heat conduction is formed on the substrate 70 to form a circumferentially distributed temperature gradient, wherein the direction of the arrow in the figure is the direction of decreasing temperature, and the three rows of receiving holes are respectively in different numerical regions T2 and ⁇ 3 of the temperature gradient due to the positional relationship. ⁇ 4, and then the samples to be tested placed in each row of the receiving holes are respectively at different temperatures.
  • the samples to be tested used in each row in this embodiment may be composed of the same material or different materials; the discontinuous samples to be tested may be the same or different.
  • the plurality of discontinuous samples to be tested may be composed of three different materials, and are divided into three groups according to different constituent materials, and each sample to be tested is in each group.
  • a certain numerical region of the temperature gradient that is, the temperature of each sample to be tested in each group is different from other samples in the same group, and as the number of samples to be tested increases, it may have 10, 20
  • Each of the 30, or more samples to be tested is in a different numerical region of the temperature gradient, providing more data for subsequent steps.
  • the grouping status of the specific sample to be tested and the specific number of samples to be tested in each group are determined by actual needs.
  • a continuous form of a plurality of samples to be tested is heat-treated, as shown in FIG. 8A, a plurality of continuous forms 800 of the sample to be tested are directly formed on the carrier substrate 80, and the constituent structures of the plurality of samples 80 to be tested are formed.
  • the content of a component/structure within it gradually decreases in the direction of the arrow shown (for example, as shown in the figure, Stepwise reduction from 100% to 0), whereby it can laterally divide several sub-regions 801, 802, 803, 804, 805, 806, 807, 808, 809, each sub-region and other
  • the constituent materials of the sub-regions are different, and each sub-region can be longitudinally divided into several consecutive sub-sub-regions (sub-regions and sub-sub-regions, as indicated by the vertical dotted line in the figure), ie
  • Each sub-area corresponds to a sample group containing a plurality of samples to be tested continuously;
  • the heat-bearing substrate is formed in the longitudinal direction of the carrier substrate in the direction indicated by the arrow in the figure Gradient, this such that different areas of the same sub-sub-sub-areas divided in the longitudinal direction, at different temperature values, and different sub-
  • direct heating of the sample to be tested may also be used.
  • the sub-region 808 divided by one of them is used as an example to directly heat the partial regions 811, 812, 813, 814, 815 of the divided sub-subregions, such that each sub-region The defined partial regions are at different temperature gradients, and the heat treatment methods for other sub-regions are similar, and the description will not be repeated.
  • the second step of the high-throughput sample testing method of the present invention may further comprise a temperature-controlling process, that is, maintaining the temperature of at least two samples at different temperatures at a certain value.
  • a temperature-controlling process that is, maintaining the temperature of at least two samples at different temperatures at a certain value.
  • the temperature rising mode disclosed above is further changed to maintain the temperature of the individual heating to a certain time when heating alone, or to maintain a certain gradient of the temperature gradient for a certain period of time, for example, a temperature of 500 ° C to 1600 ° C. Gradient for a certain time.
  • the time for the heat preservation may be as needed, and may be several hours, ten hours or tens of hours or days, and the like.
  • the specific manner of temperature control is well known to those skilled in the art and can be carried out in various known ways, such as constant temperature heating and the like, which will not be described here.
  • the monitoring of the sample can be started at any time as long as sufficient phase change data of the sample to be tested can be obtained, wherein
  • the phase change refers to the change of the sample to be tested from solid to liquid or the change from the reverse liquid to the solid state, the data of the phase change of the sample to be tested, including the temperature data of the phase change, the time data, and the like.
  • the monitoring may start from the first step of the self-test method, start monitoring and collect data, or may start monitoring and collecting data after the temperature of the sample to be tested rises to a certain value. , can be determined according to specific needs. Further, for different samples to be tested, the continuous monitoring time will be different. To obtain enough data, the whole process may last for hours, ten hours, several days, and so on.
  • the method for monitoring the phase change of the sample on the carrier member during the heat treatment may be any method known in the art, for example, using a CCD (Charging Coupled Devi ce, CCD) photographic method, using X-ray diffraction, One or more of infrared spectroscopy, polarized light microscopy, and the like.
  • the sample can be continuously or periodically sampled by photographic method.
  • the sample should be scanned periodically.
  • the sampled results obtained by the monitoring are transmitted to the database in real time for analysis at the end of the experiment.
  • These monitoring methods are performed by instruments known in the art, such as CCD cameras, diffractometers, optical instruments, polarized microscopes, and the like.
  • the carrier member 900 is provided with a receiving groove of a 6 ⁇ 8 matrix arrangement, and each horizontal row 911, 912
  • the 913, 914, 915, and 916 include the same sample to be tested in the receiving slot.
  • the eight receiving slots respectively contain the same sample to be tested 901.
  • each horizontally arranged receiving groove at different positions is Different temperature values, while in the same longitudinal row (shown by the vertical dashed line in the figure, formed by the receiving grooves of different horizontal rows at the same longitudinal position), the different samples to be tested are at the same temperature, temperature monitoring
  • the device 91 monitors the temperature of the entire environment, and the image monitoring device 92 monitors the phase change and time of each sample monomer and records the data. Further, the processing data processing system for monitoring the obtained data mainly integrates and analyzes the recorded data and gives the desired results.
  • Data integration mainly involves extracting records of temperature records, time records, and sample phase changes from a database, and corresponding samples to specific rules.
  • a sample to be tested will have several samples in the direction along the temperature gradient, so the temperature record here includes the temperature of the sample to be tested at different temperature points.
  • the time record is consistent with the record of the phase monitoring, and a phase monitoring record corresponds to a time record.
  • the data analysis mainly analyzes the phase monitoring records, and records at the beginning of the phase change of the sample at a temperature point is a valid record, such as records with crystal appearance and records with liquid phase.
  • the effective record is extracted, and new data including temperature, time, phase change information, and the like is obtained.
  • the temperature, time, crystallization and phase change information of the sample are extracted from the data record, and the temperature and time are plotted as coordinates, and the sample point information at different temperatures recorded at different times can be obtained in the coordinate system.
  • the curve obtained by connecting the time points at which crystallization occurs at different temperatures is
  • T. T. T. curve The temperature at which the solid-liquid equilibrium exists at the end of the measurement is the liquidus temperature of the material system.
  • a T. T. T. curve of a plurality of sample systems can be obtained in one test. If the sample systems tested have the same composition and only the composition ratios are different, the phase diagram of the material system can be obtained by connecting the liquidus temperature points.
  • a T. T. T. chart of the material can be obtained by applying the subsequent steps of the test method of the present invention. If several samples can be divided into several groups, each of which is composed of a material different from the other groups, then the subsequent steps of the test method of the present invention can be used to obtain several materials at a time.
  • T. T. T. map For testing the test methods involved in the present invention, testing a material or testing a plurality of materials can be set by the operator. Further, for the overall form of several samples (for details, please refer to the foregoing), the test method involved in the present invention is more capable of testing a large number of materials composed of different components at one time, greatly speeding up the new one. The speed of research and development of materials.
  • the method for testing the phase change of the high-flux solid sample according to the present invention can also be applied to the accuracy of the TTT pattern of the different material samples detected.
  • TTT maps of 10 different samples are obtained, but the accuracy is not determined.
  • the method according to the present invention can be used for detection, and one material sample in each TTT image is taken as For the sample to be tested, 10 different samples to be tested are obtained, and 10 samples to be tested are heat-treated to respective predetermined temperatures, and phase change data of relevant temperature and time are recorded, and 10 different samples to be tested are respectively obtained.
  • the data of the phase transition point of a certain temperature, and then, the phase transition point data at a certain temperature of the different samples to be tested is returned to the TTT map of each sample to be tested, and the phase transition confirmed is confirmed. Whether the position of the point coincides with the position on the TTT map to be inspected, thus confirming the pending The accuracy of the TTT map.
  • the number of samples to be tested selected for detection may be one, or may be multiple, as needed. Therefore, the application of this method can test the ⁇ . ⁇ . ⁇ . diagram of several samples to be tested at one time, which greatly improves the efficiency and thus reduces the cost.
  • Yet another aspect of the present invention is to provide a sample testing system that can be used to test a plurality of samples, the technical solution of which is: a sample testing system including a carrier member, a heat treatment system, and a monitoring system, wherein the carrier member is used for carrying For several samples, a heat treatment system is used to heat treat these samples, and at the same time the heat treatment temperatures of at least two samples are different.
  • the monitoring system is used to monitor the heat treatment process and record the collected information.
  • the carrier member may be a carrier substrate composed of a high temperature resistant ceramic material or the like.
  • sample to be tested for example, several samples to be tested are composed of the same substance; or some samples to be tested are divided into different groups, and the constituent substances of the samples to be tested of each group are different from the other groups.
  • the sample to be tested corresponds to the sample testing system of the present invention, which can perform testing of a plurality of samples of a single class, and can also test a plurality of samples of a high-throughput multi-class.
  • Still another aspect of the present invention is to provide a test procedure for a plurality of samples, as shown in Fig. 11, which includes a sample preparation step, a sample placement step, a heating step, a temperature monitoring step, a sample monitoring step, and a data processing step. Further, it is also possible to increase the temperature maintaining step after the heating step. Further, it may further comprise, according to the obtained data, adding a test sample after the data processing step ⁇ . ⁇ . ⁇ .
  • the high-throughput sample testing method and system thereof disclosed in the present invention can perform testing on a plurality of samples at one time, and obtain sufficient data to obtain the properties of the samples. Its use is quite extensive.
  • the data obtained through testing can be used for glass materials. ⁇ . ⁇ . Rapid measurement of graphs; rapid determination of liquidus in glass materials; inorganic non-metals such as ceramics, refractories, steel materials, alloys, etc. Rapid determination of materials and metallic materials ⁇ . ⁇ . ⁇ .
  • FIG. 1 is a schematic view of a method for preparing a plurality of independent samples by high-throughput according to the present invention
  • FIG. 2A is a schematic view showing an embodiment of a plurality of samples according to the present invention
  • FIG. 2B is a view of a plurality of samples according to the present invention
  • 2C is a schematic view of still another embodiment of the overall form of the thousands of samples according to the present invention
  • FIG. 2D is a schematic view showing still another embodiment of the overall form of several samples according to the present invention
  • 3 is a schematic view of an embodiment of a carrying device according to the present invention
  • FIG. 4 is a schematic view of an embodiment of a method for carrying a sample of a carrier device according to the present invention
  • FIG. 5 is a schematic view showing still another embodiment of a method for carrying a sample of a carrier device according to the present invention
  • Figure 6 is a schematic illustration of one embodiment of heat treatment of a plurality of sample monomers placed on a carrier
  • Figure 7 is a schematic illustration of yet another embodiment of heat treating a plurality of sample monomers placed on a carrier
  • Figure 8A is a schematic illustration of one embodiment of heat treatment of the overall form of several samples placed on a carrier member
  • Figure 8B is a schematic illustration of yet another embodiment of heat treatment of the overall form of several samples placed on a carrier member
  • FIG. 9 is a schematic view of one embodiment of a test method for a high-throughput solid sample according to the present invention.
  • Figure 10 is a T. T. T. diagram of a sample drawn by data obtained by applying the detection method of the present invention.
  • Figure 11 is a flow chart of a sample test according to the present invention. detailed description
  • the first stage preparation of two glass samples
  • a substrate which is provided with two sample melting tanks, and a plurality of glass samples in a block shape are placed in the sample melting tank, and each sample tank has a small hole at the bottom, and a fine bottom is connected to the bottom of the hole.
  • the second step is to heat the sample tank to melt the sample block therein, and control the heating temperature so that the molten glass sample is dropped into the lower thin tube along the small hole at the bottom of the tank, and is solidified into a size in the thin tube. A uniform sample pellet.
  • the first step of drawing the prepared TTT pattern of the two glass samples the prepared two kinds of glass sample beads are placed on the substrate with the groove, wherein the groove The diameter is 5mm, the arrangement matrix is 2X8, and each row has 8 grooves for placing the same glass sample;
  • the substrate for carrying the sample is made of platinum material, the area of the substrate is 40cm 2 , and the thickness of the substrate is 2cm;
  • the substrate carrying the sample is placed in a space, protected by nitrogen, and then rapidly heated to the desired temperature; wherein one end of the substrate (left end) is heated by an infrared lamp, and the environment of the infrared lamp and the cavity is utilized.
  • the temperature is controlled so that the temperature of each row of the sample on the substrate changes linearly from 900 °C to 550 °C with a temperature interval of 50 per sample.
  • C from left to right, is 900 °C, 850 °C, 800 °C, 750 °C, 700. C, 650. C, 600. C, 550. C; the temperature on the substrate is uniform in a direction perpendicular to the temperature gradient, and the temperature monitoring of the entire system is monitored by an infrared thermometer;
  • the heating system is controlled to stabilize the substrate temperature; wherein the temperature sensitive temperature camera is used to monitor the temperature and temperature gradient of the substrate and the temperature at different positions is recorded; the crystallization and phase of the sample are performed by the CCD The situation is observed and recorded in real time; the sample is heated and kept for 12 hours, and the CCD monitors the crystallization and phase transition of the sample for 12 hours. The phase change and temperature information of each sample at different times are fixed. The rules are recorded;
  • the fourth step is to extract the temperature, time, crystallization and phase change information of the sample from the data record, and plot the temperature and time as coordinates.
  • the sample point information at different temperatures recorded at different times can be obtained.
  • TTT curves were obtained by joining the time points at which crystallization occurred at different temperatures.

Abstract

L'invention concerne un procédé pour détecter des échantillons. Selon ce procédé, les données relatives à un certain échantillon peuvent être obtenues simultanément à des températures différentes. En outre, sur la base de ces données, un diagramme TTT des échantillons peut être obtenu pour caractérisés certaines natures de l'échantillon. Le procédé de détection de la présente invention comprend les stades suivantes: 1) placer divers échantillons à détecter dans des régions prédéterminée d'un dispositif de support fourni; 2) effectuer le traitement à la chaleur des échantillons, de manière à régler la température pour toute la durée pour au moins deux échantillons; 3) et détecter les états des échantillons pour obtenir les données de transformation temps - température et enregistrer les données de manière à rendre le diagramme TTT des échantillons. L'application du procédé fourni permet d'accélérer la R & D d'un nouveau matériau.
PCT/CN2006/002350 2005-09-09 2006-09-11 Procede de detection a haut debit destine aux echantillons solides et systeme correspondant WO2007028344A1 (fr)

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US60/715,850 2005-09-09

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CN102162799A (zh) * 2011-04-06 2011-08-24 上海大学 金属熔体的速冻方法
CN111896595A (zh) * 2020-07-06 2020-11-06 天津大学 一种系统集成高通量制备和高通量电化学测试的方法

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JP2002214172A (ja) * 2001-01-12 2002-07-31 Matsushita Electric Ind Co Ltd ガラス試験方法
US6438497B1 (en) * 1998-12-11 2002-08-20 Symyx Technologies Method for conducting sensor array-based rapid materials characterization
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JP2001272365A (ja) * 2000-03-27 2001-10-05 National Institute For Materials Science ガラス熱物性評価方法およびガラス物性評価装置
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CN102162799A (zh) * 2011-04-06 2011-08-24 上海大学 金属熔体的速冻方法
CN111896595A (zh) * 2020-07-06 2020-11-06 天津大学 一种系统集成高通量制备和高通量电化学测试的方法
CN111896595B (zh) * 2020-07-06 2023-08-15 天津大学 一种系统集成高通量制备和高通量电化学测试的方法

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