CN114804931B - Low-temperature corrosion method for AlON transparent ceramic - Google Patents
Low-temperature corrosion method for AlON transparent ceramic Download PDFInfo
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- CN114804931B CN114804931B CN202210511364.0A CN202210511364A CN114804931B CN 114804931 B CN114804931 B CN 114804931B CN 202210511364 A CN202210511364 A CN 202210511364A CN 114804931 B CN114804931 B CN 114804931B
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- 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
- C04B41/91—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics involving the removal of part of the materials of the treated articles, e.g. etching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B29/00—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
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- C04B41/5353—Wet etching, e.g. with etchants dissolved in organic solvents
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Abstract
The invention provides a low-temperature corrosion method of AlON transparent ceramic, which comprises the following steps: 1) Sintering AlON transparent ceramic: firstly, al is added 2 O 3 Uniformly mixing the powder, alN powder and a sintering aid, then loading the mixture into a graphite mold, placing the graphite mold into discharge plasma sintering equipment for high-temperature sintering, and cooling the graphite mold along with a furnace after sintering is finished to obtain an AlON transparent ceramic sample; 2) Grinding and polishing the surface of the AlON transparent ceramic: grinding an AlON transparent ceramic sample by using a diamond sand disc from thick to thin, and then coating diamond polishing paste on polishing flannelette for polishing until the mirror surface is bright; 3) Chemical etching of the AlON transparent ceramic: placing an AlON transparent ceramic sample in a reaction vessel containing concentrated phosphoric acid to start corrosion; after the corrosion is completed, the sample is immersed in clear water and then taken out and washed with a large amount of flowing clear water. The method has the advantages of simple operation, safety, low energy consumption and short required time, and the etched AlON transparent ceramic has obvious crystal grains and clear crystal boundary.
Description
Technical Field
The invention relates to a low-temperature corrosion method for AlON transparent ceramic, belonging to the technical field of preparation of transparent ceramic materials
Background
AlON transparent ceramics has good high temperature resistance, thermal vibration stability, erosion resistance, light transmission and processability, has good light transmission in the range from near ultraviolet light to mid-infrared light (0.2-5.0 mu m), has the transmittance of over 80 percent and has isotropic light transmission, and is widely applied to the fields of national defense and civil use. The existing AlON transparent ceramic sintering method mainly comprises pressureless sintering, hot-pressing sintering and the like, but has long sintering time, high molding temperature, low density of the prepared AlON transparent ceramic and unsatisfactory mechanical property. And the Spark Plasma Sintering (SPS) is used as a powder metallurgy means, so that the AlON transparent ceramic can be rapidly sintered at low temperature, and a sample is high in density and good in mechanical property after being formed.
The microscopic morphology analysis is an important detection means for characterizing the ceramics according to relevant standards and regulations, and the grain size, the grain shape, the grain boundary smoothness and the distribution of internal microstructure defects and pores of the ceramics can be observed through the microscopic morphology. And the AlON transparent ceramic has good oxidation resistance and high chemical stability, and the observation of the microstructure of the AlON transparent ceramic usually depends on high-temperature thermal corrosion. The high-temperature hot corrosion temperature of the AlON transparent ceramic generally exceeds 1700 ℃, and the heat preservation is needed for a long time.
Wu Bo of the university of maritime affairs carries out thermal corrosion on the AlON transparent ceramic at different sintering temperatures under the condition that the heat preservation time is 150 min. The method needs long time, the corrosion temperature is more than 1700 ℃, the energy consumption is large, and the heating instrument can be damaged.
In the research of the preparation process of the AlON transparent ceramic by the solid-phase reaction method and the carbothermic reduction nitridation method, sun of Jiangsu university is used for corroding the AlON transparent ceramic by a high-temperature thermal corrosion method, wherein the heating temperature is 1800 ℃, the heat preservation time is 60min, and the whole process is carried out in a nitrogen atmosphere. The crystal grains corroded by the method are coarse, and the corrosion process is difficult to control.
The AlON transparent ceramic has long time in the thermal corrosion process, high cost, large energy consumption and complex operation, and the structure of the AlON transparent ceramic is changed to a certain extent (for example, crystal grains are inevitably grown) in the process, thereby influencing the observation of the original microstructure structure of the AlON transparent ceramic. Therefore, finding an etching method that is simple and feasible and can maintain the original microstructure of the AlON transparent ceramic is crucial to research of AlON transparent ceramics.
Disclosure of Invention
The invention aims to provide a low-temperature corrosion method of AlON transparent ceramic, which simplifies the operation steps, reduces the corrosion temperature and shortens the corrosion time on the premise of effectively corroding the AlON transparent ceramic.
The invention relates to a low-temperature corrosion method of AlON transparent ceramic, which mainly comprises the following process steps:
1) Sintering AlON transparent ceramic: firstly, al with the particle size of 10nm-500nm is added into the powder 2 O 3 Uniformly mixing the powder, alN powder and a sintering aid, then loading the mixture into a graphite mold, placing the graphite mold into discharge plasma sintering equipment for high-temperature sintering, raising the temperature to 1500-1650 ℃ at the heating rate of 100-300 ℃/min, keeping the sintering pressure at 30-70MPa for 1-15min, and cooling the mixture along with a furnace after sintering is finished to obtain the AlON transparent ceramic sample.
2) Grinding and polishing the surface of the AlON transparent ceramic: grinding an AlON transparent ceramic sample prepared by SPS sintering by using a diamond sand table from coarse to fine, wherein the specifications of the diamond sand table are 100 meshes, 500 meshes, 1000 meshes, 1500 meshes, 2000 meshes and 3000 meshes in sequence. The polishing mode is that fingers press the sample to the below of slant evenly hard for sample surface decorative pattern trend unanimous after polishing, later change next specification sand table, polish along the direction that the current decorative pattern of perpendicular to moves, until sample surface decorative pattern is more tiny, and move towards and the direction of the previous round decorative pattern direction is perpendicular, polish according to this method order in proper order, until use 3000 meshes sand table to polish after, sample surface does not have obvious mar.
And then polishing by using polishing flannelette and coating diamond polishing paste, wherein the specifications of the polishing paste are 6000 meshes, 10000 meshes, 13000 meshes, 18000 meshes and 30000 meshes in sequence. The polishing mode is that a sample is placed on a metallographic polishing machine with polishing flannelette, 6000-mesh polishing paste is coated firstly, a finger presses the sample, the sample moves at a constant speed along the circle center of the polishing cloth to the edge direction until polishing patterns on the surface of the sample disappear, then polishing paste of the next specification is coated, the operation is repeated until the sample is polished by 30000-mesh polishing paste, and the surface of the sample is bright.
3) Chemical etching of the AlON transparent ceramic: slowly pouring concentrated phosphoric acid with the mass concentration of 75.00-98.00% and the volume of 5-100ml into a reaction container, placing the container on a multifunctional heater, heating to 100-500 ℃ in a fume hood, then starting heat preservation, clamping an AlON transparent ceramic sample by using tweezers, slowly placing the AlON transparent ceramic sample into a beaker, completely immersing the sample in the concentrated phosphoric acid, starting timing by using a timer, after 1-30min, completely corroding, taking out the sample by using the tweezers, placing the sample into the beaker with a large amount of clear water, soaking for 0.1-5min, taking out the sample, washing by using a large amount of flowing clear water, and wiping off surface water by using dust-free paper after washing.
The etched AlON transparent ceramic sample is placed under a microscope to observe a corresponding microstructure, and the result shows that the AlON transparent ceramic etched by the method has obvious crystal grain shape and clear and visible crystal boundary.
The beneficial effects of the invention include:
the method has the advantages of simple operation, safety, low energy consumption and short required time, the AlON transparent ceramic corroded by the method has obvious crystal grains and clear crystal boundaries, can effectively observe the microstructure of the ceramic and the distribution condition of internal pores and defects, is convenient for researchers to judge the performance and sintering condition of the material, and is beneficial to making a next working plan.
Drawings
FIG. 1 is a graph of OM for the samples of example 1;
fig. 2 is a graph of OM for the sample in example 2.
Detailed Description
The invention is further illustrated, but not limited, by the following detailed description of the invention, when read in conjunction with the accompanying drawings.
Example 1
Step 1) AlON transparent ceramic sintering: firstly, al with the particle size of 50nm is added into the powder 2 O 3 Uniformly mixing the powder, alN powder and sintering aid, filling the mixture into a graphite die, and then mixingAnd placing the graphite mould in discharge plasma sintering equipment for high-temperature sintering, raising the temperature to 1650 ℃ at a heating rate of 100 ℃/min, keeping the sintering pressure at 50MPa for 5min, and cooling along with a furnace after sintering is finished to obtain the AlON transparent ceramic sample.
Step 2), grinding and polishing the surface of the AlON transparent ceramic: grinding an AlON transparent ceramic sample prepared by SPS sintering by using a diamond sand table from coarse to fine, wherein the specifications of the diamond sand table are 100 meshes, 500 meshes, 1000 meshes, 1500 meshes, 2000 meshes and 3000 meshes in sequence. The polishing mode is that fingers press the sample to the below of slant evenly hard for sample surface decorative pattern trend unanimous after polishing, later change next specification sand table, polish along the direction that the current decorative pattern of perpendicular to moves, until sample surface decorative pattern is more tiny, and move towards and the direction of the previous round decorative pattern direction is perpendicular, polish according to this method order in proper order, until use 3000 meshes sand table to polish after, sample surface does not have obvious mar.
And then polishing by using polishing flannelette and coating diamond polishing paste, wherein the specifications of the polishing paste are 6000 meshes, 10000 meshes, 13000 meshes, 18000 meshes and 30000 meshes in sequence. The polishing mode is that a sample is placed on a metallographic polishing machine with polishing flannelette, 6000-mesh polishing paste is coated firstly, a finger presses the sample, the sample moves at a constant speed along the circle center of the polishing cloth to the edge direction until polishing patterns on the surface of the sample disappear, then polishing paste of the next specification is coated, the operation is repeated until the sample is polished by 30000-mesh polishing paste, and the surface of the sample is bright.
Step 3) AlON transparent ceramic chemical corrosion: slowly pouring concentrated phosphoric acid with the mass concentration of 85% and the volume of 20ml into a reaction container, placing the container on a multifunctional heater, heating the container in a fume hood to 300 ℃, then keeping the temperature, clamping an AlON transparent ceramic sample by using tweezers, slowly placing the AlON transparent ceramic sample into a beaker, completely immersing the sample in the concentrated phosphoric acid, then starting timing by using a timer, taking out the sample by using the tweezers after 8min, placing the sample in the beaker filled with a large amount of clear water, immersing for 1min, taking out the sample, washing with a large amount of flowing clear water, and wiping the surface moisture by using dust-free paper after washing.
And 4) placing the corroded AlON transparent ceramic sample under a microscope to observe a corresponding microstructure, and finding that the AlON transparent ceramic corroded by the method has an obvious crystal grain shape and a clear and visible crystal boundary.
The microstructure of the AlON transparent ceramic etched in this example is shown in fig. 1 when observed under an optical microscope.
Example 2
Step 1) is the same as in example 1.
Step 2) is the same as in example 1.
Step 3) AlON transparent ceramic chemical corrosion: slowly pouring concentrated phosphoric acid with the concentration of 75% and the volume of 100ml into a reaction container, placing the container on a multifunctional heater, heating the container in a fume hood to 350 ℃, keeping the temperature, clamping an AlON transparent ceramic sample by using tweezers, slowly placing the AlON transparent ceramic sample into a beaker, completely immersing the sample in the concentrated phosphoric acid, then starting timing by using a timer, taking out the sample by using the tweezers after 5min, placing the sample into the beaker filled with a large amount of clear water, soaking for 2min, taking out the sample, washing with a large amount of flowing clear water, and wiping the surface moisture by using dust-free paper after washing.
4) Same as in example 1.
The microstructure of the AlON transparent ceramic etched according to this example is shown in fig. 2 when observed under an optical microscope.
Claims (4)
1. A low-temperature corrosion method for AlON transparent ceramics is characterized by comprising the following steps:
1) Sintering AlON transparent ceramic: firstly, al is added 2 O 3 Uniformly mixing the powder, alN powder and a sintering aid, then loading the mixture into a graphite mold, placing the graphite mold into discharge plasma sintering equipment for high-temperature sintering, and cooling the graphite mold along with a furnace after sintering is finished to obtain an AlON transparent ceramic sample;
Al 2 O 3 the particle size of the AlN powder is 10nm-500nm; the specific process of spark plasma sintering comprises the steps of heating up at a rate of 100-300 ℃/min, sintering at a pressure of 30-70MPa and at a sintering temperature of 1500-1650 ℃, and keeping the temperature and pressure for 1-15min;
2) Grinding and polishing the surface of the AlON transparent ceramic: grinding an AlON transparent ceramic sample by using a diamond sand disc from thick to thin, and then coating diamond polishing paste on polishing flannelette for polishing until the mirror surface is bright;
3) Chemical etching of the AlON transparent ceramic: placing an AlON transparent ceramic sample in a reaction vessel containing concentrated phosphoric acid to start corrosion, wherein the mass concentration of the concentrated phosphoric acid is 75.00-98.00%, the corrosion heating temperature is 100-500 ℃, and the corrosion time is 1-30min; and after the corrosion is finished, immersing the sample in clear water for 0.1-5min, and then taking out and washing with a large amount of flowing clear water.
2. The AlON transparent ceramic low-temperature corrosion method according to claim 1, wherein the diamond sand table is 100 meshes, 500 meshes, 1000 meshes, 1500 meshes, 2000 meshes and 3000 meshes in sequence.
3. The AlON transparent ceramic low-temperature corrosion method according to claim 1, wherein the specifications of the diamond polishing paste are 6000 meshes, 10000 meshes, 13000 meshes, 18000 meshes and 30000 meshes in sequence.
4. The AlON transparent ceramic low-temperature corrosion method according to claim 1, characterized in that the AlON transparent ceramic corroded by the method has obvious crystal grain shape and clearly visible crystal boundary.
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