CN116854500B - Method for coating high expansion coefficient film on ZTA particle surface - Google Patents
Method for coating high expansion coefficient film on ZTA particle surface Download PDFInfo
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- CN116854500B CN116854500B CN202310805275.1A CN202310805275A CN116854500B CN 116854500 B CN116854500 B CN 116854500B CN 202310805275 A CN202310805275 A CN 202310805275A CN 116854500 B CN116854500 B CN 116854500B
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- 239000002245 particle Substances 0.000 title claims abstract description 157
- 239000011248 coating agent Substances 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000000576 coating method Methods 0.000 title claims abstract description 36
- 239000011521 glass Substances 0.000 claims abstract description 76
- 238000010438 heat treatment Methods 0.000 claims abstract description 38
- 238000000498 ball milling Methods 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000003723 Smelting Methods 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012634 fragment Substances 0.000 claims abstract description 12
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000011230 binding agent Substances 0.000 claims abstract description 8
- 238000010791 quenching Methods 0.000 claims abstract description 8
- 230000000171 quenching effect Effects 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 4
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000004327 boric acid Substances 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 41
- 239000000919 ceramic Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 14
- 239000010935 stainless steel Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 6
- 239000005011 phenolic resin Substances 0.000 claims description 6
- 229920001568 phenolic resin Polymers 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 description 31
- 229910000617 Mangalloy Inorganic materials 0.000 description 26
- 239000011159 matrix material Substances 0.000 description 25
- 238000005266 casting Methods 0.000 description 16
- 239000000843 powder Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 230000008569 process Effects 0.000 description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 238000007598 dipping method Methods 0.000 description 6
- 239000011572 manganese Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 238000003892 spreading Methods 0.000 description 6
- 230000007480 spreading Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 238000009472 formulation Methods 0.000 description 5
- 230000008646 thermal stress Effects 0.000 description 5
- 229910000859 α-Fe Inorganic materials 0.000 description 5
- 239000002223 garnet Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000011819 refractory material Substances 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 244000035744 Hura crepitans Species 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- KCZFLPPCFOHPNI-UHFFFAOYSA-N alumane;iron Chemical compound [AlH3].[Fe] KCZFLPPCFOHPNI-UHFFFAOYSA-N 0.000 description 3
- 229910052810 boron oxide Inorganic materials 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 3
- 229910001948 sodium oxide Inorganic materials 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000007669 thermal treatment Methods 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000012856 weighed raw material Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
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- 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
- C23D—ENAMELLING OF, OR APPLYING A VITREOUS LAYER TO, METALS
- C23D5/00—Coating with enamels or vitreous layers
- C23D5/02—Coating with enamels or vitreous layers by wet methods
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/86—Glazes; Cold glazes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The invention provides a method for coating a high expansion coefficient film on the surface of ZTA particles, which comprises the following steps: after carrying out first ball milling on raw materials of the glass frit, placing the raw materials in an environment of 1000-1050 ℃, further heating the environment to 1400-1450 ℃, and preserving heat to obtain a smelting glass frit; quenching the smelted glass frit with water to obtain glass frit fragments; mixing the glass frit fragments with a surfactant and a binder in water, and performing a second ball milling to obtain a surface coating agent; coating a surface coating agent on the surfaces of ZTA particles; heat treatment of ZTA particles after surface coating; the raw materials of the glass frit comprise 30-35% of ferric silicate, 30-40% of silicon dioxide, 10-15% of boric acid, 8-10% of sodium carbonate, 5-6% of aluminum oxide and 3-5% of vanadium pentoxide.
Description
Technical Field
The invention belongs to the field of ceramic materials, and particularly relates to a method for coating a high expansion coefficient film on the surface of ZTA particles.
Background
Zirconia toughened alumina ceramic (ZTA) is a ceramic obtained by adding a proper amount of zirconia to alumina and then sintering the mixture. The ZTA ceramic has high hardness and better toughness than common ceramics, and is mainly a toughening mechanism of zirconium oxide in aluminum oxide, wherein the toughening mechanism can generate phase change toughening, aluminum oxide grain refinement, crack steering, bifurcation and the like. Because of high toughness and reasonable preparation cost of ZTA ceramic, in recent years ZTA ceramic particles are often used as a reinforcing phase for preparing ceramic particle reinforced high manganese steel-based composite materials, and the ZTA ceramic particles are applied to wear-resistant materials in the fields of mining, industrial crushing and the like.
At present, a ZTA ceramic particle reinforced high manganese steel matrix composite material is prepared by a common hot casting method, and the technology is as follows: (1) Mixing ZTA particles with a special adhesive, forming a porous ceramic particle preform, and fixing the ceramic particle preform into a cavity of a sand box before casting; (2) Pouring high manganese steel-based molten metal into a sand box from a pouring gate at a constant speed, wherein the molten metal enters ZTA particle gaps under the simultaneous actions of capillary effect and self gravity of molten metal; (3) Gradually cooling for a period of time, separating the sand box and the composite material casting, cutting off unnecessary parts, and completing the preparation of the ZTA particle/high manganese steel-based composite material.
The process for preparing the ZTA particle/high manganese steel-based composite material is simple, the content and the distribution of the ZTA particle are controllable, and large-size ZTA particle/high manganese steel-based composite material products can be prepared, but the thermal expansion coefficient of the ZTA particle is 7.8-8.5X10 -6/K, the expansion coefficient of a high manganese steel matrix is 15.0-20.3X10 -6/K, the difference of the expansion coefficients of the ZTA particle and the high manganese steel-based composite material is large, and the ZTA particle/high manganese steel-based composite material prepared by a hot casting method is often cracked at a material interface because of the overlarge difference of the expansion coefficients of two-phase materials, so that the bending strength of the composite material is greatly reduced, and the application field and the use performance of the ZTA particle/high manganese steel-based composite material are limited.
Disclosure of Invention
The invention aims to provide an inorganic material film which is coated on the surfaces of ZTA ceramic particles, firmly combined with a layer of ZTA particles and has an expansion coefficient of more than 10 multiplied by 10 -6/K.
The invention is realized by the following technical scheme:
A method for coating a high expansion coefficient film on the surface of ZTA particles, comprising the steps of:
After carrying out first ball milling on raw materials of the glass frit, placing the raw materials in an environment of 1000-1050 ℃, further heating the environment to 1400-1450 ℃, and preserving heat to obtain a smelting glass frit;
quenching the smelted glass frit with water to obtain glass frit fragments;
mixing the glass frit fragments with a surfactant and a binder in water, and performing a second ball milling to obtain a surface coating agent;
coating a surface coating agent on the surfaces of ZTA particles and drying;
Heat treatment of ZTA particles after surface coating;
the raw materials of the glass frit comprise 30-35% of ferric silicate, 30-40% of silicon dioxide, 10-15% of boric acid, 8-10% of sodium carbonate, 5-6% of aluminum oxide and 3-5% of vanadium pentoxide.
The ball material mass ratio of the first ball mill is 2:1;
The rotating speed of the first ball mill is 30-40r/min;
the first ball milling time is 1-2h;
the grinding balls used for the first ball milling comprise stainless steel balls.
The method for coating the high expansion coefficient film on the surfaces of the ZTA particles comprises the steps of further heating the environment temperature to 1400-1450 ℃ at the speed of 2-5 ℃/min and preserving heat for 1-2 h.
The surface coating agent comprises 50-63% of glass frit fragments, 2-4% of surfactant, 5-6% of binder and 30-40% of water.
The binder comprises a water-soluble phenolic resin;
The surfactant includes polyethylene glycol 400.
The ball-material ratio of the second ball mill is 1.5:1;
the rotating speed of the second ball milling is 270-300r/min;
The second ball milling time is 12-16h.
The method for coating the high expansion coefficient film on the surfaces of the ZTA particles comprises the steps of immersing the ZTA particles in the surface coating agent, drying for 8-12h at room temperature, then drying for 2-4h at 80 ℃, heating to 120-140 ℃, preserving heat for 2-3h, and naturally cooling.
The heat treatment comprises the steps of heating to 400-450 ℃ at the speed of 2-3 ℃/min, preserving heat for 30-60min, heating to 1300-1350 ℃ at the speed of 4-5 ℃/min, preserving heat for 1-2h, cooling to 1200-1250 ℃ at the speed of 5-10 ℃/min, and preserving heat for 2-3 h.
The method for coating the high expansion coefficient film on the surfaces of the ZTA particles further comprises the step of cleaning the surfaces of the ZTA particles.
The method for coating the high expansion coefficient film on the surfaces of the ZTA particles comprises the steps of soaking the ZTA ceramic particles in absolute ethyl alcohol with the concentration of 5wt%, ultrasonically cleaning for 20-40 minutes at the frequency of 2000-4000Hz, and then drying at 80 ℃.
Compared with the prior art, the invention has the following beneficial effects:
The invention adopts the inorganic material film which is coated on the surface of ZTA ceramic particles and firmly combined with a layer of ZTA particles, and has the expansion coefficient of more than 10 multiplied by 10 -6/K. When the coated ZTA particles are used as reinforcements and the ZTA particle/high manganese steel matrix composite material is prepared by adopting a hot casting method, the film material on the surface of the ZTA particles can be well wetted with the high manganese steel matrix, and meanwhile, the film material with high expansion coefficient is used as a buffer layer between the ZTA particles and the high manganese steel matrix, so that the thermal stress between the ZTA particles and the high manganese steel in the ZTA particle/high manganese steel matrix composite material is reduced, the crack generation of an interface layer is restrained, and the bending strength of the composite material is greatly improved.
Drawings
Figure 1 XRD pattern of ZTA particles of the surface-coated film after heat treatment in example 1. The pictures show that the iron-aluminum garnet crystals are precipitated in the film layer after heat treatment.
Figure 2 surface topography of ZTA particles of the heat treated surface coated film of example 1. The pictures show that a large number of needle-shaped crystals are precipitated in the film layer after heat treatment, and the needle-shaped crystals are iron aluminum garnet crystals in combination with the picture 1.
Figure 3 interfacial morphology of the heat treated surface coated film and ZTA particles in example 1. The pictures show that the film layer after heat treatment has compact and straight interface with ZTA, no air holes and impurities and better interface combination.
Fig. 4 is a graph showing the expansion coefficient of the bulk material prepared by the same heat treatment process using the same glass frit as the ZTA particle surface film composition in example 1. The graph shows that the expansion coefficient of the film is 11.6238 X10: 10 -6/K in the temperature measuring range of 25-460 ℃, and the expansion coefficient of the film on the surface of the ZTA particle is higher than that of the film on the surface of the ZTA particle which is prepared into a block material by adopting the glass powder with the same component as that of the film on the surface of the ZTA particle through the same heat treatment process by adopting equivalent replacement, and the result shows that the expansion coefficient of the film on the surface of the ZTA particle is higher than that of the film on the surface of the ZTA particle which is about 11.6238X 10 -6/K.
FIG. 5 shows the morphology of the ZTA particle-Mn 13 matrix interface in the ZTA/Fe matrix composite prepared by ZTA particles in example 1; the pictures show that the film layer on the surface of the ZTA particles has good combination with Mn13 matrix, and serves as a transition layer between the ZTA particles and Mn13 with high expansion coefficient, and thermal stress cracks do not appear at the interface in the ZTA particles/Mn 13 iron-based composite material prepared by a fusion casting method.
FIG. 6 shows the morphology of ZTA particle-Mn 13 matrix interfaces in a commercially available ZTA particle/Mn 13 iron based composite; the pictures show that thermal stress cracks can appear at the interface close to ZTA particles in the ZTA particle/Mn 13 iron-based composite material prepared by the fusion casting method due to the large difference of the expansion coefficients of the ZTA particles and the Mn13 matrix.
Detailed Description
The method provided by the invention comprises the following steps:
(1) Surface cleaning of ZTA particles
The ZTA ceramic particles with the particle size of 10-14# are soaked in absolute ethanol with the concentration of 5wt% at room temperature, ultrasonically cleaned for 20-40 minutes at the frequency of 2000-4000Hz, and oil stains on the surfaces of the ZTA particles are removed, so that a preparation is made for coating a film on the surfaces of the ZTA particles.
(2) Smelting of ZTA particle surface coated glass frit
The ZTA surface coating glass frit is prepared by adopting a high-temperature smelting method, and the glass frit comprises the following components in percentage by weight:
After various raw materials are uniformly mixed, smelting is carried out in a crucible furnace at 1400-1450 ℃, wherein, silicon oxide and silicon dioxide provide silicon oxygen tetrahedron into the coated glass material to form a main network structure of the glass material, meanwhile, the silicon oxide provides ferrite octahedron into the glass material to enable the ferrite octahedron to exist in gaps of a glass network, and ferric oxide is introduced into the glass material in the form of ferric silicate, so that the glass material with higher ferric oxide content can be obtained at a lower smelting temperature. Boric acid and aluminum oxide can be combined with sodium oxide generated after sodium carbonate is decomposed in the glass frit smelting process to generate boron oxide tetrahedron and aluminum oxide tetrahedron, and the boron oxide tetrahedron and the aluminum oxide tetrahedron form a glass network structure together, and the addition of the boron oxide tetrahedron and the aluminum oxide tetrahedron can improve the stability of the formed glass frit and prevent crystallization of the glass frit in the smelting process. Vanadium pentoxide is a crystallization agent and a fluxing agent of the glass frit, and on one hand, the crystallization of the glass frit is promoted in the subsequent heat treatment process; on the other hand, vanadium pentoxide exists in the glass in a layered structure, so that the integrity of a glass network structure is damaged, and the smelting temperature of the glass frit is reduced. And (5) flowing the smelted glass frit into a heat-resistant steel water tank for water quenching to obtain water quenched glass frit fragments.
(3) Preparation of ZTA particle surface coating agent
The ZTA particle surface coating agent is prepared by adopting a stirring method, and the coating agent comprises the following components in percentage by weight:
the coated glass frit fragments are crushed in the subsequent ball milling process to become micro powder, deionized water is used as a dispersion medium of glass powder, polyethylene glycol is a dispersing agent of the glass micro powder, the polyethylene glycol is adsorbed on the surface of the glass micro powder in the ball milling process, the surface energy of the glass micro powder is reduced, the ball milling crushing efficiency of the glass micro powder is improved, the glass micro powder is prevented from agglomerating through the steric hindrance effect, and the suspension property of the glass micro powder in the coating agent is improved. The water-soluble phenolic resin is a temporary binder in the coating agent. And (3) after the ball-milled slurry passes through a 400# screen mesh, obtaining the ZTA particle surface coating agent.
(4) Coating treatment of ZTA particle surfaces
At room temperature, dipping the ZTA particles with the surface cleaned obtained in the step 1 into the surface coating agent prepared in the step 3, taking out the ZTA particles from the coating agent by using a stainless steel screen after dipping for 1-2 minutes, coating a layer of coating agent on the surfaces of the ZTA particles, spreading the dipped ZTA particles on a No. 24 screen, drying for 8-12 hours at room temperature, preliminarily removing water in a coating agent film layer, then placing in an oven, drying for 2-4 hours at 80 ℃, further removing water in the coating agent film layer, and simultaneously, carrying out primary curing on phenolic resin in the coating agent film layer, wherein the film layer and the ZTA particles have certain bonding strength, heating to 120-140 ℃ and preserving heat for 2-3 hours, completely curing the phenolic resin, firmly adhering the coating agent film layer on the surfaces of the ZTA particles, and facilitating subsequent process operation.
(5) Thermal treatment of ZTA coated particles
And (3) spreading the ZTA coated particles obtained in the step (4) on a SiC refractory material plate with BN fine powder on the surface, and putting the SiC refractory material plate into a box-type electric furnace, wherein the BN fine powder prevents the ZTA coated particles from adhering to the SiC plate in the heat treatment process. Heating to 400-450 ℃ at the speed of 2-3 ℃/min, and preserving heat for 30-60min, wherein the temperature is slowly increased in the temperature interval, and polyethylene glycol and phenolic resin are gradually cracked and oxidized, so that the cracking of a film layer caused by the excessively rapid temperature increase is prevented. Heating to 1300-1350 ℃ at the speed of 4-5 ℃/min, preserving heat for 1-2h, and softening the glass frit on the surfaces of the ZTA particles at the preserving heat to become a low-viscosity fluid, wherein the glass frit film layer contains a certain amount of sodium oxide, so that the sodium oxide can provide 'free oxygen' for the alumina on the ZTA surface to form Na-O-Al bonds, and the wettability and binding force between the glass frit film layer and the ZTA particles are improved. Then cooling to 1200-1250 ℃ at the speed of 5-10 ℃/min, and preserving heat for 2-3h, wherein a large amount of ferrite octahedrons exist in gaps of a glass network structure in a glass material film layer, and V 5+ exists in the glass material, so that the glass material has more positive charges and stronger aggregation effect on surrounding O 2-, the ferrite octahedrons in the glass network gaps are promoted to aggregate to the periphery of the glass material, the glass material starts to phase separation, and a ferrite aluminum garnet phase with a larger expansion coefficient is separated, so that ZTA particles with the surfaces coated with the microcrystalline glass film with the high expansion coefficient are obtained.
The application is further illustrated below with reference to specific examples.
Example 1
The embodiment provides a technology for coating a high expansion coefficient film on the surface of ZTA particles, which comprises the following specific steps:
(1) Surface cleaning of ZTA particles
ZTA ceramic particles with particle size of 12-14# are soaked in absolute ethanol with concentration of 5wt% at room temperature, ultrasonically cleaned for 20 minutes at a frequency of 3000Hz, and then dried in an 80-degree oven, thus finishing the surface cleaning of the ZTA particles.
(2) Smelting of ZTA particle surface coated glass frit
The ZTA surface coating glass frit is prepared by adopting a high-temperature smelting method, and the glass frit comprises the following components in percentage by weight:
Pouring the weighed raw materials into a stainless steel ball milling jar with the diameter of 400mm, adding stainless steel balls with the diameter of 10mm according to the mass ratio of 2:1, and enabling the rotation speed of the ball milling jar to be 40r/min. And ball milling the raw materials for 2 hours, and taking out to obtain the coated glass frit smelting raw materials.
Heating the crucible furnace to 1050 ℃ at the speed of 8 ℃/min, plugging a material rod, pouring mixed smelting raw material powder, heating the furnace to 1450 ℃ at the speed of 5 ℃/min, preserving heat for 1h, lifting the material rod, allowing the smelted glass material to flow into a heat-resistant molten steel tank for water quenching, collecting the glass material fragments after water quenching, and drying for later use.
(3) Preparation of ZTA particle surface coating agent
The ZTA particle surface coating agent is prepared by adopting a stirring method, and the coating agent comprises the following components in percentage by weight:
Respectively weighing the raw materials according to the proportion, pouring the raw materials into a corundum ball milling jar with the diameter of 400mm, adding zirconia balls with the diameter of 10-20mm according to the mass ratio of the balls to the glass frit of 1.5:1, and enabling the rotation speed of the ball milling jar to be 300r/min. After ball milling for 12 hours, the ground slurry is filtered by a 400# screen mesh to obtain the ZTA particle surface coating agent.
(4) Coating treatment of ZTA particle surfaces
At room temperature, dipping the ZTA particles with the surface cleaned obtained in the step 1 in the surface coating agent prepared in the step 3, fishing out the ZTA particles from the coating agent by using a stainless steel screen after dipping for 2 minutes, spreading the dipped ZTA particles on a No. 24 screen, drying for 12 hours at room temperature, then placing the ZTA particles in a drying oven, drying for 4 hours at 80 ℃, then heating to 140 ℃ and preserving heat for 2 hours, taking out the ZTA particles, and naturally cooling at room temperature to finish the surface coating treatment of the ZTA particles.
(5) Thermal treatment of ZTA coated particles
Spreading the ZTA coated particles obtained in the step 4 on a SiC refractory material plate with BN fine powder on the surface, putting the plate into a box-type electric furnace, heating to 450 ℃ at a speed of 3 ℃/min, preserving heat for 30min, heating to 1300 ℃ at a speed of 5 ℃/min, preserving heat for 2h, cooling to 1250 ℃ at a speed of 10 ℃/min, preserving heat for 3h, cooling Guan Lu along with the furnace, and obtaining ZTA particles with high expansion coefficient films coated on the surface.
From fig. 1 and fig. 2, it can be seen that a layer of compact microcrystalline film with iron aluminum garnet crystals precipitated can be formed on the surface of ZTA particles by adopting the process of the invention, fig. 3 shows that the film can form good interface bonding with ZTA particles after heat treatment, and fig. 4 shows that the film material has a larger expansion coefficient.
Putting the ZTA particles prepared in the embodiment 1 into a mixer, adding a certain amount of water glass, uniformly mixing, putting into a porous ceramic preform forming die, forming under 5-10MPa pressure, solidifying at 80 ℃ for 4 hours, demoulding to obtain the ZTA particle porous ceramic preform, fixing the preform at a designated part of a casting mould sand mould, casting Mn13 ferroalloy melt into the sand mould, casting at 1480 ℃, cooling the casting, cutting a ZTA/Fe-based composite mechanical test strip by a water knife, wherein the test strip size is 20 multiplied by 150mm, grinding the surface of the test strip by a vertical grinder, the surface roughness Ra0.2mu m of the test strip, and measuring the tensile strength of the test strip on a comprehensive mechanical testing machine, wherein the average tensile strength of the 5 mechanical test strips is 320MPa. Fig. 5 shows that the high expansion coefficient film on the surface of the ZTA particles can achieve good wetting with the Mn13 matrix, and simultaneously act as a transition layer between the ZTA particles and the high expansion coefficient Mn13, so that the thermal stress between the ZTA particles and the Mn13 matrix can be effectively reduced, and stress cracks at the ZTA particle interface are avoided.
Putting commercially available 12-14# ZTA particles into a mixer, adding a certain amount of water glass, uniformly mixing, putting into a porous ceramic preform forming die, forming under 5-10MPa pressure, solidifying at 80 ℃ for 4 hours, demoulding to obtain a ZTA particle porous ceramic preform, fixing the preform at a designated part of a casting mould sand mould, casting Mn13 iron alloy melt into the sand mould, casting at 1480 ℃, cooling the casting, cutting a ZTA/Fe-based composite mechanical test strip by a water knife, wherein the size of the test strip is 20 multiplied by 150mm, grinding the surface of the test strip by a vertical grinder, and the surface roughness Ra0.2mu m of the test strip, and then measuring the tensile strength of the test strip on a comprehensive mechanical tester, wherein the average tensile strength of the 5 mechanical test strips is 280MPa. Fig. 6 shows that the difference between the expansion coefficients of the common ZTA particles and the Mn13 matrix is large, and thermal stress cracks can occur at the interface close to the ZTA particles in the ZTA particle/Mn 13 iron-based composite material prepared by the fusion casting method.
Example 2
The embodiment provides a technology for coating a high expansion coefficient film on the surface of ZTA particles, which comprises the following specific steps:
(1) Surface cleaning of ZTA particles
ZTA ceramic particles with particle size of 12-14# are soaked in absolute ethanol with concentration of 5wt% at room temperature, ultrasonically cleaned for 40 minutes at a frequency of 2000Hz, and then dried in an 80-degree oven, thus finishing the surface cleaning of the ZTA particles.
(2) Smelting of ZTA particle surface coated glass frit
The ZTA surface coating glass frit is prepared by adopting a high-temperature smelting method, and the glass frit comprises the following components in percentage by weight:
Pouring the weighed raw materials into a stainless steel ball milling jar with the diameter of 400mm, adding stainless steel balls with the diameter of 10mm according to the mass ratio of 2:1, and enabling the rotation speed of the ball milling jar to be 30r/min. And ball milling the raw materials for 1h, and taking out to obtain the coated glass frit smelting raw materials.
Heating the crucible furnace to 1000 ℃ at the speed of 5 ℃/min, plugging a material rod, pouring mixed smelting raw material powder, heating the furnace temperature to 1400 ℃ at the speed of 2 ℃/min, preserving heat for 2h, lifting the material rod, allowing the smelted glass material to flow into a heat-resistant molten steel tank for water quenching, collecting the glass material fragments after water quenching, and drying for later use.
(3) Preparation of ZTA particle surface coating agent
The ZTA particle surface coating agent is prepared by adopting a stirring method, and the coating agent comprises the following components in percentage by weight:
Respectively weighing the raw materials according to the proportion, pouring the raw materials into a corundum ball milling jar with the diameter of 400mm, adding zirconia balls with the diameter of 10-20mm according to the mass ratio of the balls to the glass frit of 1.5:1, and enabling the rotation speed of the ball milling jar to be 270r/min. After ball milling for 16 hours, the ground slurry was filtered with a 400# screen to obtain a ZTA particle surface coating agent.
(4) Coating treatment of ZTA particle surfaces
At room temperature, dipping the ZTA particles with the surface cleaned obtained in the step 1 in the surface coating agent prepared in the step 3, fishing out the ZTA particles from the coating agent by using a stainless steel screen after dipping for 1 minute, spreading the dipped ZTA particles on a No. 24 screen, drying for 8 hours at room temperature, then placing the dried ZTA particles in a drying oven, drying for 2 hours at 80 ℃, then heating to 120 ℃ and preserving heat for 3 hours, taking out the ZTA particles, and naturally cooling at room temperature to finish the surface coating treatment of the ZTA particles.
(5) Thermal treatment of ZTA coated particles
Spreading the ZTA coated particles obtained in the step 4 on a SiC refractory material plate with BN fine powder on the surface, putting the plate into a box-type electric furnace, heating to 400 ℃ at a speed of 2 ℃/min, preserving heat for 60min, heating to 1350 ℃ at a speed of 5 ℃/min, preserving heat for 1h, cooling to 1200 ℃ at a speed of 5 ℃/min, preserving heat for 2h, cooling Guan Lu along with the furnace, and obtaining ZTA particles with high expansion coefficient films coated on the surface.
A ZTA particle/high manganese steel matrix composite material was prepared in the same manner as in example 1, and the tensile strength of the obtained material was 323MPa.
Example 3
The difference from example 1 is that the weight percentage formulation of the frit is as follows:
a ZTA particle/high manganese steel matrix composite was prepared in the same manner as in example 1, and the tensile strength of the obtained material was 325MPa.
Example 4
The difference from example 1 is that the weight percentage formulation of the frit is as follows:
A ZTA particle/high manganese steel matrix composite was prepared in the same manner as in example 1, and the tensile strength of the obtained material was 317MPa.
Example 5
The difference from example 1 is that the weight percentage formulation of the frit is as follows:
A ZTA particle/high manganese steel matrix composite was prepared in the same manner as in example 1, and the tensile strength of the obtained material was 322MPa.
Example 6
The difference from example 1 is that the weight percentage formulation of the frit is as follows:
A ZTA particle/high manganese steel matrix composite was prepared in the same manner as in example 1, and the tensile strength of the obtained material was 327MPa.
Example 7
The difference from example 1 is that the weight percentage formulation of the frit is as follows:
A ZTA particle/high manganese steel matrix composite was prepared in the same manner as in example 1, and the tensile strength of the obtained material was 319MPa.
Example 8
The difference from example 1 is that the coating agent is formulated in weight percent as follows:
A ZTA particle/high manganese steel matrix composite was prepared in the same manner as in example 1, and the tensile strength of the obtained material was 328MPa.
Example 9
The difference from example 1 is that the coating agent is formulated in weight percent as follows:
A ZTA particle/high manganese steel matrix composite was prepared in the same manner as in example 1, and the tensile strength of the obtained material was 333MPa.
Example 10
The difference from example 1 is that the coating agent is formulated in weight percent as follows:
a ZTA particle/high manganese steel matrix composite was prepared in the same manner as in example 1, and the tensile strength of the obtained material was 325MPa.
Example 11
The difference from example 1 is that the coating agent is formulated in weight percent as follows:
A ZTA particle/high manganese steel matrix composite was prepared in the same manner as in example 1, and the tensile strength of the obtained material was 330MPa.
Example 12
The difference from example 1 is that the coating agent is formulated in weight percent as follows:
A ZTA particle/high manganese steel matrix composite was prepared in the same manner as in example 1, and the tensile strength of the obtained material was 326MPa.
Claims (9)
1. A method for coating a high expansion coefficient film on the surface of ZTA particles, which is characterized by comprising the following steps:
After carrying out first ball milling on raw materials of the glass frit, placing the raw materials in an environment of 1000-1050 ℃, further heating the environment to 1400-1450 ℃, and preserving heat to obtain a smelting glass frit;
quenching the smelted glass frit with water to obtain glass frit fragments;
mixing the glass frit fragments with a surfactant and a binder in water, and performing a second ball milling to obtain a surface coating agent;
coating a surface coating agent on the surfaces of ZTA particles and drying;
Heat treatment of ZTA particles after surface coating;
the raw materials of the glass frit comprise 30-35% of ferric silicate, 30-40% of silicon dioxide, 10-15% of boric acid, 8-10% of sodium carbonate, 5-6% of aluminum oxide and 3-5% of vanadium pentoxide;
The heat treatment comprises the steps of heating to 400-450 ℃ at the speed of 2-3 ℃/min, preserving heat for 30-60min, heating to 1300-1350 ℃ at the speed of 4-5 ℃/min, preserving heat for 1-2h, cooling to 1200-1250 ℃ at the speed of 5-10 ℃/min, and preserving heat for 2-3 h.
2. The method for coating the surfaces of ZTA particles with a high expansion coefficient film according to claim 1, which is characterized in that:
the ball material mass ratio of the first ball mill is 2:1;
The rotating speed of the first ball mill is 30-40r/min;
the first ball milling time is 1-2h;
the grinding balls used for the first ball milling comprise stainless steel balls.
3. The method for coating the surfaces of ZTA particles with a high expansion coefficient film according to claim 1, which is characterized in that:
Further heating the environment temperature to 1400-1450 ℃ at the speed of 2-5 ℃/min and preserving the heat for 1-2h to obtain the smelting glass material.
4. The method for coating the surfaces of ZTA particles with a high expansion coefficient film according to claim 1, which is characterized in that:
the surface coating agent comprises 50-63% of glass frit fragments, 2-4% of surfactant, 5-6% of binder and 30-40% of water.
5. The method for coating the surfaces of the ZTA particles with the high expansion coefficient film as set forth in claim 4, which is characterized in that:
the binder comprises a water-soluble phenolic resin;
The surfactant includes polyethylene glycol 400.
6. The method for coating the surfaces of ZTA particles with a high expansion coefficient film according to claim 1, which is characterized in that:
The ball-material ratio of the second ball mill is 1.5:1;
the rotating speed of the second ball milling is 270-300r/min;
The second ball milling time is 12-16h.
7. The method for coating the surfaces of ZTA particles with a high expansion coefficient film according to claim 1, which is characterized in that:
comprises the steps of immersing ZTA particles in the surface coating agent, drying for 8-12h at room temperature, then drying for 2-4h at 80 ℃, heating to 120-140 ℃ and preserving heat for 2-3h, and naturally cooling.
8. The method for coating the surfaces of ZTA particles with a high expansion coefficient film according to claim 1, which is characterized in that:
Further comprising a step of surface cleaning of the ZTA particles.
9. The method for coating the surfaces of ZTA particles with a high expansion coefficient film according to claim 8, which is characterized in that:
comprises the steps of soaking ZTA ceramic particles in absolute ethanol with the concentration of 5wt%, ultrasonic cleaning for 20-40 minutes at the frequency of 2000-4000Hz, and drying at 80 ℃.
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| CN104276839A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | Sealing method for ceramic vitrification |
| CN111020360A (en) * | 2019-12-23 | 2020-04-17 | 昆明理工大学 | Non-infiltration type ceramic particle reinforced steel-based composite material and preparation method thereof |
| CN218063883U (en) * | 2022-08-15 | 2022-12-16 | 湖南西拓新材料科技有限公司 | Lightweight wear-resistant ceramic pump truck pipeline |
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| EP0161578A3 (en) * | 1984-05-02 | 1987-11-19 | Rutgers, The State University | Glass coated ceramic particles |
| CN104276838B (en) * | 2013-07-12 | 2016-01-06 | 中国科学院上海硅酸盐研究所 | Pottery vitrified method for sealing two with metal |
| CN108585808A (en) * | 2018-04-03 | 2018-09-28 | 昆明理工大学 | A kind of preparation method with the good modified ZTA complex phase ceramics of steel fusant wetability |
| CN111809100B (en) * | 2020-07-17 | 2022-02-11 | 西安交通大学 | NiCrAlY high-temperature sintered ZTA particle reinforced steel-based composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104276839A (en) * | 2013-07-12 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | Sealing method for ceramic vitrification |
| CN111020360A (en) * | 2019-12-23 | 2020-04-17 | 昆明理工大学 | Non-infiltration type ceramic particle reinforced steel-based composite material and preparation method thereof |
| CN218063883U (en) * | 2022-08-15 | 2022-12-16 | 湖南西拓新材料科技有限公司 | Lightweight wear-resistant ceramic pump truck pipeline |
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