WO2017138695A1 - Réacteur - Google Patents

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WO2017138695A1
WO2017138695A1 PCT/KR2016/015034 KR2016015034W WO2017138695A1 WO 2017138695 A1 WO2017138695 A1 WO 2017138695A1 KR 2016015034 W KR2016015034 W KR 2016015034W WO 2017138695 A1 WO2017138695 A1 WO 2017138695A1
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metal
metal precursor
reactor
formula
nanoparticles
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PCT/KR2016/015034
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English (en)
Korean (ko)
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박진호
김홍탁
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영남대학교 산학협력단
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Publication of WO2017138695A1 publication Critical patent/WO2017138695A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles

Definitions

  • the present application relates to a reactor capable of controlling the reaction rate of a highly reactive compound.
  • Gallium nitride is a semiconductor material with a wide bandgap energy of 3.4 eV, direct band transitions, high energy radiation and high stability to high temperatures. In view of these properties, gallium nitride is known as a promising material for light emitting diodes, short wavelength lasers, UV detectors and solar cell windows in space.
  • the gallium nitride film may be mixed with a solution containing a gallium precursor and a solution containing sodium dimethyldithiocarbamate to form metal precursor nanoparticles, followed by coating the nanoparticles on a substrate and performing heat treatment.
  • the gallium precursor and sodium dimethyldithiocarbamate has a very high reactivity, when a simple mixing of the gallium precursor and sodium dimethyldithio carbamate, an explosive reaction occurs. Therefore, a phenomenon in which the metal precursor nanoparticles formed during the reaction may be aggregated may occur. In this case, it may be difficult to control the particle size of the metal precursor nanoparticles evenly, and the base layer may include a solution containing the metal precursor nanoparticles. When coating on, it may be difficult to form a uniform and thin coating layer. Furthermore, in the past, an expensive microchannel reactor was used to control the reaction rate of such a highly reactive compound, but a method of controlling the reaction rate at a lower cost is required.
  • the present application provides a reactor capable of controlling the reaction rate of a highly reactive compound.
  • the present application relates to a reactor.
  • a reactor of the present application by suppressing the explosive reaction rate of the metal nanoparticle precursor by injecting a solution containing the metal precursor to a solution containing a reactive compound having a very high reactivity with the metal precursor,
  • the particle size of the precursor nanoparticles can be controlled to be small, whereby a film having a uniform surface roughness can be produced in a large area.
  • FIG. 1 exemplarily shows a reactor 100 of the present application.
  • An exemplary reactor of the present application includes a reaction vessel 120 and a reaction rate controller 110.
  • the reactor 120 refers to a water tank or a container in which the reaction takes place, and in one example, the reactor 120 may be filled with a solution containing a reactive compound reacting with a metal precursor.
  • the metal precursor may include one or more selected from the group consisting of metal nitrate, metal acetate, and metal chlorides.
  • the metal is not particularly limited as long as it is a metal capable of reacting with the reactive compound.
  • the metal may be a metal of Group 8, Group 11, Group 12, or Group 13.
  • the metal may be at least one selected from the group consisting of gallium, aluminum, indium, thallium, zinc, copper, iron, and tin, and may be, for example, gallium, aluminum, or indium, but is not limited thereto. It doesn't happen.
  • the metal precursor may be gallium nitrate (Ga (NO 3 ) 3 ⁇ 8H 2 O), gallium acetate or gallium chloride.
  • the reactive compound is a compound having a very high reactivity with the metal precursor, the reaction of the metal precursor and the reactive compound may satisfy the following general formula (1).
  • Rp represents a rate of increase in particle size that is a reactant of the metal precursor and a reactive compound within Ts time
  • 2 is a graph illustrating a change in particle size or diameter according to a reaction time.
  • the particle size may change in the form of a quadratic function.
  • the point of time corresponding to the boundary between the area where the particle size grows explosively according to the reaction time and the area where the particle size grows slowly according to the reaction time that is, the time that the growth of the particle size saturates is Ts.
  • Ts is the time at the point where the first straight line of the graph meets the first straight line of the graph during the time that the particle size grows in the graph of FIG. It may mean.
  • the particle size grows explosively, for example, the rate of increase of the particle size in the left region of the Ts time may be 1 ⁇ m / min or more. .
  • the growth of the particle size does not occur or grows at a very low rate depending on the reaction time, for example, the increase rate of the particle size in the right region of the Ts time is 1 ⁇ m / min. May be less than.
  • the reactive compound may be a compound represented by Formula 1 below.
  • M 1 is a Group 1 metal
  • R 1 and R 2 each independently represent alkyl having 1 to 12 carbon atoms.
  • M 1 may be a Group 1 alkali metal, such as lithium, sodium or potassium, and in one example may be sodium.
  • each of R 1 and R 2 may be independently an alkyl group having 1 to 12 carbon atoms, for example, 1 to 8 carbon atoms, 1 to 6 carbon atoms, or 1 to 4 carbon atoms.
  • R 1 and R 2 may be each independently methyl, ethyl, propyl, butyl, pentyl or hexyl, and in one example may be methyl, but is not limited thereto.
  • the compound of Formula 1 may be sodium dimethyldithiocarbamate (CH 3 ) 2 NCSSNa.2H 2 O), the solution containing the reactive compound is sodium dimethyldithiocarba Mate.
  • the reaction rate control unit 110 is a device that controls the reaction rate of the metal precursor and the reactive compound occurring in the reaction tank 120.
  • a reactive compound such as the compound of Formula 1
  • an explosive reaction occurs when the first solution and the second solution are simply mixed, an explosive reaction occurs. Therefore, aggregation of the formed metal precursor nanoparticles may occur. In this case, it is difficult to evenly control the particle size of the metal precursor nanoparticles, and the solution containing the metal precursor nanoparticles may be coated on the substrate layer. In this case, it may be difficult to form a uniform and thin coating layer.
  • the solution comprising the metal precursor and the solution comprising the reactive compound may be mixed by a spray device 100, in one example, the solution comprising the metal precursor is The mixed solution may be prepared by spraying on a solution containing a reactive compound.
  • the compound of Formula 2 is tris (N, N-dimethyldithiocarbamate) -gallium (III) (Tris (N, N-dimethyldithiocarbamato) -gallium (III), Ga (DmDTC) 3 ),
  • the third solution may comprise tris (N, N-dimethyldithiocarbamate) -gallium (III), preferably, the residual sodium dimethyldithio contained in the second solution Carbamate and the tris (N, N-dimethyldithiocarbamate) -gallium (III).
  • the average particle diameter of the metal precursor nanoparticles of Formula 2 may be 5 to 100 nm, for example, 10 to 70 nm, or 15 to 50 nm, preferably 20 to 40 nm.
  • the particle size distribution of the metal precursor nanoparticles of Formula 2 has a very small standard deviation, and in one example, the particle size distribution of the metal precursor nanoparticles is 5 to 40 nm, for example, It can have a standard deviation of 10 to 30 nm, 10 to 20 nm.
  • the obtained metal precursor nanoparticles of the formula (2) may be dissolved in a second solvent, the metal precursor nanoparticle solution prepared according to may include the metal precursor nanoparticles of the formula (2).
  • the coating layer of the metal precursor nanoparticle solution may be formed to have a thickness of 15 ⁇ m or less, and the metal nitride layer formed after the heat treatment to be described later may have a thickness of 10 ⁇ m or less.
  • the second solvent for dispersing the metal precursor nanoparticles of Chemical Formula 2 may be used without limitation as long as it is a highly evaporative solvent.
  • chloroform CH 3 Cl
  • methanol It may be at least one selected from the group consisting of ethanol and ether, and in one example, may be chloroform, but is not limited thereto.
  • the metal precursor nanoparticle solution layer coated on the substrate layer may be heat treated under a nitrogen gas or ammonia gas atmosphere, and by the heat treatment, the sulfur atom of the compound of Formula 2 in the metal precursor nanoparticle solution layer is nitrogen gas or ammonia It may be substituted with a nitrogen atom of the gas. Accordingly, a film including a metal nitride layer having a final thin thickness and a uniform thickness can be manufactured.
  • FIG. 3 is a diagram illustrating an apparatus 200 in which a heat treatment is performed in the manufacturing method of the present application.
  • the metal nitride layer formed by the heat treatment of the metal precursor nanoparticle solution layer including the metal precursor nanoparticles of Formula 2 may be formed according to the following schemes 1 and 2.
  • the present application also relates to a film produced by the above-described manufacturing method.
  • Exemplary film of the present application as prepared using the metal precursor nanoparticles obtained by the reactor of the present application described above, comprises a very thin and uniform thickness of the metal nitride layer of several micrometers, and also, Sulfur atoms in the metal precursor nanoparticles of doped the metal nitride layer, the sulfur component on the surface has a feature that is detected in the photoluminescence (PL) spectrum.
  • PL photoluminescence
  • FIG. 4 is a cross-sectional view schematically showing a film of the present application.
  • the photoluminescence (PL) spectrum measured using a laser of 325 nm wavelength satisfies the following general formula (2).
  • E (I max ) represents the bandgap energy at the position having the maximum intensity value of the photoluminescence spectrum
  • Eg represents the bandgap energy of the metal nitride
  • Photoluminescence refers to a phenomenon in which a material is stimulated by light to emit light by itself, and more specifically, when an electron in a light-absorbing material becomes excited and then returns to its original state. It means the phenomenon of emitting light.
  • Photoluminescence (PL) Spectrum is a spectrum showing the relative intensity representing the energy-specific distribution of light emitted from a material irradiated with light by using light luminescence.
  • the intensity of the photoluminescence spectrum has a maximum intensity value (hereinafter, referred to as a peak value) in an energy band unique to a material. Since the intensity value of the photoluminescence spectrum is a relative value, it is expressed in units of a.u. (arbitrary unit).
  • the PL measurement may be performed using a He-Cd laser having a center wavelength of 325 nm for the excitation light source.
  • the measurement temperature is not particularly limited, but it is preferable to perform the measurement at 20 K or lower.
  • Examples of the device capable of measuring PL under such conditions include Omnichrome series 74 He-Cd laser, Acton SpectraPro 2300i spectrometer, Princeton Instruments PI-MAX1024HQ-Blu CCD detector, and the like.
  • the PL spectrum signal can be easily detected by using a low temperature PL of 20 K or less.
  • the metal nitride layer 12 may be formed by replacing sulfur atoms in the metal precursor nanoparticles of Chemical Formula 2 with nitrogen atoms when heat-treating the coating layer including the metal precursor nanoparticles of Chemical Formula 2.
  • sulfur atoms in the metal precursor nanoparticles of Chemical Formula 2 are doped into some metal nitride layers 12, and sulfur components are detected in a photoluminescence (PL) spectrum on the surface.
  • PL photoluminescence
  • the metal nitride layer satisfying Formula 2 has a maximum intensity value of the photoluminescence (PL) measured using a laser of 325 nm wavelength of 2.8 to It will be in the range of 3.2 eV. This is because, as described above, sulfur atoms in the metal precursor nanoparticles of Chemical Formula 2 are doped into some metal nitride layers 12 so that sulfur components are detected in the photoluminescence (PL) spectrum at the surface.
  • PL photoluminescence
  • the bandgap energy at the position having the maximum intensity value of the photoluminescence spectrum represented by the sulfur component is 2.95 eV
  • the bandgap energy of gallium nitride is 3.44 eV. Therefore, k value calculated according to the general formula (2) is 4.9, thereby satisfying the general formula (2).
  • the sulfur component detected on the surface of the metal nitride layer 12 may also be confirmed by X-ray photoelectron spectroscopy (XPS) analysis.
  • the metal nitride layer 12 may include Mg after removing a surface oxide layer with an ion gun using an inert gas.
  • the maximum intensity value of the XPS spectrum measured on the basis of K ⁇ X-ray may be in the range of 160.0 eV to 170.0 eV.
  • the maximum intensity value of the XPS spectrum can be found around about 164 eV (based on the carbon 1s peak of 284.5 eV, sulfur 2p3 / 2 peak).
  • it can be confirmed that it contains sulfur within 5% by weight through quantitative analysis through XPS.
  • the "XPS analysis” is a method of using X-rays as a light source in electron spectroscopy, and when X-rays are irradiated to a substance, photoelectrons are emitted out of the substance, and the kinetic energy is at an original position under the cabinet electrons of the atoms constituting the substance. Since it reflects the magnitude of the binding force, this means a method of investigating the atomic composition of a material and the bonding state of electrons.
  • the center line average roughness is measured under the standard of JIS B0031, JIS B0601 or ISO 468.
  • the metal may be one or more selected from the group consisting of gallium, aluminum, indium and lead, for example, gallium, but is not limited thereto.
  • the base layer 11 may have a melting point of 300 ° C. or higher. When the melting point of the base layer 11 is less than 300 ° C., the components of the base layer may melt during the heat treatment process, and thus carbon or carbon-related byproducts may remain in the metal nitride layer.
  • the substrate layer 11 may include at least one polymer substrate selected from the group consisting of acrylonitrile, polyphenylenevinylene, polytetrafluoroethylene, polyvinylcarbazole, and polyimide, or
  • the layer 11 may include one or more selected from the group consisting of alumina, silicon carbide (SiC), silicon, quartz, glass, and stainless steel. In one example, the base layer 11 may be alumina. However, it is not limited thereto.
  • the precursor nano by spraying a solution containing the metal precursor to a solution containing a reactive compound having a very high reactivity with the metal precursor to suppress the explosive reaction rate of the metal nanoparticle precursor, the precursor nano at a low cost
  • the particle size of the particles can be controlled small, whereby a film having a uniform surface roughness can be produced in a large area.
  • FIG. 3 exemplarily shows an apparatus in which a heat treatment is performed in the method of the present application.
  • FIG. 4 is a cross-sectional view schematically showing a film of the present application.
  • Ga (DmDTC) and 1 H-NMR spectrum of the nanoparticles 3 is a graph and a photograph showing the size distribution and shape of Ga (DmDTC) 3 nanoparticles.
  • FIG. 7 is a graph illustrating a pyrolysis reaction of Ga (mDTC) 3 using a thermogravimetric analyzer.
  • FIG. 10 shows XRD patterns and SEM photographs of epitaxial gallium nitride films grown on gallium nitride layers pyrolyzed by MOCVD.
  • Nanoparticles were identified using a 1 H-Fourier transform magnetic resonance system ( 1 H-FT-NMR, Bruker DPX300).
  • Nanoparticles synthesized in the following examples and comparative examples The size of nanoparticles is not only measured by transmission electron microscope (TEM, Hitachi, H-7600) and X-ray diffraction (X-ray diffraction, XRD, PANalytical, X'pert PRO), but also by particle size analyzer (Beckman Coulter, N5).
  • TEM transmission electron microscope
  • XRD X-ray diffraction
  • PANalytical X'pert PRO
  • particle size analyzer Beckman Coulter, N5
  • a gallium nitride layer was formed on the alumina base layer.
  • the gallium nitrate solution was ultrasonically sprayed on the sodium dimethyldithiocarbamate ligand solution for 30 minutes at room temperature, and the flow rate of the gallium nitrate solution was maintained at 10 ml / hr during the spraying process.
  • the Ga (DmDTC) 3 nanoparticles were synthesized by a very slow sedimentation process, and the precipitated material was filtered using a centrifugation process.
  • the synthesized Ga (DmDTC) 3 nanoparticles were washed several times with deionized water and dried in a vacuum oven at 60 ° C. for 4 hours.
  • the average particle size of the prepared In (DmDTC) 3 nanoparticles was measured as 30 nm
  • prepared In (DmDTC) of 3 nanoparticle particle size distribution is measured by 3 nm
  • the centerline surface roughness of the indium nitride layer was measured to be 9 nm.
  • Ga (DmDTC) 3 nanoparticles were formed in the same manner as in Example 1, except that the gallium nitrate solution was not ultrasonically sprayed on the sodium dimethyldithiocarbamate ligand solution, but was simply mixed.
  • To produce a gallium nitride thin film. 10 is an image taken using a scanning electron microscope (Scanning Electron Microscope, SEM) of the gallium nitride thin film prepared in Comparative Example. As shown in FIG. 10, the manufactured gallium nitride thin film did not form a continuous thin film form, and it was very difficult to form a 5 ⁇ m thick layer, and showed a very nonuniform and irregular porous structure. Accordingly, the surface roughness of the gallium nitride thin film could not be calculated according to Equation 1 above.
  • FIG. 6 (a) shows the XRD pattern of the gallium nitride layer by pyrolytic deformation of Ga (DmDTC) 3 film in an ammonia flowing environment.
  • the XRD peaks of the gallium nitride layer are mainly observed at 34.6 ° and 73.1 ° 2 ⁇ and are assigned contributing from the (0002) and (0004) planes of the hexagonal structure phase. In addition, no peak attributable to the ⁇ -Ga 2 S 3 phase was observed in the XRD pattern.
  • the Ga (DmDTC) 3 phase turns into a ⁇ -Ga 2 S 3 phase under a nitrogen environment above 500 ° C., which indicates that Ga (DmDTC) 3 is thermally decomposed into adducts of ⁇ -Ga 2 S 3 and CN (CH 3 ). It is known to represent.
  • the pyrolysis reaction from Ga (DmDTC) 3 to gallium nitride layer under ammonia can be simply expressed by the thermal decomposition of Ga (DmDTC) 3 and the chemical reaction between ⁇ -Ga 2 S 3 and ammonia. This reaction can be summarized as in Schemes 1 and 2.
  • the reason why the pyrolyzed gallium nitride layer is well arranged in the culture direction first is expected from the recrystallization process during the pyrolysis reaction.
  • the deposited Ga (DmDTC) 3 film was changed to Ga 2 S 3 by pyrolysis, and the sulfur (S) component was simultaneously replaced with a nitrogen (N) component.
  • the pyrolyzed gallium nitride layer undergoes a recrystallization process, and because of the low surface energy of the (0002) plane in the hexagonal structure, the crystalline structure of gallium nitride is mainly arranged in the (0002) first culture direction.
  • the gentle slope observed in the XRD pattern confirms the presence of an amorphous phase in the gallium nitride layer.
  • 6 (b) shows SEM images of the surface and cross section of the gallium nitride layer, showing a dense structure and a small crystalline phase. Although the gallium nitride layer was 5 mu m thick, it did not show any voids or cracks. From this, it can be seen that the amorphous phase plays a major role in reducing the lattice mismatch between the gallium nitride layer and the alumina substrate. The reason why the amorphous phase appears in the pyrolyzed gallium nitride layer can be explained as follows.
  • Ga 2p 3/2 represents a high-resolution XP spectrum of the N 1s and O 1s peak.
  • the Ga 2p 3/2 deconvolution of peaks (peak deconvoluted) of was observed at 1118.3 eV and 1120.8 eV which apparently moving from the core levels of 1116.5 to 1116.7 eV of gallium. From this, apparent movement of the Ga 2p 3/2 it can be seen that the point has been mixed with the gallium atoms are nitrogen and oxygen in the film.
  • the peak region 1120.8 eV due to oxygen mixing was very small compared to the peak region 1118.3 eV due to nitrogen mixing, indicating that oxygen contamination is sufficiently low in non-vacuum methods.
  • oxygen peaks range from 529 to 535 eV, and peaks near 529 to 530 eV represent lattice oxygen, while peaks of 530 to 535 eV are related to carbon uptake or contamination by organic material on the film surface. do.
  • the O 1s XPS peaks at 530.8 eV and 531.8 eV are assigned to the chemisorption of the film surface.

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Abstract

La présente invention concerne un réacteur. Le réacteur selon la présente invention supprime la vitesse de réaction explosive d'un précurseur de nanoparticules métalliques par pulvérisation d'une solution comprenant un précurseur de métal sur une solution comprenant un composé réactif très fortement réactif au précurseur métallique, et peut ainsi réguler les nanoparticules de précurseur pour qu'elles aient une petite taille de particule même à faible coût, et par conséquent obtenir un film ayant une rugosité en surface uniforme et une zone importante.
PCT/KR2016/015034 2016-02-12 2016-12-21 Réacteur WO2017138695A1 (fr)

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CN110976845A (zh) * 2019-12-04 2020-04-10 华南理工大学 一种消除激光3d打印成形7075铝合金热裂纹的粉末改性方法

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