• 专利附录
  • 专利说明
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    • 专利摘要:
    The present invention relates to a device (1) for the observation and in situ characterization of a sample (2) subjected to very high pressure and heated to a temperature of between 1300 K and 1900 K, including a CED (3). ) with diamond anvils (31, 32) arranged on seats (51, 52) resistant to high pressure and constituting a high temperature thermal insulator, this CED (7) being associated with an induction heating mode (7) at least one turn (730).
    公开号:FR3081222A1
    申请号:FR1854066
    申请日:2018-05-15
    公开日:2019-11-22
    发明作者:Philippe Rosier；Pascal Munsch
    申请人:Centre National de la Recherche Scientifique CNRS；Museum National dHistoire Naturelle；Universite de Limoges；Institut de Recherche pour le Developpement IRD；Sorbonne Universite；
    IPC主号:
    专利说明:

    DEVICE FOR IN SITU OBSERVATION AND CHARACTERIZATION
    SAMPLES IN EXTREME CONDITIONS OF TEMPERATURE AND
    PRESSURE AND INSTALLATION COMPRISING SUCH A DEVICE
    TECHNICAL AREA
    The present invention relates to the field of diamond anvil cells (usually designated by the acronym CED) and to their use for the observation and in situ characterization of samples of materials under extreme conditions of temperature and pressure.
    STATE OF THE ART
    Experimentation in extreme conditions of pressure and temperature is an essential approach for the understanding of several processes in the fields applied to industry and to those of fundamental research, whether in Physical Sciences (study of condensed matter and ultra-hard materials) or in Earth Sciences (study of planetary interiors, experimental petrology and volcanological manifestations). For several decades, experimental tools have been developed to reproduce in the laboratory different pressure and temperature conditions relevant to their studies.
    Among the various devices, the diamond anvil cell (CED) uj-uj is to date the most versatile and efficient characterization device. Existing in many versions [4] , this tool makes it possible to reach a very wide range of static pressure (up to several hundred GPa) and temperature, which can go up to a few thousand Kelvin when this tool is coupled to a laser heating type device. An advantage of CED is the transparency of diamonds in a very wide spectral range, ranging from far infrared to hard X-rays: this allows observation and characterization, in situ and in real time, of the transformation process from materials to using a wide variety of investigative methods using laboratory techniques (eg Raman, FTIR, Brillouin) or sources of synchrotron radiation.
    There are currently two main types of heating for CEDs, namely external heating, generally resistive, and internal heating using a 1101 power laser.
    Resistive external heating makes it possible to obtain a homogeneous heating but limited to approximately 1300 K. Thus, if a resistive heating sleeve (for example based on graphite) is used for this around the CED or around the diamonds, this sleeve only works reproducibly up to 700 K (if it is around the CED) or 1300 K (if it is around the diamonds). On the other hand, internal heating by power laser makes it possible to reach several thousand K, but has intrinsic limits in terms of thermal gradients, temporal stability and metrology for temperatures below 1700 K.
    Consequently, he follows than range of temperatures between 1300 and 1900 K is not of facto covered, because of the difficulties linked at the temperature generation and from 1 ' absence of a precise metrology.
    However, many fundamental natural processes occur at high pressure precisely in this range of temperatures. Thus, for example in the case of magmas, surface lavas have temperatures up to 1600 K and deep magmas are more than 1500 K. The transition zone (410-660 km) inside the Earth , which is a region of central importance for the understanding of mantle processes, is characterized by temperatures between 1500 K and 1700 K [1 U. Experimentation at high pressure in this temperature range is also of the greatest interest in planetology because it corresponds to that estimated for the deep coats and the nuclei of small telluric planets or of the Moon (between 1300 and 1900 K) [1 2 ]. In materials science, the field between 1300 K and 1900 K is particularly relevant for the processes of fusion and synthesis of several materials with remarkable properties.
    In fundamental physics, this temperature domain is very relevant for the study of the liquid phases of alkaline elements (in particular, Li and Na) and molecular compounds (like CO2 [13] and H2O).
    Furthermore, tungsten carbide seats are traditionally used in CEDs on which the diamond anvils are placed. However, these seats degrade in the envisaged temperature range (1300 K to 1900 K). If zirconia seats were used instead, these would be thermal insulators up to around 1400 K, and would not withstand high pressure at such a high temperature.
    DESCRIPTION OF THE INVENTION
    To resolve these defects and drawbacks, the applicant has developed a device allowing the observation and characterization in situ of a sample subjected to very high pressure and heated to a temperature between 1300 K and 1900 K, comprising a cell to diamond anvils arranged on seats resistant to high pressure and constituting a thermal insulator at high temperature, this
    CED being associated with an induction heating mode, chosen for its efficiency and simplicity of integration [1 4].
    More particularly, the present invention therefore relates to a device for the observation and in situ characterization of a sample when it is subjected to very high pressures and heated to a temperature between 1300 K and 1900 K, said device including:
    a diamond anvil cell comprising:
    at least one seal comprising essentially planar rhenium and pierced in its center to form the side walls of a high pressure chamber, said seal having an upper planar face and a lower planar face coming into contact with two diamond anvils which are each fixed in a ceramic seat, said anvils being identical and each comprising a head having a cylinder head (face in contact with the sample), said anvils being arranged symmetrically with respect to said joint so that each of the cylinder heads is in contact respectively with the upper and lower flat faces of said seal and hermetically seal said high pressure chamber when said anvils are pressurized, means for pressing the diamonds against each other comprising a substantially cylindrical body and containing said anvils and said seal and a capillary membrane capable of transmitting a tightening force age on said anvils, so as to apply a pressure which can go up to 100 GPa (typically of the order of 20 to 50 GPa) in the high pressure chamber, means for guiding said anvils in said body;
    means for heating the sample, and means for cooling disposed in or at the outer periphery of said body;
    said device being characterized in that said ceramic seats are made of silicon nitride and alumina (ceramic usually designated by the acronym SiAlON), and in that said heating means comprises:
    • said joint comprising rhenium, • two plates or stacks of plates of molybdenum or rhenium, which are each pierced in their center so as to surround the head of said diamond anvils, and are in direct contact with said rhenium joint and the diamonds, and • an inductor with at least one turn surrounding said plates or stacks of plates.
    By very high pressure is meant, within the meaning of the present invention, a pressure between several tens of MPa and 100 GPa.
    The seats in silicon nitride and alumina (or SiAlON) make it possible to combine mechanical strength under high pressure and thermal insulation at high temperature (above 1300 K).
    Induction heating using the inductor is simple to integrate into the device according to the invention and efficient and stable in the temperature range 1300 K-1900 K. The means of heating the device according to the invention is suitable for operating under vacuum, and in particular in high vacuum between 10 ~ 5 mbar and 10 ~ 6 mbar.
    Advantageously, the plates or stacks of plates can each have a thickness of between 0.2 mm and 0.6 mm.
    Advantageously, the joint comprising rhenium may have a thickness of between 0.1 mm and 0.4 mm, preferably of the order of 0.2 mm.
    Advantageously, the joint comprising rhenium can be surrounded by a ring of ceramic material resistant to high temperature.
    Advantageously, the joint comprising rhenium can be a composite joint comprising an external part made of rhenium and a central part made of a material chosen from cubic boron nitride (CBN) [1 sj, a compound based on kapton, boron amorphous and epoxy resin [16] , or rhenium diboride [1 7].
    Advantageously, the high pressure chamber can be a cylindrical chamber having a height of between 10 μm and 60 μm and a diameter of between 10 μm and 500 μm.
    Advantageously, the cooling means can be in the form of a ring, in which a cooling fluid such as water circulates, this ring being arranged around said diamond anvil cell (CED). One can also use perfluorohexane CgF ^ as heat transfer fluid.
    The present invention also relates to an installation for the observation and in situ characterization of a sample when it is subjected to very high pressure and heated to a temperature between 1300 K and 1900 K, said installation comprising:
    • a vacuum chamber provided with at least one porthole containing the device according to the invention and the heating means, in which the inductor passes through a vacuum-tight ceramic flange passing through said body of said anvil cell diamond (CED), and • a pressure generator for putting the membrane of the device according to the invention under very high pressure, • a vacuum pump connected to the vacuum chamber, which is capable of producing a vacuum up to 10 ~ 6 mbar, and • a means for observation and / or in situ characterization of the sample.
    By pressure generator is meant, in the sense of the presentation, a device capable of generating a pressure between 0 and 200 bars, such as for example a compressor or an inflator.
    The vacuum chamber of the installation according to the invention makes it possible to create an atmosphere free of oxygen in high vacuum, between 10 ~ 5 mbar and 10 ~ 6 mbar, which avoids the graphitization of the diamond above 1400 K and the deterioration by oxidation of the ceramics present in the device according to the invention (in particular the seats, or where appropriate the ring made of ceramic material surrounding the joint).
    The heating means of the device according to the invention is adapted to operate under vacuum, and in particular in high vacuum between 10 ~ 5 mbar and 10 ~ 6 mbar.
    As means for the observation and / or the in situ characterization of the sample which can be used in the installation according to the invention, it is in particular possible to use a diffractometer, a spectrometer, an infrared pyrometer or a synchrotron-type instrument.
    Preferably use an infrared pyrometer positioned above the porthole of the vacuum chamber.
    Other advantages and particularities of the present invention will result from the description which follows, given by way of nonlimiting example and made with reference to the appended figures and to the corresponding examples:
    Figure 1 shows a schematic sectional view of an exemplary device according to the invention;
    Figure 2 shows a detailed sectional view of the CED of the device of Figure 1 showing in particular the heating means;
    Figure 3 shows a schematic top view of the device according to the invention illustrated in Figure 1;
    FIG. 4 represents a schematic sectional view of an example of installation according to the invention, showing in particular the CED associated with the heating and cooling means;
    FIG. 5 represents a schematic sectional view of an example of installation according to the invention, showing in particular the vacuum chamber;
    FIGS. 6A and 6C are photographs taken at ambient temperature of a diamond anvil of the CED of the installation according to the invention, these photographs having been taken before heating (FIG. 6A) and after heating (FIG. 6C), FIG. 6B is a video image of a diamond anvil taken in situ during an induction heating test at 1400 ° C (1673.15 K) using the installation according to the invention and recorded with the pyrometer ;
    Figure 6D is a photograph of a anvil diamond of the CED of 1'installation according to 1'invention, who has summer taking at room temperature
    after graphitization at 1400 ° C (1673.15 K) under noxal, while FIG. 6E (video image taken by the pyrometer) shows that the pyrometric aiming through this graphitized diamond is not possible;
    FIG. 7A is a video image obtained with an infrared pyrometer during an induction heating test at 1767 ° C (2040.15 K) of a platinum sample, under a vacuum of 10 ~ 5 mbar (example 2) ; Figure 7B shows a photograph of the platinum sample of Figure 7A when fused observed at room temperature;
    FIG. 8A is a video image obtained with an infrared pyrometer during an induction heating test at 1300 ° C. (1573.15 K) of a sample of inconel 718, under a vacuum of 10 ~ 5 mbar (example
    3);
    Figure 8B shows a photograph of the platinum sample of Figure 8A when melted observed at room temperature;
    Figures 9 and 10 are curves showing the evolution of the temperature as a function of time during a vacuum induction heating test using the installation according to the invention, with a rhenium seal between the two diamond anvils (figure 9) and with a stack of three rhenium joints between the two diamond anvils (figure 10).
    Identical elements shown in Figures 1 to 5 are identified by identical reference numerals.
    Figures 6 to 9 are described in more detail in the examples which follow, which illustrate the invention without limiting its scope.
    DESCRIPTION OF AN EMBODIMENT OF THE DEVICE ACCORDING TO THE INVENTION
    FIG. 1 shows a schematic sectional view of an example of a device 1 according to the invention for the observation and characterization in situ of a sample 2 when it is subjected to very high pressure and heated to a temperature between 1300 K and 1900 K. FIG. 1 shows in particular that the device 1 comprises:
    a cell 3 with diamond anvils (CED), a heating means 71, 72, 73 of the sample 2, and a cooling means 8 (visible in the figure
    4) disposed in or at the outer periphery of the body 101 of the CED 3 (visible in FIGS. 1 and 3).
    Figures 1 to 4 show in particular that cell 3 with diamond anvils (CED) comprises:
    at least one seal comprising rhenium 30 (visible in FIGS. 2 and 3), which essentially plane and pierced in its center to form the side walls of a high pressure chamber 4 (visible in FIG. 2), the seal 30 having an upper planar face 301 and a lower planar face 302 in contact with two identical diamond anvils 31, 32 which are each fixed in a seat 51, 52 (visible in FIGS. 1 to 3), these anvils 31, 32 each comprising a head 310, 320 having a yoke (face in contact with the sample) and being arranged symmetrically with respect to the joint 30 so that each of the yokes of the heads 310, 320 are in contact respectively with the upper planar faces 301 and lower 302 of the seal 30 and seal the high pressure chamber 4 hermetically when the anvils 31, 32 are pressurized, means for pressing the diamonds 31, 32 against each other.
    As regards more particularly the joint comprising rhenium 30 (visible in FIGS. 2 and 3), a joint is used whose thickness is of the order of 0.2 mm. In the context of the present example, the joint 30 is a composite joint comprising an outer part 304 of rhenium and a central part 303 of a material chosen from cubic boron nitride (CBN), rhenium diboride or a compound based on kapton, amorphous boron and epoxy resin. This seal is surrounded by a ring 33 of ceramic material resistant to high temperature, which allow when a very high pressure is applied to the chamber 4 at high pressure, to keep the anvils 31, 32 in contact with the plates 71, 72 in molybdenum or rhenium of the heating medium (see below).
    With regard more particularly to the diamond anvils 31, 32, diamonds are generally used whose size is adapted to the CEDs, having a cylinder head which is truncated either by a flat face, as illustrated in FIGS. 1 and 2, or bevelled on two slopes. In the context of this embodiment, advantageously use diamonds of Almax-Boehler geometry. Each of these anvils 31, 32 is fixed in a seat 51, 52 in S1A1ON, for example marketed under the trade name Syalon 050 by International Syalons.
    As regards more particularly the means for pressing the diamonds 31, 32, these comprise • a substantially cylindrical body 101 (visible in FIG. 1) which contains the anvils 31, 32 of the CED 3 and the joint 30, and • a capillary membrane 102 resting on a wedge 103 (visible in FIG. 1) and capable of transmitting a clamping force on the anvils 31, 32 via a shrouded plate 106 (hoop 107: plate and hoop visible in FIG. 1) pressing on the upper anvil 31 of the CED 3 (see FIG. 2) and a hooped ball joint 109 (hoop 108: ball joint and hoop visible in FIGS. 1 and 3) on which the lower anvil 32 of the CED 3 is arranged, and • means 61 for guiding the anvils 31, 32 in the body 101 consisting of an alignment rod passing through the ball joint 109 and the plate 106 for aligning the anvils 31, 32 in the CED 3.
    FIG. 2 shows a schematic sectional view of the heating means 71, 72, 73 of the CED 3. This comprises, in addition to the seal 30 comprising rhenium:
    • two plates 71, 72 of molybdenum or rhenium each having a thickness of between 0.2 mm and 0.6 mm, these plates 71, 72 being pierced in their center so as to surround the head 310, 320 of the diamond anvils 31, 32, and are in direct contact with the rhenium seal 30 and the diamond diamond anvils 31, 32, and • an inductor 73 with at least one turn 730 of 18 mm in diameter surrounding the plates 71, 72.
    FIG. 4 shows a schematic sectional view of the means of the cooling means 8, which is in the form of a ring 8, in which water circulates, this ring being arranged around the CED 3.
    DESCRIPTION OF A MODE OF CARRYING OUT THE INSTALLATION ACCORDING TO
    THE INVENTION
    Figures 4 and 5 are schematic sectional views of an example of installation according to the invention, Figure 4 showing in particular the CED 3 associated with the heating means 71, 72, 73, 74 and cooling 8 and the FIG. 5 showing in particular the vacuum chamber 9. These two figures show that this example of installation according to the invention comprises:
    a vacuum chamber 9 provided with a front porthole 91 (FIG. 5 showing more precisely the housing of the front porthole 91) and a rear porthole 92, this vacuum chamber 9 containing the device 1 as illustrated in the Figures 1 to 3 associated with inductor 73 passing through a ceramic flange 74, vacuum tight and passing through the body 101 of the CED 3, the ceramic flange 74 with inductor 73 being connected to an induction head 76 via an inductor holder 75: the CUBE 64 5.6 kW HIGH PERFORMANCE generator with a 64 SERIE 900 heating head will be used in the following examples as an induction generator; and • a pressure generator (not visible in FIGS. 4 and 5) for placing the capillary membrane 10 of the device 1 under very high pressure;
    • a vacuum pump (not visible in Figures 4 and
    5) connected to said vacuum chamber 9 capable of producing a vacuum up to 10 -6 mbar, and • an infrared pyrometer (not visible in the figures and 5) positioned above the porthole 91.
    EXAMPLES
    EXAMPLE 1 Start-up of the installation according to the invention
    The installation according to the invention illustrated in FIGS. 4 and 5 is used without the CED 3, in which a high vacuum is produced in the chamber 9 at 1.5 × 10 -5 mbar. It is possible to take measurements under vacuum at 10 -4 mbar in ten minutes and at 10 -5 mbar in less than 2 hours.
    A crucible in shapal on a pyrophilite washer is inserted in the center of the coil 73. A 5x5 mm 2 joint of Rhenium serves as a heating element by reacting to the induction. Induction was tested up to 1780 ° C (2053.15 K) on the rhenium vacuum joint.
    EXAMPLE 2 Study of the non-graphitization of diamonds
    Induction heating tests are carried out at 1400 ° C. (1673.15 K) in the installation according to the invention without the CED 3 (as in example 1), in which a cut diamond of Almax geometry is placed. Boehler on a rhenium joint in the installation according to the invention. These tests are illustrated by FIGS. 6A to 6E:
    FIG. 6A shows the diamond before heating: of yellowish appearance, the facets are clearly visible from the cylinder head.
    During heating, the video image clearly shows the color of the rhenium seal through the diamond (Figure 6B). The latter is therefore not opaque;
    Figure 6C confirms with the naked eye what we see with the pyrometer, the diamond is very transparent.
    For these tests, the cumulative heating time is one hour, with a vacuum level maintained between 1.5 and 3.1CU 5 mbar.
    In chamber 9, the same brightness and the same transparency of the lamp reflection on the rhenium seal are observed.
    We observe that there was no total graphitization of the diamond at 1400 ° C (1673.15 K) at this vacuum level, nor even a graphite veil that could interfere with optical operation.
    An example of an opaque diamond (obtained after graphitization at 1400 ° C ((1673.15 K) under noxal) is shown in Figure 6D, Figure 6E shows that it is impossible to make a pyrometric sight through this diamond.
    EXAMPLE 3: Calibration of the pyrometer
    We use an OPTRIS CTV 2MH1 CFV CB3C infrared pyrometer with an integrated video output. This pyrometer can read the temperature from 490 ° C to 2000 ° C (i.e. between 763.15 K and 2273.15 K) on metal bodies at a focal distance of 100 mm and over an area of 0.3 mm in diameter.
    In order to calibrate the pyrometer, we have, in the crucible in shapal on a rhenium joint in the center of the coil 73, different metal samples, which we heat until they reach their melting point:
    up to 1085 ° C (1358.15 K), by visualizing the fusion of a piece of copper, up to 1335 ° C (1608.15 K) by visualizing the fusion of a piece of Inconel 718, as illustrated in FIGS. 8A and 8B, and up to 1768 ° C (2041.15 K) by visualizing the melting of the platinum, as illustrated in FIGS. 7A and 7B.
    This made it possible to define the emissivity coefficient at 0.3 for the Rhenium joint.
    EXAMPLE 4
    Vacuum induction heating tests are carried out using the installation according to the invention, with a rhenium joint between the two diamond anvils (FIG. 9) and with a stack of three rhenium joints between the two anvils diamond (figure 10).
    Induction acts on conductive materials. The greater the volume of the heating means, the greater the power deposited on these ovens by induction.
    Thus we see that with a single rhenium joint between the diamond anvils (see Figure 9), the power applied to the rhenium joint 30 is quite low since it takes 600 seconds to reach 1600 ° C (1873.15 K ), with a power that is set on the generator of 100%. Despite this, we still manage to reach our goal.
    With three seals (see Figure 10), the power applied to the rhenium 30 seal is then much greater since it takes only 200 seconds to reach 1600 ° C (1873.15 K), with only 80% of set power on the generator. This therefore leaves a safety margin on the installation.
    The curves in FIGS. 9 and 10 also show that the temperature rise is fairly rapid (200 seconds), which opens up prospects in fundamental research, in particular relating to the study of materials in thermal cycling under high pressure.
    REFERENCES [1] Weir C.E., et al. (1959) J. Res. Nat. Off. Standards (US) 63A, 55-62.
    [2] Jamiesen J.C. et al. (1959), Rev. Salt. Instr. 30, 10161019.
    [3] Van Valkenburg A. (1964) Diamond Research 1964, 17-20.
    [4] Bassett W.A. (2009) High Pressure Research, 29, 163-186 [5] Bassett W.A. (2003) Eur. J. Mineral., 15, 773-780.
    [6] Burchard et al., (2003) Rev Sci. Instr. 74, 1263.
    [7] Petitgirard S. et al. (2009) Rev. Sci. Instr. 80, 033906.
    [8] Pasternack S. et al. (2008) Rev. Sci. Instr. 79, 085103.
    [9] Munsch P. et al. (2015) Eur. J. Miner. 27, 365-375.
    [10] Tateno S. et al. (2010) Phys. Earth and Planet. Int. 181, 54-59.
    [11] Frost D.J. (2008) Elements 4, 171-176.
    [12] Antonangeli et al., (2015) PNAS 112 (13), 3916-3919.
    [13] Datchi et al. (2016) Phys. Rev. B94.014201 [14] Keiji Shinoda et al. (2008) AIP, Rev. Sci. Instr. 79, 015101 [15] Lobanov et al (2015) J. Appl. Phys. 118, 035905 [16] S. Merkel & T. Yagi Rev. Sci. Instrum., 76, 046109 (2005) [17] Hsiu-Ying Chung et al (2007) Science 316, 436
    权利要求:
    Claims (9)
    [1" id="c-fr-0001]
    1. Device (1) for the observation and characterization in situ of a sample (2) when it is subjected to very high pressure and heated to a temperature between 1300 K and 1900 K, said device (1) comprising :
    a diamond anvil cell (3) comprising: at least one seal comprising rhenium (30) essentially planar and pierced in its center to form the side walls of a high pressure chamber (4), said seal (30) having an upper planar face (301) and a lower planar face (302) coming into contact with two diamond anvils (31, 32) which are each fixed in a seat (51, 52) made of ceramic, said anvils (31, 32 ) being identical and each comprising a head (310, 320) having a yoke (face in contact with the sample), said anvils (31, 32) being arranged symmetrically with respect to said joint (30) so that each of the yokes of said heads (310, 320) are in contact respectively with the upper planar (301) and lower (302) faces of said seal (30) and hermetically seal said high pressure chamber (4) when said anvils (31, 32) are placed under pressure, means for pressing the s diamonds (31, 32) against each other comprising a body (101) substantially cylindrical and containing said anvils (31, 32) and said seal (30) and a capillary membrane (102) capable of transmitting a force of clamping on said anvils (31, 32), so as to cause a pressure of up to 100 GPa in the high pressure chamber (4) to prevail, means for guiding (61) of said anvils (31, 32) in said body ( 101);
    means for heating (71, 72, 73) of said sample (2), and cooling means (8) disposed in or at the outer periphery of said body (101);
    said device (1) being characterized in that said ceramic seats (51, 52) are made of silicon nitride and alumina, and in that said heating means (7) comprises:
    • said joint (30) comprising rhenium, • two plates (71, 72) or stacks of molybdenum or rhenium plates, which are each pierced at their center so as to surround the head (310, 320) of said diamond anvils (31, 32), and are in direct contact with said rhenium seal (30) and the diamonds, and • an inductor (73) to at least one turn (730) surrounding said plates (71, 72) or stacks of plates.
    [2" id="c-fr-0002]
    2. Device (1) according to claim 1, characterized in that the plates (71, 72) or stacks of plates each have a thickness between 0.2 mm and 0.6 mm.
    [3" id="c-fr-0003]
    3. Device (1) according to claims 1 or 2, characterized in that said seal (30) comprising rhenium present between 0.1 mm and 0.4 mm, preferably of the order of 0.2 mm.
    [4" id="c-fr-0004]
    4. Device (1) according to any one of claims 1 to 3, characterized in that said seal (30) comprising rhenium is surrounded by a ring (33) of ceramic material resistant to high temperature.
    [5" id="c-fr-0005]
    5. Device (1) according to any one of claims 1 to 4, characterized in that said seal (30) comprising rhenium is a composite seal has an outer part (304) in rhenium and a central part (303) in a material chosen from cubic boron nitride, rhenium diboride or a compound based on kapton, amorphous boron and epoxy resin.
    [6" id="c-fr-0006]
    6. Device (1) according to any one of claims 1 to 4, characterized in that said high pressure chamber (4) is a cylindrical chamber having a height between 10 pm and 60 pm and a diameter between 10 pm and 500 pm.
    [7" id="c-fr-0007]
    7. Device (1) according to any one of claims 1 to 3, characterized in that said cooling means (8) is a ring in which circulates a cooling fluid (81), said ring (8) being arranged around of said cell (3) with diamond anvils (CED)
    [8" id="c-fr-0008]
    8. Installation for the observation and characterization in situ of a sample (2) when it is subjected to very high pressure and heated to a temperature between 1300 K and 1900 K, said installation comprising:
    • a vacuum chamber (9) provided with at least one window (91) containing a device (1) as defined in any one of claims 1 to 7 and said heating means (7), in which the inductor passes through a vacuum-tight ceramic flange (74) passing through said body (101) of said cell (3) with diamond anvils (CED), and • a pressure generator for placing under very
    5 high pressure of the membrane (10) of said device (D, • a vacuum pump connected to said vacuum chamber (9) capable of producing a vacuum up to 10 ~ 6 mbar, and • a means for observation and / or the
    10 in situ characterization of the sample (2).
    [9" id="c-fr-0009]
    9. Installation according to claim 8, according to which said means for the observation and / or the characterization of the sample (2) is an infrared pyrometer positioned above the window (91).
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    同族专利:
    公开号 | 公开日
    FR3081222B1|2020-06-12|
    WO2019220032A1|2019-11-21|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US5154551A|1991-02-11|1992-10-13|Gte Valenite Corporation|Adjustable boring bar|
    WO2021108871A1|2019-12-06|2021-06-10|Centro Nacional De Pesquisa Em Energia E Materiais - Cnpem|Compression device, compression process, method for producing synthetic materials and method for characterizing a sample|
    CN111175119A|2020-01-15|2020-05-19|吉林大学|Insulation method for metal gasket in diamond anvil cell|
    法律状态:
    2019-05-29| PLFP| Fee payment|Year of fee payment: 2 |
    2019-11-22| PLSC| Search report ready|Effective date: 20191122 |
    2020-05-27| PLFP| Fee payment|Year of fee payment: 3 |
    2021-05-28| PLFP| Fee payment|Year of fee payment: 4 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1854066A|FR3081222B1|2018-05-15|2018-05-15|DEVICE FOR THE IN SITU OBSERVATION AND CHARACTERIZATION OF SAMPLES IN EXTREME CONDITIONS OF TEMPERATURE AND PRESSURE AND INSTALLATION COMPRISING SUCH A DEVICE|
    FR1854066|2018-05-15|FR1854066A| FR3081222B1|2018-05-15|2018-05-15|DEVICE FOR THE IN SITU OBSERVATION AND CHARACTERIZATION OF SAMPLES IN EXTREME CONDITIONS OF TEMPERATURE AND PRESSURE AND INSTALLATION COMPRISING SUCH A DEVICE|
    PCT/FR2019/051007| WO2019220032A1|2018-05-15|2019-04-30|Device for observation and in situ characterisation of samples under extreme temperature and pressure conditions, and installation comprising such device|
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