CN117985949B - Silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder and preparation method thereof - Google Patents
Silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder and preparation method thereof Download PDFInfo
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- CN117985949B CN117985949B CN202410399308.1A CN202410399308A CN117985949B CN 117985949 B CN117985949 B CN 117985949B CN 202410399308 A CN202410399308 A CN 202410399308A CN 117985949 B CN117985949 B CN 117985949B
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- 239000000843 powder Substances 0.000 title claims abstract description 73
- 238000005507 spraying Methods 0.000 title claims abstract description 53
- -1 Silicon yttrium aluminum chromium magnesium oxide Chemical compound 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 29
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 25
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 24
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000000706 filtrate Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000011230 binding agent Substances 0.000 claims abstract description 17
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007921 spray Substances 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 7
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 7
- 239000011029 spinel Substances 0.000 claims abstract description 7
- LESLIVVVRHWISC-UHFFFAOYSA-N [O--].[O--].[O--].[Cr+3].[Y+3] Chemical compound [O--].[O--].[O--].[Cr+3].[Y+3] LESLIVVVRHWISC-UHFFFAOYSA-N 0.000 claims abstract description 6
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 claims abstract description 6
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims abstract description 5
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 22
- 229910052573 porcelain Inorganic materials 0.000 claims description 20
- 239000013078 crystal Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 15
- 239000011268 mixed slurry Substances 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 2
- 238000000576 coating method Methods 0.000 abstract description 44
- 239000011248 coating agent Substances 0.000 abstract description 43
- 239000011521 glass Substances 0.000 abstract description 36
- 239000000758 substrate Substances 0.000 abstract description 22
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 abstract description 20
- 238000005530 etching Methods 0.000 abstract description 12
- 230000007704 transition Effects 0.000 abstract description 10
- 230000009286 beneficial effect Effects 0.000 abstract description 9
- 238000002468 ceramisation Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 229910000000 metal hydroxide Inorganic materials 0.000 description 9
- 150000004692 metal hydroxides Chemical class 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000001556 precipitation Methods 0.000 description 8
- 238000005245 sintering Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 230000035882 stress Effects 0.000 description 6
- 239000002002 slurry Substances 0.000 description 5
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- GVHCUJZTWMCYJM-UHFFFAOYSA-N chromium(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GVHCUJZTWMCYJM-UHFFFAOYSA-N 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- QBAZWXKSCUESGU-UHFFFAOYSA-N yttrium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QBAZWXKSCUESGU-UHFFFAOYSA-N 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910000423 chromium oxide Inorganic materials 0.000 description 2
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- DEXZEPDUSNRVTN-UHFFFAOYSA-K yttrium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Y+3] DEXZEPDUSNRVTN-UHFFFAOYSA-K 0.000 description 2
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- WVMWBQHUTLGEFF-UHFFFAOYSA-N [O-2].[Cr+3].[O-2].[Y+3] Chemical compound [O-2].[Cr+3].[O-2].[Y+3] WVMWBQHUTLGEFF-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- GSWGDDYIUCWADU-UHFFFAOYSA-N aluminum magnesium oxygen(2-) Chemical compound [O--].[Mg++].[Al+3] GSWGDDYIUCWADU-UHFFFAOYSA-N 0.000 description 1
- DVZCSECSHMWCTC-UHFFFAOYSA-N aluminum;magnesium;chromium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mg+2].[Al+3].[Cr+3] DVZCSECSHMWCTC-UHFFFAOYSA-N 0.000 description 1
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- Coating By Spraying Or Casting (AREA)
Abstract
The application relates to the field of transition layer spraying powder, and particularly discloses silicon-yttrium-aluminum-chromium-magnesium-oxygen intermediate phase spraying powder and a preparation method thereof. The silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder comprises the following components: yttria crystalline phase, yttrium chromium oxide crystalline phase, yttrium aluminum oxide crystalline phase, magnesium aluminum spinel phase, and amorphous silica; the average grain diameter of the spraying powder is 5-45 mu m; the preparation method comprises the following steps: mixing and dissolving aluminum nitrate, yttrium nitrate and chromium nitrate, and controlling the pH value to be not more than 7; adding silicon dioxide and magnesium oxide into the mixture, adjusting the pH value to be alkaline, performing heat treatment and aging, filtering to obtain a filtrate, and washing; mixing the washed filtrate with water, adding binder, dispersing uniformly, performing high temperature ceramization at 2800-3500 deg.C, and atomizing. The silicon yttrium aluminum chromium magnesium oxide mesophase spray powder disclosed by the application is beneficial to improving the adhesion strength of the yttrium oxide coating and a glass substrate, prolonging the service life of the yttrium oxide coating and improving the etching quality of a wafer.
Description
Technical Field
The application relates to the field of transition layer spraying powder, in particular to silicon-yttrium-aluminum-chromium-magnesium-oxygen intermediate phase spraying powder and a preparation method thereof.
Background
Yttria coatings have been widely used as protective coatings for metals, alloys, glasses operating at high temperatures and/or under severe stress conditions due to their excellent thermal and mechanical properties. The yttrium oxide coating can also achieve the effect of reducing light transmission and heat transfer on the surface of the glass product.
However, glass is a fragile product with low toughness, yttrium oxide coating is flatly distributed on the glass by adopting a meltallizing process, and the surface of the glass is difficult to be subjected to deep roughening treatment by adopting a conventional process, so that the adhesive force between the coating and the glass is low; meanwhile, the thermal expansion coefficient of the yttrium oxide and that of the glass are large in difference, and the yttrium oxide coating is easy to be separated from the glass dislocation during high-temperature etching, so that the high-fluorine etching atmosphere is easy to extend to the surface of the glass along the corrosion of the coating air holes, the coating is enabled to fall off to generate particles, a wafer or a chip is polluted, the functionality of the wafer or the chip is out of control, the yield of the chip is reduced, and the manufacturing cost is increased.
Aiming at the related technology, the application provides an intermediate carrier phase of a transition medium, in particular a silicon-chromium-yttrium-aluminum-magnesium-oxygen composite material, which is used as a transition layer between a glass substrate and an yttrium oxide coating after spraying to improve the service life of the yttrium oxide coating and the etching quality of a wafer.
Disclosure of Invention
In order to obtain the transition layer spraying powder between the glass substrate and the yttrium oxide coating, the application provides the silicon-yttrium-aluminum-chromium-magnesium-oxygen intermediate phase spraying powder and a preparation method thereof.
In a first aspect, the application provides a silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder, which adopts the following technical scheme:
The silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder comprises the following components: yttria crystalline phase, yttrium chromium oxide crystalline phase, yttrium aluminum oxide crystalline phase, magnesium aluminum spinel phase, and amorphous silica;
yttria, yttrium chromium oxide, yttrium aluminum oxide, magnesium aluminum oxide, and silica;
The average grain size of the spraying powder is 5-45 mu m.
By adopting the technical scheme, yttrium chromium oxide, yttrium aluminum oxide and magnesium aluminum spinel are doped in the mixed matrix of yttrium oxide and silicon dioxide, the doping of the chromium oxide, aluminum oxide and magnesium oxide ensures that the coating has excellent strength, toughness and hardness, and the expansion coefficients of the chromium oxide, the aluminum oxide and the magnesium oxide are between the expansion coefficients of the silicon dioxide and the yttrium oxide, so that the coating can play a good role in bridging in order reduction, reduce stress change caused by overlarge thermal expansion phase difference during high-temperature etching, and improve the adhesion strength of the coating; the grain boundaries of various metal oxide crystals are slender and narrow, the inside and outside of a well repaired crystal lattice keep extremely low porosity, the eutectic point is moved downwards, the coating has higher density, in the subsequent high-temperature etching, the glass substrate weakens the expansion and contraction stress due to the transitional buffer effect of the coating, the adhesive force attenuation of the coating to the glass substrate is relieved, and the etching quality of a wafer is improved.
The spraying powder is doped with high entropy, and a plurality of different atomic nuclei exist, so that a plurality of groups of phonon scattering centers are generated, the free path of phonons is shortened, and the glass temperature is stabilized; the high-entropy doped spraying powder has obvious toughening effect after high-temperature coating, and is beneficial to improving the heat insulation effect of the glass substrate and relieving stress change caused by different expansion coefficients of the coating and the glass substrate.
In summary, the coating formed by spraying the silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder can be used as a transition layer between a glass substrate and a yttrium oxide coating, so that the adhesion of the yttrium oxide coating to the glass substrate is improved, the adhesion attenuation of the coating to the glass substrate is relieved, the glass substrate is better protected during high-temperature etching, and the etching quality of a wafer is improved.
Preferably, the average particle size of the spraying powder is 35-40 mu m.
By adopting the technical scheme, the particle size of the spraying powder is controlled, so that the coating formed after spraying is more compact and uniform.
Preferably, the preparation raw materials of the spraying powder comprise the following components: yttrium nitrate, aluminum nitrate, chromium nitrate, magnesium oxide, and silicon dioxide;
In the preparation raw materials, the molar ratio of yttrium element to aluminum element to chromium element to magnesium element to silicon element is 1 (2.2-2.6), 0.2-0.6, 0.16-0.2 and 1.6-2.
In a second aspect, the application provides a preparation method of silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder, which adopts the following technical scheme:
the preparation method of the silicon-yttrium-aluminum-chromium-magnesium-oxygen intermediate phase spraying powder comprises the following steps:
Step 1: mixing and dissolving aluminum nitrate, yttrium nitrate and chromium nitrate to obtain a mixed solution, and controlling the pH value of the mixed solution to be not more than 7;
Step 2: adding silicon dioxide and magnesium oxide into the mixed solution, adjusting the pH value to be alkaline, performing heat treatment and aging, filtering to obtain a filtrate, and washing;
Step 3: mixing the washed filtrate with water, adding a binder, and uniformly dispersing to obtain mixed slurry;
step 4: and (3) carrying out high-temperature porcelain on the mixed slurry at 2800-3500 ℃ and then atomizing to obtain the silicon-yttrium-aluminum-chromium-magnesium-oxygen intermediate phase spraying powder.
By adopting the technical scheme, the pH values of the solutions in the step 1 and the step 2 are controlled, so that the aluminum nitrate, the yttrium nitrate and the chromium nitrate in the step 1 are fully dissolved under neutral or weak acid conditions, and the possibility of generating metal hydroxide precipitation is reduced; adding silicon dioxide and magnesium oxide in the step 2, then adjusting the pH value to be alkaline, and promoting the precipitation of aluminum hydroxide, yttrium hydroxide and chromium hydroxide precipitates to be attached to the surfaces of the silicon dioxide and magnesium oxide particles through a heat treatment reaction, so that the silicon dioxide particles and the magnesium oxide particles are fully coated by the aluminum yttrium chromium hydroxide precipitates;
step3, the slurry is treated through the binder, so that the dispersion of powder particles is promoted, and the spray powder is guaranteed to have better sphericity, uniformity and compaction density;
In the step 4, various metal compounds are melted at 2800-3500 ℃, the formed metal oxides are closely adjacent and are in a proper atomic vibration reaction distance, and yttrium oxide crystal phases, magnesia-alumina spinel phases, yttrium oxide-alumina crystal phases and yttrium oxide-chromium oxide crystal phases are formed, silicon dioxide is fully coated by the metal oxides and is not easy to gasify and overflow, and the silicon dioxide is re-solidified into amorphous silicon dioxide particles after cooling, so that the generation of metal-silicon-oxygen intermediate phases is reduced, the quality and application effect of spray powder are guaranteed, and finally the silicon-yttrium-aluminum-chromium-magnesium-oxygen intermediate phase spray powder with high crystallization degree, good sphericity, uniform particle size distribution and good dispersibility can be prepared.
Preferably, in the step 2, ammonia water is used to adjust the pH value to 8-9.
Preferably, the mass concentration of the ammonia water is 5-10%.
By adopting the technical scheme, the metal hydroxide is slowly and uniformly separated out, so that the silicon dioxide and magnesium oxide particles are fully coated by the metal hydroxide precipitate, and the uniformity and sphericity of the powder particles are ensured.
Preferably, the primary crystal grain size of the silicon dioxide is 20-80 nanometers, and the primary crystal grain size of the magnesium oxide is 50-80 nanometers.
By adopting the technical scheme, the primary crystal particle size of the silicon dioxide and the magnesium oxide on the microscopic level is limited, the crystal performance of the silicon dioxide and the magnesium oxide is optimized, the uniform adhesion and coating of metal hydroxide precipitation are facilitated, and the control of the relative uniformity of the element components of the metal hydroxide coating before and after sintering is facilitated.
Preferably, in the step 2, the heat treatment aging treatment conditions are as follows: heating to 80-90 deg.C and ageing for 3-6 hr.
By adopting the technical scheme, the precipitation of the metal hydroxide is facilitated, the precipitation crystallinity and purity of the metal hydroxide are improved, the quality and uniformity of precipitation are improved, the quality of the spraying powder is improved, the sphericity is improved, and the uniformity of particle size distribution is promoted.
Preferably, in the step 3, the mass ratio of the filtrate to the water is 1 (1-2), and the mass of the binder is 1-2% of the total mass of the filtrate and the water.
Preferably, the binder is a polyvinyl alcohol binder.
By adopting the technical scheme, the powder particles are promoted to be uniformly dispersed, so that the spray powder has better sphericity, uniformity and compaction density.
Preferably, in the step 4, the treatment conditions of high-temperature ceramization are as follows: treating at 2800-3500 deg.C for 2-8H under the condition of plasma current and Ar-H 2 mixed atmosphere.
By adopting the technical scheme, the hydrogen forms free radicals and high-temperature atoms after plasma impact, and contacts oxygen to form oxyhydrogen flame after meltallizing, thereby being beneficial to increasing the temperature of plasma airflow and improving sintering effect.
In summary, the application has the following beneficial effects:
1. The coating formed by spraying the silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder can be used as a transition layer between a glass substrate and a yttrium oxide coating, so that the adhesion of the yttrium oxide coating to the glass substrate is improved, the adhesion attenuation of the coating to the glass substrate is relieved, the glass substrate is better protected during high-temperature etching, and the etching quality of a wafer is improved;
2. According to the application, the doping of yttrium chromium oxide, yttrium aluminum oxide and magnesium aluminum spinel enables the glass surface coating to have excellent strength, toughness and hardness, and can play a good role in bridging along potential reduction, so that stress variation caused by overlarge thermal expansion phase difference during high-temperature etching is reduced, and the adhesion strength of the coating is improved; the grain boundaries of various metal oxide crystals are slender, narrow and dense, the inside and outside of a well repaired crystal lattice keep extremely low porosity, and the eutectic point is moved downwards, so that the glass surface coating has higher density, and the adhesive force attenuation of the glass surface coating to a glass substrate is relieved; meanwhile, by the high-entropy doping technology, the spraying powder generates a plurality of groups of phonon scattering centers, shortens the free path of phonons, is beneficial to stabilizing the glass temperature, has obvious toughening effect, is beneficial to improving the heat insulation effect of the glass substrate and relieving stress changes caused by different expansion coefficients of the coating and the glass substrate;
3. According to the method, by controlling the high-temperature porcelain condition and sintering temperature, the silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder which has the advantages of high crystallization degree, good sphericity, uniform particle size distribution and good dispersibility can be prepared;
4. The method of the application controls the pH value of the mixed solution step by step, fully dissolves aluminum nitrate, yttrium nitrate and chromium nitrate under neutral or weak acid condition, and promotes the full precipitation of aluminum hydroxide, yttrium hydroxide and chromium hydroxide precipitate and is uniformly adhered on the surface of silicon dioxide and magnesium oxide particles in the heat treatment aging reaction;
5. The method optimizes the crystal performance of the silicon dioxide and the magnesium oxide by limiting the primary crystal grain sizes of the silicon dioxide and the magnesium oxide on the microscopic level, is beneficial to the uniform adhesion and coating of metal hydroxide precipitation, and is beneficial to controlling the relative consistency of the element components of the metal hydroxide coating before and after sintering.
Drawings
FIG. 1 is a view of the morphology of the SiYAG mesophase powder obtained in example 1 of the present application observed by a scanning electron microscope;
FIG. 2 shows the results of an X-ray diffraction analysis of the SiYAG-MgAl intermediate phase spray powder prepared in example 1 of the present application.
Detailed Description
To further assist understanding of the technical solution of the present invention, the technical solution of the present invention will be described in more detail below by providing several specific implementation examples, all of which are only some of the embodiments of the present invention, but not all of them;
The following embodiments may be combined with each other, and the same or similar concepts or processes may not be described in detail in some embodiments; the reaction apparatus, monomer compound, binder, solvent, etc. according to the following examples are commercially available.
The following specific embodiments may be combined with each other and may not be described in detail in some embodiments for the same or similar concepts or processes therein.
The following examples are further illustrative of the invention, which is not limited thereto. The embodiment is not specifically described, and the percentage content is mass percentage.
Examples
Example 1
The embodiment discloses silicon yttrium aluminum chromium magnesium intermediate phase spraying powder, which is prepared by the following steps:
250kg of aluminum nitrate nonahydrate (about 731 mol), 111kg of yttrium nitrate hexahydrate (about 290 mol) and 47kg of chromium nitrate nonahydrate (about 149 mol) were dissolved in water to obtain a mixed solution, and the pH was adjusted to about 6.5 with 8% ammonia water;
adding 30kg of silicon dioxide (about 500 mol) and 2kg of magnesium oxide (about 50 mol) into the mixed solution, dispersing uniformly, regulating the pH value to about 8.5 by 8% ammonia water, heating to 80 ℃ for heat treatment and ageing for 4 hours, filtering to obtain a filtrate, and washing until the nitrate concentration in the washing liquid is less than 100ppm;
Mixing the filtrate with water according to a mass ratio of 1:1.5, adding a binder accounting for 1% of the total mass of the filtrate and the water, and stirring and dispersing for 30min at a rotating speed of 1500r/min by using a high-speed dispersing machine to obtain mixed slurry;
And (3) pumping the mixed slurry into a high-temperature porcelain furnace by using a slurry pump, regulating plasma current to 600A, regulating hydrogen flow to 9nlpm and argon flow to 40nlpm, heating to 3000 ℃ in a porcelain region, sintering at high temperature for 5 hours to obtain porcelain powder, treating the porcelain powder by using an atomizing disc to ensure that the particle size is in the range of 35-40 mu m, sieving, and collecting 325-mesh sieve offal to obtain the silicon-yttrium-aluminum-chromium-magnesium-oxygen mesophase spraying powder.
In the embodiment, the original grain diameter of the silicon dioxide ranges from 20 nm to 80nm, and the original grain diameter of the magnesium oxide ranges from 50 nm to 80nm; the binder is a commercially available polyvinyl alcohol binder.
Example 2
The embodiment discloses silicon yttrium aluminum chromium magnesium intermediate phase spraying powder, which is prepared by the following steps:
201kg of aluminum nitrate nonahydrate (about 588.5 mol), 102kg of yttrium nitrate hexahydrate (about 265 mol) and 33kg of chromium nitrate nonahydrate (about 105 mol) were dissolved in water to obtain a mixed solution, and the pH was adjusted to about 6.5 with 8% ammonia water;
adding 30kg of silicon dioxide (about 500 mol) and 2kg of magnesium oxide (about 50 mol) into the mixed solution, dispersing uniformly, regulating the pH value to about 8.5 by 8% ammonia water, heating to 80 ℃ for heat treatment and ageing for 4 hours, filtering to obtain a filtrate, and washing until the nitrate concentration in the washing liquid is less than 100ppm;
Mixing the filtrate with water according to a mass ratio of 1:1.5, adding a binder accounting for 1% of the total mass of the filtrate and the water, and stirring and dispersing for 30min at a rotating speed of 1500r/min by using a high-speed dispersing machine to obtain mixed slurry;
and (3) pumping the mixed slurry into a high-temperature porcelain furnace by using a slurry pump, regulating plasma current to 600A, regulating hydrogen flow to 9nlpm and argon flow to 40nlpm, heating to 3000 ℃ in a porcelain region, sintering at high temperature for 5 hours to obtain porcelain powder, treating the porcelain powder by using an atomizing disc to ensure that the average particle size is in the range of 35-40 mu m, sieving, and collecting 325-mesh sieve offal to obtain the silicon-yttrium-aluminum-chromium-magnesium-oxygen mesophase spraying powder.
Example 3
The difference between this embodiment and embodiment 1 is that the original grain size range of the silica is 4 μm-8 μm, and the original grain size range of the magnesia is 4 μm-8 μm.
Example 4
This example differs from example 1 only in that no hydrogen gas was introduced during the high temperature ceramization. The preparation method of the silicon yttrium aluminum chromium magnesium intermediate phase spraying powder comprises the following steps:
250kg of aluminum nitrate nonahydrate, 111kg of yttrium nitrate hexahydrate and 47kg of chromium nitrate nonahydrate are dissolved in water to obtain a mixed solution, and the pH value is regulated to be about 6.5 by 8% ammonia water;
Adding 30kg of silicon dioxide and 2kg of magnesium oxide into the mixed solution, dispersing uniformly, regulating the pH value to be about 8.5 by 8% ammonia water, heating to 80 ℃ for heat treatment and ageing for 4 hours, filtering to obtain a filtrate, and washing until the nitrate concentration in the washing liquid is less than 100ppm;
Mixing the filtrate with water according to a mass ratio of 1:1.5, adding a binder accounting for 1% of the total mass of the filtrate and the water, and stirring and dispersing for 30min at a rotating speed of 1500r/min by using a high-speed dispersing machine to obtain mixed slurry;
And (3) pumping the mixed slurry into a high-temperature porcelain furnace by using a slurry pump, regulating plasma current to 600A, regulating argon flow to 48nlpm, heating to 3000 ℃ in a porcelain region, sintering at high temperature for 5 hours to obtain porcelain powder, treating the porcelain powder by using an atomizing disc to ensure that the particle size is in the range of 35-40 mu m, sieving, and collecting 325-mesh sieve offcuts to obtain the silicon-yttrium-aluminum-chromium-magnesium oxide mesophase spraying powder.
Example 5
This example differs from example 1 only in that the ammonia water is replaced by a 5% sodium hydroxide solution. The preparation method of the silicon yttrium aluminum chromium magnesium intermediate phase spraying powder comprises the following steps:
250kg of aluminum nitrate nonahydrate, 111kg of yttrium nitrate hexahydrate and 47kg of chromium nitrate nonahydrate are dissolved in water to obtain a mixed solution, and the pH value is regulated to about 6.5 by 5% sodium hydroxide solution;
Adding 30kg of silicon dioxide and 2kg of magnesium oxide into the mixed solution, dispersing uniformly, regulating the pH value to about 8.5 by using 5% sodium hydroxide solution, heating to 80 ℃ for heat treatment and ageing for 4 hours, filtering to obtain a filtrate, and washing until the nitrate concentration in the washing solution is less than 100ppm;
Mixing the filtrate with water according to a mass ratio of 1:1.5, adding a binder accounting for 1% of the total mass of the filtrate and the water, and stirring and dispersing for 30min at a rotating speed of 1500r/min by using a high-speed dispersing machine to obtain mixed slurry;
And (3) pumping the mixed slurry into a high-temperature porcelain furnace by using a slurry pump, regulating plasma current to 600A, regulating hydrogen flow to 9nlpm and argon flow to 40nlpm, heating to 3000 ℃ in a porcelain region, sintering at high temperature for 5 hours to obtain porcelain powder, treating the porcelain powder by using an atomizing disc to ensure that the particle size is in the range of 35-40 mu m, sieving, and collecting 325-mesh sieve offal to obtain the silicon-yttrium-aluminum-chromium-magnesium-oxygen mesophase spraying powder.
Performance test
The silicon yttrium aluminum chromium magnesium oxide mesophase spray powder prepared in examples 1-5 was plasma sprayed onto a glass substrate with a coating thickness of 40 μm to obtain a transition layer, and a coating thickness of 160 μm of a plasma sprayed yttrium oxide spray powder (from Suzhou Gaogong semiconductor Co., ltd.) was applied to the transition layer to obtain examples 1-5.
And (3) directly performing plasma spraying on yttrium oxide spraying powder to the surface of the glass substrate, wherein the coating thickness is 200 mu m, and obtaining a blank comparison sample.
The vickers hardness of each of the samples and the blank was measured by reference to standard GB-T4340.1-2009, and the peel strength of each of the samples and the blank was measured by reference to standard GB/T41511-2022. The results are summarized in Table 1.
TABLE 1
Referring to fig. 1, it can be seen that the silicon yttrium aluminum chromium magnesium oxide mesophase spray powder prepared in example 1 has a better sphericity and a more uniform particle size distribution.
Referring to fig. 2, it can be seen that the silicon yttrium aluminum chromium magnesium oxide intermediate phase spray powder prepared in example 1 is mainly a Y 2O3 crystal phase, doped with YCrO 3 crystal phase, Y 3.24Al4.76O12 crystal phase and al 2O4 spinel phase, and the silica does not show diffraction peaks, probably because the silica is amorphous and amorphous, and the silicon yttrium aluminum chromium magnesium oxide intermediate phase spray powder does not contain a metal-silicon-oxygen intermediate crystal phase.
By combining examples 1-5 and blank comparison and combining Table 1, it can be seen that spraying the transition layer and then spraying the yttrium oxide coating on the glass substrate with the SiYttrium aluminum chromium magnesium oxide mesophase spray powder prepared by the method is beneficial to improving the adhesion strength of the yttrium oxide coating on the glass substrate and the mechanical properties of the coating.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (10)
1. The silicon-yttrium-aluminum-chromium-magnesium oxide intermediate phase spraying powder is characterized by comprising the following components: yttria crystalline phase, yttrium chromium oxide crystalline phase, yttrium aluminum oxide crystalline phase, magnesium aluminum spinel phase, and amorphous silica;
The average grain size of the spraying powder is 5-45 mu m.
2. The silicon yttrium aluminum chromium magnesium oxide mesophase spray powder according to claim 1, wherein the average particle size of the spray powder is 35-40 μm.
3. The silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder according to claim 1, wherein the spraying powder is prepared from the following raw materials: yttrium nitrate, aluminum nitrate, chromium nitrate, magnesium oxide, and silicon dioxide;
In the preparation raw materials, the molar ratio of yttrium element to aluminum element to chromium element to magnesium element to silicon element is 1 (2.2-2.6), 0.2-0.6, 0.16-0.2 and 1.6-2.
4. A method for preparing the silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder according to any one of claims 1 to 3, which comprises the following steps:
Step 1: mixing and dissolving aluminum nitrate, yttrium nitrate and chromium nitrate to obtain a mixed solution, and controlling the pH value of the mixed solution to be not more than 7;
Step 2: adding silicon dioxide and magnesium oxide into the mixed solution, adjusting the pH value to be alkaline, performing heat treatment and aging, filtering to obtain a filtrate, and washing;
Step 3: mixing the washed filtrate with water, adding a binder, and uniformly dispersing to obtain mixed slurry;
step 4: and (3) carrying out high-temperature porcelain on the mixed slurry at 2800-3500 ℃ and then atomizing to obtain the silicon-yttrium-aluminum-chromium-magnesium-oxygen intermediate phase spraying powder.
5. The method for preparing the silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder according to claim 4, wherein in the step 2, ammonia water is adopted to adjust the pH value to 8-9.
6. The method for preparing the silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder according to claim 4, wherein the primary crystal grain size of the silicon dioxide is 20-80 nanometers, and the primary crystal grain size of the magnesium oxide is 50-80 nanometers.
7. The method for preparing the silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder according to claim 4, wherein in the step 2, the heat treatment aging treatment conditions are as follows: heating to 80-90 deg.C and ageing for 3-6 hr.
8. The method for preparing the silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder according to claim 4, wherein in the step 3, the mass ratio of the filtered material to the water is 1 (1-2), and the mass of the binder is 1-2% of the total mass of the filtered material and the water.
9. The method for preparing the silicon-yttrium-aluminum-chromium-magnesium oxide intermediate phase spraying powder according to claim 8, wherein the binder is a polyvinyl alcohol binder.
10. The method for preparing the silicon yttrium aluminum chromium magnesium oxide intermediate phase spraying powder according to claim 4, wherein in the step 4, the high temperature porcelain treatment conditions are as follows: treating at 2800-3500 deg.C for 2-8H under the condition of plasma current and Ar-H 2 mixed atmosphere.
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