WO2018047994A1 - Poudre de pulvérisation à fluidité élevée et son procédé de production - Google Patents

Poudre de pulvérisation à fluidité élevée et son procédé de production Download PDF

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WO2018047994A1
WO2018047994A1 PCT/KR2016/010071 KR2016010071W WO2018047994A1 WO 2018047994 A1 WO2018047994 A1 WO 2018047994A1 KR 2016010071 W KR2016010071 W KR 2016010071W WO 2018047994 A1 WO2018047994 A1 WO 2018047994A1
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powder
organic monomer
granular
spray
granule
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PCT/KR2016/010071
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English (en)
Korean (ko)
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문흥수
신평우
이훈철
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(주)세원하드페이싱
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Priority to JP2018550758A priority Critical patent/JP6659872B2/ja
Priority to KR1020187014428A priority patent/KR102085258B1/ko
Priority to PCT/KR2016/010071 priority patent/WO2018047994A1/fr
Publication of WO2018047994A1 publication Critical patent/WO2018047994A1/fr

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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C4/00Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • C23C4/11Oxides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605Treating the starting powders individually or as mixtures
    • C04B35/62645Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/62665Flame, plasma or melting treatment
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628Coating the powders or the macroscopic reinforcing agents
    • C04B35/62802Powder coating materials

Definitions

  • the present invention relates to a high flow sprayed powder and a method for producing the same, and more particularly, to a high flow sprayed powder coated with an organic monomer and a method for producing the same.
  • Ceramic spray coating technology using thermal spray powder is applied to various fields. By industry, it is most actively applied to general machinery, semiconductor, liquid crystal, steel and printing. With the expansion of market sizes in China, Korea, and Singapore, Asia's market size is a very promising technology that is growing to the same level as the US and EU.
  • Spray coating methods using thermal spray powders include arc spraying, flame spraying, high speed flame spraying, plasma spraying, cold spray (CS), suspension plasma spray, and SPPS (Solution precursor plasma spray). .
  • thermal spraying materials we are actively developing and selling stabilized zirconia (YSZ) used for thermal barrier coating, Al 2 O 3 as insulation material, and TiO 2 for photocatalyst. Avatar is also being developed for application as a high value-added thermal spray coating material. Tungsten (W) is also an important material as a high-temperature material for shielding radiation or plasma bulkheads in nuclear fusion reactors, and thermal spray coatings are being developed for its application.
  • YSZ stabilized zirconia
  • Al 2 O 3 as insulation material
  • TiO 2 for photocatalyst.
  • Avatar is also being developed for application as a high value-added thermal spray coating material.
  • Tungsten (W) is also an important material as a high-temperature material for shielding radiation or plasma bulkheads in nuclear fusion reactors, and thermal spray coatings are being developed for its application.
  • Ceramic spray coating technology has been applied to a variety of wear-resistant coatings to improve the wear resistance, the wear-resistant coating by the thermal spray coating has a sufficient mechanical strength.
  • Thermal spray coatings provide a significant level of thermal spray coating material for ceramic powders to provide control over friction and abrasion to withstand contact with other structural surfaces that come in contact in the form of sliding, rolling or impact. Used as Such ceramic coatings enable effective control of wear and friction as described above, and thus applications in industrial fields are continuously expanding.
  • the greatest influence on the quality of the thermal spray coating film is to maintain the discharge rate of the thermal spray powder discharged from the thermal spray powder supply portion. If the velocity of the thermal sprayed powder is not kept constant during the thermal spray coating, the uniformity of the thermal sprayed coating film and the rate of generation of pores are out of the design value, or have a disadvantageous effect such as the strength of the thermal sprayed coating.
  • the powder used for the spray coating is produced in a slurry, and the slurry is used by discharging, the clogging phenomenon may be suppressed, and a discharge amount may be generated according to a predetermined pressure.
  • the powder discharge using the slurry is caused to deteriorate the quality of the thermal spray coating due to the organic impurities contained in the slurry production.
  • the spray powder produced through spray drying the quality of the thermal spray coating occurs due to the shape of the granules, the surface roughness of the granules.
  • thermal spray powders currently applied are sphericalized by spray drying to reduce friction between powders and control the center of gravity of the powders by spherical centers, thereby reducing clogging and applying to the thermal spray coatings.
  • the flow characteristic value of the powder is low, resulting in a decrease in the spray coating quality.
  • the spray coating powder is obtained by forming a sealing film on the outer surface of the ceramic powder and surrounding it, and heat treating the sealing organic substance powder in the state surrounding the outer surface.
  • the particle diameter ratio of the ceramic powder and the said organic substance powder is 1: 0.1-0.3, The range is narrowed further, The thermal spraying powder whose content ratio of the ceramic powder and the organic substance powder was adjusted to 1: 0.2-0.5 is disclosed.
  • the prior art is to form a sealing film of the thermal spray coating at the time of forming the thermal spray coating, there is a problem that the quality, such as uniformity of the thermal spray coating film is degraded due to the aggregation of the thermal spray powder because a large amount of organic material is coated on the ceramic powder. .
  • the first technical problem to be achieved by the present invention is to provide a high flow powder with improved flow characteristics during powder discharge.
  • the second technical problem to be achieved by the present invention is to provide a method for producing a high-flow sprayed powder for achieving the first technical problem.
  • the present invention for achieving the above-described first technical problem, to provide a high flow spray powder characterized in that it comprises a granulated powder and an organic monomer attached to the surface of the granulated powder.
  • the granular powder may have any one selected from the group consisting of ZrO 2 , Y 2 O 3 , Al 2 O 3 , AlN, HfO 2 , TiO 2 and stabilized zirconia.
  • the granulated powder is characterized in that the high flow sprayed powder, which is a powder produced through a granulation process.
  • the granulated powder is characterized in that the high flow sprayed powder which is a powder surface-treated by plasma.
  • the surface of the granule powder is melted by the plasma, characterized in that the high-flow sprayed powder of which the surface density of the granule powder is increased.
  • the granular powder is characterized in that the high fluid spray powder is stabilized zirconia.
  • the content of the organic monomer is characterized in that the high fluid spray powder in the range of 0.05 wt% to 5.0wt% relative to the weight of the granule powder.
  • the organic monomer is characterized in that the high flow sprayed powder occupying 5% to 100% of the surface area of the granule powder.
  • the organic monomer may have any one selected from the group consisting of anionic surfactants, cationic surfactants, amphoteric surfactants, and nonionic surfactants.
  • the present invention for achieving the above-described second technical problem, preparing a granulated powder prepared through a granulation process, preparing an organic monomer solution by adding an organic monomer to a solvent, the granules in the organic monomer solution It is to provide a method for producing a high flow sprayed powder comprising the step of adding a powder, mixing and coating the organic monomer on the surface of the granule powder while evaporating the solvent.
  • the granulated powder is ZrO 2 , Y 2 O 3 , Al 2 O 3 , AlN, HfO 2 , TiO 2 and a method of producing a high flow spray powder, characterized in that any one selected from the group consisting of stabilized zirconia.
  • the method of producing a high flow sprayed powder characterized in that it further comprises the step of plasma-treated the sprayed powder.
  • the surface of the granule powder is melted by the plasma surface treatment, so that the surface density of the granule powder is increased, and the surface roughness is reduced.
  • the granulated powder is a method for producing a high flow sprayed powder, characterized in that the stabilizing zirconia.
  • the flow characteristics of the powder during the thermal spray coating of the organic coating powder is improved, there is an effect that the clogging phenomenon in the spray nozzle is suppressed.
  • the use of the powder with improved flow characteristics has the effect of prolonging the continuous use time of the plasma spray gun for the spray coating.
  • FIG. 1 is a flowchart illustrating a process of coating an organic monomer on a sprayed powder surface according to an embodiment of the present invention.
  • Figure 2 is a 300 times electron microscope image of the granule powder in the range of 5 ⁇ m to 25 ⁇ m in accordance with a preferred embodiment of the present invention.
  • Figure 3 is a 1000 times electron microscope image of the granule powder in the range of 5 ⁇ m to 25 ⁇ m in accordance with a preferred embodiment of the present invention.
  • Figure 4 is a 300 times electron microscope image of the granule powder in the range of 15 ⁇ m to 45 ⁇ m in accordance with a preferred embodiment of the present invention.
  • 5 is a 1000-fold electron microscope image of granule powder in the range of 5 ⁇ m to 25 ⁇ m in accordance with a preferred embodiment of the present invention.
  • 6 is an electron microscope image of 300 times the powder of the plasma surface treatment of the granule powder in the range of 15 ⁇ m to 45 ⁇ m according to an embodiment of the present invention.
  • Figure 7 is an electron microscope image of 1000 times the powder of the plasma surface treatment of the granule powder in the range of 15 ⁇ m to 45 ⁇ m in accordance with a preferred embodiment of the present invention.
  • FIG. 8 is a schematic view of a cross section of a granular powder coated with an organic monomer according to an embodiment of the present invention.
  • FIG. 9 is a schematic view of a cross section of the plasma surface-treated granulated powder coated with an organic monomer according to an embodiment of the present invention.
  • FIG. 10 is a schematic diagram of an experimental apparatus for measuring the flow rate of the sprayed powder according to an embodiment of the present invention.
  • FIG. 11 is a cross-sectional image of a coating layer formed of a thermal spray coating using the thermal spray powder according to an embodiment of the present invention.
  • FIG. 12 is a cross-sectional image of the coating layer measured by enlarging the dash circle area of FIG. 11 according to an exemplary embodiment of the present invention.
  • FIG. 1 is a flowchart illustrating a process of coating an organic monomer on a sprayed powder surface according to an exemplary embodiment of the present invention.
  • the sprayed powder is manufactured by the spray drying method which is a conventional method.
  • the powder produced by spray drying is a powder in the form of granules, which is a powder in the form of an aggregate of fine powder.
  • the granular powder is calcined or calcined to be used as a sprayed powder.
  • the calcination process is 4 hours or less at 1200 ° C., and the firing process is then 4 hours or less at 1600 ° C., but the heat treatment step is performed according to the required properties of the thermal sprayed powder. This process can be carried out to prepare a sprayed powder.
  • the granulated powder is added to the solution in which the organic monomer is dissolved. After the granular powder is charged, the solution is stirred and the granular powder is allowed to sufficiently disperse in the solution.
  • the solution is heated to evaporate the solvent. Subsequently, the coating of the organic monomer on the surface of the thermal spray powder is completed so that the organic monomer is coated on the surface of the thermal spray powder.
  • Solvent evaporation does not occur at a high rate and is heated in a bath in order to uniformly heat the entire solution. The solvent evaporation rate varies depending on the total amount, but is controlled by process optimization.
  • the thermal sprayed powder After all of the solvent has evaporated, the thermal sprayed powder is in an apparent aggregated state. This can resolve the coagulation state through a sieving process or a simple disintegration process.
  • the amount of the organic monomer coating on the surface of the granular powder may be determined by adjusting the amount of the organic monomer added during preparation of the initial solution or the amount of the sprayed powder introduced into the solution.
  • Figure 2 is a 300 times electron microscope image of the granule powder in the range of 5 ⁇ m to 25 ⁇ m in accordance with a preferred embodiment of the present invention.
  • FIG. 2 it is an electron microscope image of the granulated powder prepared by the spray drying method, and the granular powder has a size distribution in the range of 5 ⁇ m to 25 ⁇ m.
  • Figure 3 is a 1000 times electron microscope image of the granule powder in the range of 5 ⁇ m to 25 ⁇ m in accordance with a preferred embodiment of the present invention.
  • the image on the electron microscope can be seen that there is a considerable level of internal pores, the surface area of the powder is large, it can be expected that the amount of static electricity due to friction between the powders. Electrostatic charges are generated due to excessive charge on the surface of the granular powder, and the frequency of contact between the powders is increased within a predetermined space so that the agglomeration of the granular powder is easily generated.
  • the powder is optimized for the thermal spray coating by using a powder whose change in powder surface state or powder distribution is optimized by the firing process of the granulated powder, but the quality or coating efficiency of the thermal spray coating is not improved.
  • Figure 4 is a 300 times electron microscope image of the granule powder in the range of 15 ⁇ m to 45 ⁇ m in accordance with a preferred embodiment of the present invention.
  • FIG. 4 it is an electron microscope image of the granulated powder prepared by the spray drying method, and the granular powder has a size distribution in the range of 15 ⁇ m to 45 ⁇ m.
  • 5 is a 1000-fold electron microscope image of granule powder in the range of 15 ⁇ m to 45 ⁇ m in accordance with one preferred embodiment of the present invention.
  • 6 is an electron microscope image of 300 times the powder of the plasma surface treatment of the granule powder in the range of 15 ⁇ m to 45 ⁇ m according to an embodiment of the present invention.
  • the size distribution of the sprayed powder plasma surface treatment is a spray powder in the range of 15 ⁇ m to 45 ⁇ m.
  • Figure 7 is an electron microscope image of 1000 times the powder of the plasma surface treatment of the granule powder in the range of 15 ⁇ m to 45 ⁇ m in accordance with a preferred embodiment of the present invention.
  • FIG. 8 is a schematic view of a cross section of a granular powder coated with an organic monomer according to an embodiment of the present invention.
  • FIG. 9 is a schematic view of a cross section of the plasma surface-treated granulated powder coated with an organic monomer according to an embodiment of the present invention.
  • this structure is a form in which the surfactant is adsorbed on the surface of the granulated powder in a micelle structure.
  • the micelle structure is a structure of an organic monomer adsorbed on the surface of the powder in which the part which is bonded to the surface of the powder is a hydrophobic part and the part which is in contact with air is a hydrophilic part.
  • the organic monomer is bonded to the surface of the granular powder.
  • the solvent is water, the surface of the granule powder adheres to the organic monomer of the lipophilic portion, and the hydrophilic portion is located toward the solvent. In this state, the granulated powder is dispersed in the solvent.
  • the sprayed powder is dispersed in the solution containing the organic monomer, and the solvent is slowly evaporated to obtain the sprayed powder coated with the organic monomer, thereby obtaining the sprayed powder coated with the organic monomer.
  • the surface of the granular powder coated with the organic monomer is not significantly reduced in the surface roughness, but the friction force between the granular powders is reduced due to the coating formed with the organic monomer, and due to the proper amount of electrostatic charge generated in the coating formed with the organic monomer, Agglomeration is in a controlled state.
  • FIG. 10 is a schematic diagram of an experimental apparatus for measuring the flow rate of the sprayed powder according to an embodiment of the present invention.
  • FIG. 10 it is a schematic diagram of a powder flow measurement apparatus including a sample cup 70 including a measuring funnel 100 loaded with powder and a specific gravity cup 60 containing free falling powder.
  • the sample cup 70 and the specific gravity cup 60 have a distance 80 between cups of 48 mm, and the internal volume of the specific gravity cup 60 is about 100 cc.
  • Standard measurement methods for fluidity characteristics are specified in KS L 1618-4. This standard is the result of the research of enactment of the KS standard for abrasive materials and special ceramic products, which is part of the standardized academic research service project conducted in 2002.
  • the diameter range of the granular powder of ceramic material is mostly 20 micrometers to 500 micrometers, this range is limited to tens to hundreds of micrometers, and most ceramic granules will be included in the diameter range of this granular powder.
  • the measurement procedure for measuring the flow rate of the powder is as follows. After filling the measurement funnel 100 with the measurement sample which is the thermal spray powder, the filling sample falls freely into the specific gravity cup 60 through the powder discharge port 90. The time for free fall of the powder is measured, and it is calculated by averaging three times in total.
  • the flow rate F is calculated to three decimal places according to the following equation, and after three measurements, the arithmetic average of the three measurement results is calculated.
  • F is the flow rate (g / s)
  • w 1 is the mass (g) of the specific gravity cup (60)
  • w 2 is the mass (g) of the sum of the samples dropped in the specific gravity cup (60) and the specific gravity cup (60).
  • t is the time it takes for the sample to fall (s, second). That is, w 2 -w 1 is the mass of the sample free falling into the specific gravity cup 60.
  • the solution is prepared using palmitic acid as an organic monomer material. 0.2g of palmitic acid is prepared, and the mixture is put into a beaker containing 200 ml of ethanol and dissolved by stirring for a sufficient time of about 0.5 hr. Note that the amount of ethanol is not excessively reduced during the dissolution of palmitic acid.
  • the size distribution of the powder produced by the above-described method was little different from the size distribution of the granulated powder initially introduced. Since the weight content of palmitic acid (CH 3 (CH 2 ) 14 COOH) is 0.2 wt% relative to the granular powder, the size of the granular powder is hardly increased.
  • the flow characteristics of the granitic powder coated with palmitic acid prepared as described above were measured. In the case of stabilized zirconia granule powder before palmitic acid coating, the measured value is almost zero with very low flow characteristics. In contrast, the granitic powder coated with palmitic acid significantly increased the flow characteristics, and the flow characteristics were measured as 1.0912 g / sec.
  • Electron microscopic images of the granitic powder coated with palmitic acid show an image similar to that of FIGS. 2 to 5.
  • the coating thickness of 0.2 wt% palmitic acid is very small, which is difficult to see by electron microscopy.
  • the surface roughness of the granular powder was measured to be 20 nm or more, and the surface roughness of the palmitic acid-coated granular powder was measured to be less than 20 nm. As a result, the coating of palmitic acid on the granular powder surface can be indirectly confirmed.
  • the coating amount of palmitic acid is preferably 0.01 wt% to 5.0 wt%, but is not limited thereto.
  • polystyrene polystyrene
  • a beaker containing 200 ml of ethanol agitation is performed for a sufficient time of about 0.5hr to dissolve the polystyrene (polystylene).
  • Polystyrene coating was performed on 100 g of stabilized zirconia granule powder in the same manner as in Example 1.
  • the flow characteristics of the prepared polystyrene-coated stabilized zirconia granule powder were carried out.
  • the flow characteristic value of the polystyrene coated stabilized zirconia granule powder was determined to be 0.4453 g / sec.
  • thermal spray powder prepared as described above was loaded on the plasma gun, and the thermal spray powder was discharged to prepare a thermal spray coating film.
  • the produced thermal spray coating film had an uneven surface, and a sharp protrusion was also observed. It is presumed that the quality of the thermal spray coating has occurred due to the clogging phenomenon or the partial aggregation of the thermal spray powder when the thermal spray powder is discharged. In order to improve the quality of a thermal sprayed coating, the flow characteristic of a thermal sprayed powder needs to be improved.
  • trimeric glycolic acid which is an oligomer polymerized with a small number of molecules, is prepared and introduced into a beaker containing 200 ml of ethanol, followed by a sufficient time of about 0.5hr to dissolve.
  • trimeric glycolic acid coating was performed on 100 g of stabilized zirconia granule powder.
  • the flow characteristics of trimeric glycolic acid coated stabilized zirconia granules were measured.
  • the flow characteristic value of the polystyrene coated stabilized zirconia granule powder was determined to be 0.6521 g / sec.
  • the flow characteristics were improved to a small level compared to the polymer coated granule powder, and showed good results as a spray powder applied to the thermal spray coating.
  • 0.2g of palmitic acid is prepared and added into a beaker containing 200 ml of ethanol, followed by a sufficient time of about 0.5hr to dissolve. Take care to maintain the amount of ethanol in the process of dissolving palmitic acid.
  • the flow characteristics of the granitic powder coated with palmitic acid prepared as described above were measured. In the case of stabilized zirconia granule powder before palmitc acid coating, the measured value is almost zero with very low flow characteristics. In contrast, the granitic powder coated with palmitic acid significantly increased the flow characteristics, and the flow characteristics were measured as 1.9084 g / sec.
  • the spray coating process was performed using the granitic powder coated with palmitic acid prepared as described above.
  • the coating amount of palmitic acid is preferably 0.01 wt% to 2.0 wt% relative to the isolated powder, but is not limited thereto.
  • FIG. 11 is a cross-sectional image of a coating layer formed of a thermal spray coating using the thermal spray powder according to an embodiment of the present invention.
  • FIG. 12 is a cross-sectional image of the coating layer measured by enlarging the dash circle area of FIG. 11 according to an exemplary embodiment of the present invention.
  • FIG. 12 is an enlarged image of the coating area 110. It can be seen that there is very little).
  • the pore content of the thermal sprayed coating layer using the granular powder in Example 2 was measured using an image analysis system, the pore content of about 5% was measured.
  • the thermal sprayed coating was prepared using the prepared thermal spray powder of Example 1, and the pore content of the thermal sprayed coating was measured to be 6% or more. This shows that the properties of the thermal sprayed coating can be controlled by controlling the flow characteristics of the thermal sprayed powder.
  • 0.2g of palmitic acid is prepared and added into a beaker containing 200 ml of ethanol, followed by a sufficient time of about 0.5hr to dissolve. Take care to maintain the amount of ethanol in the process of dissolving palmitic acid.
  • each of the stabilized stabilized zirconia granulated powder was plasma-treated into the ethanol solution in which palmitic acid was dissolved, and the mixture was stirred while stirring until the total powder was 100 g.
  • Plasma surface-treated stabilized zirconia granule powder was coated with palmitic acid using a size ranging from 15 ⁇ m to 45 ⁇ m. For a sufficient time of at least 1 hour, stirring was performed until the powder could be dispersed in solution.
  • the flow characteristics of the granitic powder coated with palmitic acid prepared as described above were measured.
  • Plasma surface-treated stabilized zirconia granules powder before palmitc acid was coated with very low flow characteristics, resulting in nearly zero measurements.
  • the plasma surface-treated stabilized zirconia granule powder coated with palmitic acid significantly increased the flow characteristics, and the flow characteristics were measured as 2.0152 g / sec.
  • the spray coating process was performed using the granitic powder coated with palmitic acid prepared as described above.
  • the thermal spray coating was performed using the powder prepared as described above, and the thermal spray coating film was evaluated, the pore internal content, which is the same level as the thermal spray coating prepared in Example 2, was measured to a value within 5%.
  • the organic monomer is coated on the surface of the granulated powder treated with plasma surface, and its flow characteristics are improved. This is due to the improved uniformity of the organic monomers coated on the powder surface.
  • the spray gun can be used for a longer time, and the quality of the sprayed coating can be improved. In addition, it becomes easier to control the properties of the thermal spray coating.
  • 0.2g of polystyrene is prepared and introduced into a beaker containing 200 ml of ethanol, followed by a sufficient time of about 0.5hr to dissolve.
  • Polystyrene coating was performed on 100 g of the stabilized zirconia granule powder subjected to the plasma surface treatment as in Example 1. In addition, the flow characteristics of the polystyrene-coated stabilized zirconia granule powder were measured. The flow characteristic value of the polystyrene coated stabilized zirconia granule powder was determined to be 0.4128 g / sec.
  • Tetraethyl orthosilicate (TEOS) or Hexamethyldisiloxane may be used to coat the granular powder surface. In this case as well, it shows improved flow characteristics.
  • the surface of the powder can be coated.
  • At least one selected from the group consisting of acid (C 21 H 43 COOH) may be used to coat the surface of the granular powder.
  • the granulated powder surface-coated with the organic monomer is loaded into the spray gun, and the sprayed spray process is performed by discharging the powder into the flame from the spray gun.
  • the powder for thermal spray coating is a thermal spray powder
  • the thermal spray powder may be a granulated powder coated with an organic monomer or a granulated powder coated with a plasma.
  • organic monomer 20 surface of granule powder

Abstract

L'invention concerne une poudre à fluidité élevée qui améliore la caractéristique d'écoulement d'une poudre de pulvérisation à introduire dans un pistolet de pulvérisation, de façon à améliorer la qualité d'un film de revêtement par pulvérisation, et un procédé de revêtement l'utilisant. La caractéristique d'écoulement de la poudre de pulvérisation peut être considérablement améliorée par application d'un monomère organique sur la surface d'une poudre de pulvérisation granulée, d'une poudre de pulvérisation traitée à la chaleur ou d'une poudre de pulvérisation traitée en surface par plasma. En outre, la caractéristique d'écoulement améliorée de la poudre de pulvérisation revêtue du monomère organique peut augmenter la compétitivité de la poudre de pulvérisation en termes de coût car le rendement de revêtement, la qualité d'une couche de revêtement et la durée d'utilisation du pistolet de pulvérisation sont augmentés.
PCT/KR2016/010071 2016-09-08 2016-09-08 Poudre de pulvérisation à fluidité élevée et son procédé de production WO2018047994A1 (fr)

Priority Applications (3)

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JP2018550758A JP6659872B2 (ja) 2016-09-08 2016-09-08 高流動性溶射用粒子及びその製造方法
KR1020187014428A KR102085258B1 (ko) 2016-09-08 2016-09-08 고유동성 용사용 입자 및 이의 제조 방법
PCT/KR2016/010071 WO2018047994A1 (fr) 2016-09-08 2016-09-08 Poudre de pulvérisation à fluidité élevée et son procédé de production

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PCT/KR2016/010071 WO2018047994A1 (fr) 2016-09-08 2016-09-08 Poudre de pulvérisation à fluidité élevée et son procédé de production

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KR102347575B1 (ko) * 2019-09-09 2022-01-06 대동산업 주식회사 도자타일용 고유동성 과립분말의 제조방법 및 도자타일의 제조방법

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