Classifications

• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
  • C23C14/34—Sputtering
  • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
  • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
  • C23C14/228—Gas flow assisted PVD deposition
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B82—NANOTECHNOLOGY
  • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
  • B82Y40/00—Manufacture or treatment of nanostructures
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/32—Gas-filled discharge tubes
  • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
  • H01J37/3402—Gas-filled discharge tubes operating with cathodic sputtering using supplementary magnetic fields
  • H01J37/3405—Magnetron sputtering
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/32—Gas-filled discharge tubes
  • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
  • H01J37/3402—Gas-filled discharge tubes operating with cathodic sputtering using supplementary magnetic fields
  • H01J37/3405—Magnetron sputtering
  • H01J37/3408—Planar magnetron sputtering
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/32—Gas-filled discharge tubes
  • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
  • H01J37/3411—Constructional aspects of the reactor
  • H01J37/3435—Target holders (includes backing plates and endblocks)
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/32—Gas-filled discharge tubes
  • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
  • H01J37/3411—Constructional aspects of the reactor
  • H01J37/345—Magnet arrangements in particular for cathodic sputtering apparatus
  • H01J37/3452—Magnet distribution
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/32—Gas-filled discharge tubes
  • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
  • H01J37/3411—Constructional aspects of the reactor
  • H01J37/345—Magnet arrangements in particular for cathodic sputtering apparatus
  • H01J37/3458—Electromagnets in particular for cathodic sputtering apparatus
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/32—Gas-filled discharge tubes
  • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
  • H01J37/3411—Constructional aspects of the reactor
  • H01J37/3461—Means for shaping the magnetic field, e.g. magnetic shunts

Definitions

• the invention relates to a device for producing nanoparticles.
• the invention also relates to a method for depositing nanoparticles.
• the synthesized particles often have sizes 0 less than 100 nm and preferably between 1 and 20 nm.
• a conventional nanoparticle production device comprises a target 1.
• the target 1 preferably has a plate shape, and is made of a material from which atoms will be torn out so as to generate the nanoparticles.
• the face of the target from which the atoms are torn off is called the source face 1a nanoparticles.
• the target 1 is mounted on a magnetron 2, and the source face 1 of the nanoparticles is opposite the magnetron 2.
• a sputtering gas is used during the generation of the nanoparticles. Therefore, the production device may also include a cooled enclosure in which are disposed the target 1 and the magnetron 2.
• the target 1 and the magnetron 2 of Figure 1 then form an element also called sputtering element.
• a magnetron 2 comprises, as in FIG. 1, a cathode 3 at the rear of which magnets 4a, 4b are arranged.
• a first magnet 4a may have the shape of a hollow cylinder and a second magnet 4b may have the shape of a hollow cylinder, or full, inserted into the hollow cylinder of the first magnet 4a.
• the polarities of the first and second magnets 4a, 4b are reversed.
• One of the poles of the first magnet 4a is oriented towards the cathode 3
• one of the poles of the second magnet 4b is oriented towards the cathode 3, preferably the two poles mentioned are in contact with the cathode 3.
• the target 1 is in direct contact with the cathode 3 on one face of the cathode 3 opposite the face in contact with the magnets 4a, 4b.
• the magnetron 2 comprises a compression element 5 of soft iron.
• This element 5 of soft iron is intended to trap the field lines of the magnetic field generated by the magnets 4a, 4b of the magnetron 2 on its rear face 2a (the front face being defined by the face of the cathode 3 bearing the target 1) , and in the particular case of Figure 1 to pass from the first magnet 4a to the second magnet 4b or vice versa.
• the magnetic field comprises outgoing C field lines of the target 1 before retracing it.
• the magnetron 2 further comprises an anode 6 radially surrounding the magnet / element 5 of soft iron and cathode 3.
• WO95 / 12003 discloses a device for producing particles from a target. Magnets are mounted in a cathode. A target of ferromagnetic material is mounted on the cathode. A magnetic shunt is made by iron elements.
• the object of the invention is to provide a device for producing nanoparticles whose performance of pulverized nanoparticles is improved.
• a magnetron generating a first magnetic field
• the target being mounted on the magnetron and the first magnetic field forming field lines at the source face of the nanoparticles
• balancing means the first magnetic field at the target, arranged to close fleeing field lines of the first magnetic field and maintain said lines closed at said source face of the nanoparticles, said balancing means being separate magnetron and arranged so that the first magnetic field on the source side has a minimum value B min and a maximum value B max , the dispersion of the first magnetic field defined by the formula being less than 0.5.
• the balancing means comprise a plate provided with a ferromagnetic element, said plate being arranged between the target and the magnetron.
• the plate may comprise at least one material selected from Fe, Co, Ni, Mn.
• the balancing means comprise a magnetic coil generating a second magnetic field, said magnetic coil being controlled by control means comprising a state in which the leaky field lines of the first magnetic field are closed, said lines being maintained at said source face.
• the absolute value of the difference between B min and B max is less than 5 * 10 -2 Tesla
• the device comprises a temperature measurement sensor arranged facing the source face.
• the invention also relates to a use of a device for producing nanoparticles in a nanoparticle deposition device.
• the device for producing nanoparticles may comprise an enclosure in which the magnetron, the target and the balancing means are disposed, said enclosure comprising an arrival of a sputtering gas and an outlet orifice of the nanoparticles.
• the deposition device comprises a first chamber in which the outlet orifice of the enclosure opens, and a second chamber provided with a nanoparticle deposition substrate, the first chamber communicating with the second chamber through a hole, and said second chamber chamber being in depression with respect to the first chamber.
• the invention also relates to a method for depositing nanoparticles using a magnetron on which is mounted a target provided with a nanoparticle source face, the magnetron generating a magnetic field forming field lines at the source face of the nanoparticles.
• the method comprises a step of adjusting the magnetic field of closing off leaking field lines of the magnetic field and maintaining said lines closed at said nanoparticle source face, the adjustment being made by balancing means separate from the magnetron so that after adjustment the magnetic field on the source face (1a) of the target has a minimum value B min and a maximum value B max , the dispersion of the magnetic field defined
• FIG. 1 illustrates a device for producing nanoparticles as seen in section according to the prior art.
• FIG. 2 illustrates a device for producing nanoparticles, seen in section according to a first embodiment.
• FIG. 3 illustrates a sectional view along A-A of FIG. 2.
• FIG. 4 illustrates a device for producing nanoparticles seen in section according to a second embodiment.
• Figure 5 illustrates a combination of the first and second embodiments.
• Figure 6 illustrates a particular implementation of the device for producing nanoparticles.
• Figure 7 illustrates a plot of the probability of nucleation of nanoparticle seeds as a function of temperature.
• FIG. 8 illustrates a curve representative of the temperature as a function of the distance away from the target.
• Figure 9 illustrates a device for depositing nanoparticles.
• Figure 10 illustrates the evolution of the temperature as a function of the distance of the target for a modified device and a standard device. DESCRIPTION OF PREFERRED EMBODIMENTS The device described below differs from those of the prior art in that it comprises means for balancing the magnetic field at the target.
• a magnetron according to the prior art is not intrinsically balanced, and is rather unbalanced.
• unbalanced means that the magnetic field at the target has leaking field lines Ct (see Figure 1).
• These leaking field lines C f are in fact lines coming out of the target 1, moving away from the target 1 without going back there.
• the greater the magnetron was unbalanced that is, the more the field lines leaked) the lower the efficiency of the nanoparticle deposition.
• the device for producing nanoparticles comprises a target 1 provided with a source face 1a of the nanoparticles, and a magnetron 2 generating a first magnetic field.
• the target is mounted on the magnetron 2.
• the source face 1 has nanoparticles is opposed to a mounting face of the target 1, the mounting face being oriented towards the magnetron 2.
• the first magnetic field forms C-field lines at the source face 1a of the nanoparticles.
• Balancing means the first magnetic field at the target 1, are arranged to close leaking field lines of the first magnetic field and maintain said lines closed at said source face 1a nanoparticles.
• These balancing means are distinct from the magnetron 2. Separate from the magnetron is notably distinct from the magnets generating the first magnetic field.
• the level of the source face of the target is meant as illustrated in FIG. 2 that the field lines come out and re-enter, through the source face 1a of the nanoparticles, into the target 1 while remaining close to said source face 1a of the target 1.
• field lines C project from the target 1, and remain close to its surface, whereas without the balancing means, some of these field lines would become elusive.
• the magnetron 2 may comprise a cathode 3 and a compression element 5 of the field lines, for example of soft iron, sandwiching magnets 4a, 4b.
• a first magnet 4a may have the shape of a hollow cylinder
• a second magnet 4b may have the shape of a cylinder which is also hollow, or alternatively solid, inserted into the hollow cylinder of the first magnet 4a, as illustrated in particular in the figure
• the two poles mentioned are in contact with the cathode 3.
• the poles opposite to those in contact with the cathode 3 are, preferably, in contact with the compression element 5.
• This contention element 5 is intended to trap the field lines of the first magnetic field generated by the magnets 4a, 4b of the magnetron 2 on the rear face 2a of the magnetron 2 opposite the target 1, and to pass them from the first magnet 4a to the second magnet 4b or vice versa.
• the magnetron 2 may comprise a cathode 3 provided with a first face, and a second face opposite to said first face. On the first face are mounted magnets 4a, 4b, permanent or not, and the target 1 is mounted on the second face forming the front face of the magnetron 2.
• the magnetron 2 further comprises an anode 6. This anode 6 may, for example, form a guard surrounding the edges of the cathode assembly 3 / magnets 4a, 4b / contention element 5.
• FIG. 2 relates to a magnetron 2 provided with a circular flat cathode 3 with a diameter of 50 mm.
• the first magnet 4a is preferably of toroidal shape with a height of 1 cm, an outside diameter di of 50 mm and an inside diameter d 2 of 40 mm (hollow cylinder).
• the second magnet 4b can be a hollow cylinder, or full, outer diameter d3 2cm, inner diameter d 4 1cm (if hollow), and height 1cm.
• height is meant the dimension l- ⁇ of Figure 2, and a dimension not visible in Figure 3 but oriented perpendicular to the plane of Figure 3.
• the invention is not limited to the particular example of magnetron described above. The skilled person may use different magnetrons of his knowledge commonly used in physical vapor deposition.
• the cathode 3 may have a rectangular plate shape and the magnets 4a, 4b a horseshoe shape.
• the balancing means comprise a plate 7 comprising a ferromagnetic element.
• This plate 7 can also be called a magnet plate.
• the plate 7 is disposed between the target 1 and the magnetron 2, more particularly between the target 1 and the cathode 3.
• the plate 7 may comprise only this ferromagnetic element or an alloy of several ferromagnetic elements.
• the ferromagnetic element or elements are chosen from Fe, Co, Ni, Mn.
• the target 1 can be mounted on the cathode 3 of the magnetron 2 by interposition of the plate 7.
• the plate 7 can be arranged in direct contact with the cathode 3, then the plate 7 receives in direct contact the target 1.
• the source face has portions of the first target and portions of the target second.
• the nanoparticle mixture can also be obtained through a target whose source face is substantially flat, and is in the form of a mosaic based on at least two materials.
• Fixing supports (not shown) that do not modify the first magnetic field induced by the magnetron 2 can also be used to hold the target 1 against the cathode 3.
• the plate 7 is in contact with a face of the magnetron 2.
• cathode 3 opposite magnets of magnetron 2.
• the thickness of the plate 7 is calculated as a function of the power of the magnets 4a, 4b of the cathode 3, and the thickness of the target 1 so that the field lines of the first magnetic field are kept close to the 1a source face of the nanoparticles.
• the magnetic permittivity of the plate 7 must be sufficient to guide the magnetic field emanating from the cathode 3, but also allow the field lines of the first magnetic field to leave the target by the source face 1a of the nanoparticles before go back there.
• the plate 7 will have a thickness of between 0.05mm and 10mm. Of course this thickness will be a function of the characteristics of the first magnetic field and the ferromagnetic characteristics of the plate 7.
• the magnetron 2 (identical to that of the first embodiment) is subjected to a magnetic element generating a second magnetic field, outside the magnetron 2, favoring the closing of the field lines. leaking from the first magnetic field.
• This second magnetic field may for example be implemented by a magnetic coil 8 balancing means.
• This coil 8 may be a solenoid type electromagnet.
• the balancing means comprise, in addition to the coil 8, control means 9 slaving the coil 8 and comprising a state in which the leaking field lines of the first magnetic field are closed, and where said closed lines are maintained at the source face 1a of nanoparticles. This state may correspond to a modulation of the second magnetic field to adjust the first magnetic field.
• Such a coil 8 may for example be arranged around the magnetron 2 in the same plane as the latter.
• the magnetron 2 is disposed in the center of the coil 8, which then surrounds its edges, the edges of the magnetron corresponding to faces joining its front face to its rear face.
• the coil 8 may be coaxial with the magnetron 2.
• the coil 8 surrounds the anode 6.
• the use of the coil 8 is more malleable than the use of the plate having ferromagnetic properties, although the plate gives better results for a frozen and known configuration. Indeed, the coil 8 makes it possible on the one hand to adjust the second magnetic field via the direction and the intensity of the current of the coil 8 whatever the first magnetic field, but on the other hand to escape in an upper part. of the target 1 some magnetic field lines parallel to the axis of the magnetron, thus participating in a minimal imbalance of the magnetron 2.
• upper part is meant a distance of about 3cm from the target 1 in a direction opposite to the magnetron 2 starting from the source face 1 a.
• minimal imbalance it is understood that the magnetron 2 is better balanced with the coil 8 than without.
• the two embodiments can also be combined as illustrated in FIG. 5, taking again the references of FIGS. 2 and 4, so that their advantages act synergistically to increase the production yield of the nanoparticles.
• the advantage of using the coil 8 in combination with the plate 7 is to prevent the adverse effects mentioned in the second embodiment while retaining flexibility of adjustment to increase the production yield of the nanoparticles.
• the balancing means comprise both the plate 7 and the coil 8 associated with its control means 9.
• the balancing means are arranged so that the first magnetic field on the source face 1a of the target 1 has a minimum value B min and a maximum value B max , the dispersion of the first magnetic field defined by the formula
• the device for producing nanoparticles may further comprise an enclosure 10 in which the target 1, the magnetron 2 and the balancing means 7, 8, 9 are arranged (whether in the first mode embodiment, in the second embodiment or in the combination of the two modes).
• the balancing means, the magnetron 2, and the target 1 may form an assembly called a sputtering element.
• the chamber 10 may include a gas inlet 11 and an outlet port 12 of the nanoparticles.
• the gas inlet 11, the outlet port 12 are placed along the same axis A1.
• the magnetron 2 and its target 1 are preferably located between the gas inlet 11 and the outlet orifice 12.
• the source face 1a of the nanoparticles is oriented towards the outlet orifice 12.
• This enclosure 10 may be cooled by a cooling element not shown.
• the gas is injected into the chamber 10 by the arrival 11 of gas.
• the anode 6 and the cathode 3 of the magnetron 2 are polarized so that the target is polarized negatively, and the gas near the target becomes positively ionized.
• a gas such as Argon will be used when arriving near the target will react in the following way:
• This phenomenon of agglomeration results from the formation of germs consisting of some atoms torn from the target (nucleation) followed by their growth by accumulation on the seed of other atoms of the target.
• the magnetron 2 associated with the balancing means 7, 8, 9 makes it possible to improve the yield of the nanoparticles by promoting nucleation.
• the quality of nucleation, and therefore of the yield depends on the cooling profile when the atoms move away from the target 1. In the particular case of the target 1 placed in an enclosure 10, the cooling profile corresponds to the evolution of the temperature between the target 1 and the outlet orifice 12.
• the nucleation theory shows that the nucleation is maximum for a given temperature T opt and can only occur if at a point, if any of the enclosure, the temperature profile approaches this value.
• the optimal cooling between the target 1 and the outlet orifice 12 induces a nucleation of germs followed by their growth, that is why in the prior art, expensive and complex cooling systems are used.
• Figure 7 illustrates the number of possible nucleations as a function of temperature for a copper target material.
• the curve has a Gaussian shape, and makes it very clear that if the temperature is too hot or too cold, there is no nucleation.
• T min -173 ° C
• Tmax 326 ° C
• T opt the value of T opt depends on the material of the target.
• FIG. 8 illustrates the evolution of the temperature as a function of the distance, from the target 1, between the target 1 and, where appropriate, the outlet orifice 12.
• the temperature is about 580 ° C, and at the orifice 12, the temperature is about 76 ° C.
• This curve makes it possible to demonstrate the importance of controlling the thermal profile. Indeed, by connecting the curve of Figure 7 with that of Figure 8, it is possible to determine a first zone where nucleation is impossible and a second zone where nucleation is possible.
• the nucleation zone extends from 25 mm to the outlet orifice 12.
• the steeper the curve associated with the temperature drop while moving away from the target the larger the zone of nucleation. nucleation within enclosure 10 will be large, and the higher the yield will be important.
• the nanoparticle production device described above provided with at least one magnetron 2 and means for balancing the first magnetic field makes it possible to act on the thermal profile. Indeed, the leaking field lines participate in the heating of distant areas of the magnetron 2.
• the enclosure is cooled to very low temperature using for example a coolant such as nitrogen liquid at -196 ° C.
• the balancing means make it possible to achieve high nanoparticle synthesis yields while avoiding, if necessary, cooling using heat-transfer fluids at negative temperatures, such as nitrogen for example.
• the balancing means Thanks to the balancing means, the leaking field lines are much fewer, the thermal profile is better controlled and costly cooling systems can be avoided, a simple water cooling system may be sufficient.
• control of the field lines C of the first magnetic field also makes it possible to homogenize the wear of the target with an area of impact of the enlarged spray ions, thus avoiding premature replacement of the target.
• the device for producing nanoparticles may comprise, as illustrated in FIGS. 4 to 6, a first temperature measuring sensor 13 arranged facing the source face 1 a, and arranged to give a temperature representative of the temperature, preferably at the source side 1a of the nanoparticles.
• the first-sensor 13 is disposed in the chamber 10 between the face 1a and the orifice 12. This first sensor 13 may be disposed a few centimeters from the source face 1a, for example between 1 cm and 5cm .
• the magnetron 2 can be polarized, and the temperature measured by the first sensor 13, once it is stabilized. This measured value can then be transmitted to the control means 9 of the coil 8 adapted to vary the second magnetic field of the coil 8 so as to obtain the smallest possible value of temperature measured by the first sensor 13. whereas the thermal profile is degressive the further away from the target 1, the temperature at a given point is minimal when the magnetron 2 is the most balanced. In this configuration we increase the probabilities of reaching or approaching T opt .
• a particular embodiment of the calibration phase can be implemented by a loop of steps. First of all the current of the coil 8 is zero, then a first temperature measurement T 0 is performed. Then, the value of the current in the coil 8 is incremented, a second temperature measurement T is carried out, and if TT 0 ⁇ 0 is continued to increase the current of the coil until T n + iT n is positive. If T n + iT n is positive then the magnetron is considered balanced.
• the device may furthermore comprise a second temperature measurement sensor 14, preferably disposed near the outlet orifice 12 (see FIG. 6) and for example connected to the control element 9.
• control element 9 can then modulate the second magnetic field of the coil 8 as a function of the temperature difference between the first sensor 13 and the second sensor 14.
• Measurements using one or two temperature sensors may also be used in the first embodiment to select the correct plate as a function of a set of ferromagnetic plates. Thus, for each plate, temperature measurements are made, then the plate associated with the smallest measurement, or the fastest falling slope, is chosen.
• FIG. 9 illustrates a particular implementation of an NP nanoparticle deposition device.
• a deposition device comprises a first chamber 15 and an enclosure 10 in which are arranged the magnetron 2, the target 1 and the balancing means (not visible in FIG. 9).
• the enclosure 10 comprises an inlet 11 of a sputtering gas and an outlet orifice 12 of the nanoparticles.
• the outlet orifice 12 of the NP nanoparticles opens into the first chamber 15.
• the device further comprises a second chamber 16 provided with a substrate 18 for depositing the nanoparticles, called deposit chamber, the first chamber 15 communicating with the second chamber
• the second chamber 16 is in depression with respect to the first chamber 15. It is this pressure difference that allows the NP nanoparticles to be projected from the chamber 10 into the first chamber 15, then into the chamber 15. the second chamber 16 to be deposited on the substrate 18.
• the magnetron 2 and the associated target 1 can generate a vapor of the target material or materials.
• the nanoparticles are generated from the source face a of the target along the axis A1 until reaching the outlet orifice 12 and then to be propelled into the deposition chamber by the hole 17 towards the substrate 18 of associated deposit.
• the deposition device may comprise a first pumping element (pumping 1) intended to evacuate in the first chamber 15, and a second pumping element (pumping 2) intended to evacuate in the second room 16.
• the interior of the enclosure 10 is cooled by a cooling element 19, for example with water (typically between 10 ° C. and 25 ° C.) making it possible to partially regulate the thermal profile of the gas in the atmosphere.
• enclosure 10 in combination with the effects of the balancing means.
• This can for example be implemented by circulating around the enclosure 10 the heat transfer fluid.
• adjusting the equilibrium of a magnetron makes it possible to increase the deposition efficiency of nanoparticles by controlling the spatial profile of the vapor that it emits, while reducing the resources required for cooling the enclosure 10.
• the inlet 11 of the gas, the outlet orifice 12 of the enclosure 10, and the hole 17 allowing the communication between the first chamber 15 and the second chamber 16 are located along the same axis A1. This promotes the displacement of the NP nanoparticles according to the direction of diffusion of the sputtering gas.
• the magnetron 2 can be arranged along this axis A1, the source face 1a being then oriented towards the orifice 12.
• nanoparticle deposition device is not limiting, and the person skilled in the art will be able to adapt other structures of deposition devices based on the device for producing nanoparticles as described above. .
• the modified device was polarized with a 150mA sputtering current, the average silver particle size was measured at 5nm, and the deposited mass per hour was 200 to 250ng / cm 2 .
• the deposited mass has been higher thanks to the balancing means used to improve the performance.
• the gain on the number of particles deposited is a factor of two, while the spraying current is 25% lower.
• the decrease in spray current is directly related to a drop of 25% of the target material consumed to obtain this result.
• the target used is a germanium target.
• Deposition experiments were performed with a standard nanoparticle producing device selected so that the dispersion of its magnetic field was greater than 0.5 and the absolute value of the difference between B min and B ma x was about 90mT is 9 * 10 -2 Tesla
• a device of identical characteristics was modified with balancing means so that the dispersion was set at 0.35 and the absolute value of the difference between B min and B ma x at about 30mT or 3 * 10 "2 Tesla.
• the industrial applications of the present deposition device relate to any product using nanoparticles for essentially surface devices ranging in size from a few square millimeters to a few square centimeters.
• optoelectronic detectors simple sensors, imagers, solar cells, optical and / or magnetism-based data storage, fuel cells, micro-batteries, any electrochemical device using catalyst nanoparticles, or thermoelectric devices, etc.
• the device for producing nanoparticles has the advantage of being close to the magnetron structures commonly used in PVD deposits.
• the invention also relates to a method for depositing nanoparticles using a magnetron 2 on which is mounted a target provided with a source face 1a of nanoparticles.
• the magnetron 2 generates a magnetic field forming field lines at the source face 1a of the nanoparticles.
• the method comprises a step of adjusting the magnetic field of closing leaking field lines of the magnetic field and maintain said lines closed at said source face 1a nanoparticles. The adjustment is made by means of balancing separate magnetron.
• the adjustment step is performed before proceeding to the deposition of nanoparticles on a support substrate, that is to say preferably before spraying the gas to react with the target. Examples of adjustment from a Gaussmeter or a temperature sensor are described above. After adjustment, it is possible to polarize the magnetron and then vaporize the spray gas so that the latter reacts with the target to generate nanoparticles that will be deposited on a substrate.
• the power supply of the magnetron can be continuous, pulsed, sinusoidal, low frequency or radiofrequency mode.
• the magnets of the magnetron may be permanent or not.
• the target may include metallic, semiconductor or dielectric materials.
• the target does not contain ferromagnetic materials.
• the balancing means are, of course, distinct from the target and advantageously allow to balance the first magnetic field.
• the target comprises ferromagnetic elements, use the embodiment or variant with the coil that can as the material of the target is consumed, adapt the first magnetic field.
• the target will be based on at least one material selected from Si, Ge, Co, Ni, Ag, Cu, Pt, etc.

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• 2011
  • 2011-03-01 FR FR1100614A patent/FR2972199B1/fr not_active Expired - Fee Related
• 2012
  • 2012-02-27 US US14/002,588 patent/US20140001031A1/en not_active Abandoned
  • 2012-02-27 EP EP12710765.4A patent/EP2681758A1/de not_active Withdrawn
  • 2012-02-27 WO PCT/FR2012/000069 patent/WO2012117171A1/fr active Application Filing

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