CN112341000B - Carbon/carbon composite material SiC coating repairing modified glass material based on laser cladding method and preparation and use methods - Google Patents

Carbon/carbon composite material SiC coating repairing modified glass material based on laser cladding method and preparation and use methods Download PDF

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CN112341000B
CN112341000B CN202011360860.8A CN202011360860A CN112341000B CN 112341000 B CN112341000 B CN 112341000B CN 202011360860 A CN202011360860 A CN 202011360860A CN 112341000 B CN112341000 B CN 112341000B
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powder
carbon
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borosilicate glass
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CN112341000A (en
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李贺军
王翰辉
滕柳
史小红
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Northwestern Polytechnical University
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    • 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
    • C03C12/00—Powdered glass; Bead compositions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
    • C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
    • 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
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • 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
    • C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Compositions (AREA)

Abstract

The invention relates to a modified glass material for repairing a carbon/carbon composite SiC coating based on a laser cladding method and a preparation and use method thereof.A borosilicate glass is modified by a rare earth element samarium, so that the absorption rate of the material on a laser wave band covered by a fiber laser is obviously improved, the cladding quality of the modified borosilicate glass can be improved, and the oxidation resistance of a repaired carbon/carbon composite SiC coating sample is improved; on the other hand, the energy loss of the laser can be effectively reduced, and the development targets of environmental protection and cost saving are achieved.

Description

Carbon/carbon composite material SiC coating repairing modified glass material based on laser cladding method and preparation and use methods
Technical Field
The invention belongs to the technical field of laser surface engineering, and relates to a modified glass material for repairing a carbon/carbon composite SiC coating based on a laser cladding method, and a preparation method and a use method thereof.
Background
The borosilicate glass serving as a material with good thermal stability cannot easily generate phase change in a high-temperature aerobic environment, and effectively avoids the generation of phase change stress. Meanwhile, the borosilicate glass and the SiC coating have similar thermal expansion coefficients, higher viscosity and lower high-temperature volatility, and can provide long-term high-temperature oxidation protection for the C/C composite material matrix when being used as a local repair material for damaging the SiC coating. Document 1, "improved oxidation resistance of coatings of borosilicate glass for reusable space systems, gaofeng Shao, yucao Lu, dorian A.H. Hanaor, sheng Cui, jian Jiao, xiaodong Shen.Corroson Science, 2019, 146" outlines the antioxidant mechanism of borosilicate glass coatings, which on the one hand have a low gas permeability and can effectively slow down the inward diffusion rate of oxygen; on the other hand, the fluidity of the self-repairing crack realizes the self-healing of the crack at high temperature, and the self-repairing crack has the capability of self-repairing micro damage. Document 2 "Transmission glass coatings in modified with upconversionon nanocrystals by laser cladding method, mingye Ding, chunhua Lu, lindai Cao, wenjuan Huang, yaru Ni, zhongzi xu applied Surface Science,2013,277, "discloses a method of synthesizing a transparent glass coating by laser cladding, although a crack-free and dense coating on the Surface is successfully produced, by CO 2 Laser implementation. At present, most industrial Selective Laser Melting (SLM) equipment is provided with a fiber laser, and borosilicate glass mainly comprises oxides, so that the absorption rate of the borosilicate glass to a laser band covered by the fiber laser is low, the cladding quality is poor, and a uniform and compact coating is difficult to prepare. Therefore, most laser cladding of glass materials is by CO 2 And (3) completing the laser.
Therefore, the borosilicate glass has important value in improving the adaptability between the borosilicate glass and the optical fiber laser as an excellent SiC oxidation-resistant coating repairing material.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a modified glass material for repairing a carbon/carbon composite SiC coating based on a laser cladding method and a preparation and use method thereof.
Technical scheme
A carbon/carbon composite material SiC coating repairing modified glass material based on a laser cladding method is characterized in that: the borosilicate glass is modified by adopting a rare earth element samarium Sm, so that the absorption rate of a laser band covered by the fiber laser is improved; the material comprises the following components: siO with 65-80 mol percent 2 Powder, 15-20% of B 2 O 3 Powder, 4-10% Al 2 O 3 Powder and 1 to 10 percent of Sm 2 O 3 And (3) pulverizing.
A preparation method of the modified glass material for repairing the SiC coating of the carbon/carbon composite material based on the laser cladding method is characterized by comprising the following steps:
step 1, raw material preparation: siO with the mol percentage of 65-80 percent 2 Powder, 15-20% of B 2 O 3 Powder, 4-10% of Al 2 O 3 Mixing the powder with 1-10% of Sm 2 O 3 Ball milling the powder and mixing uniformly;
step 2, melting and forming: placing the mixed raw material powder into a corundum crucible, placing the corundum crucible into a muffle furnace, heating the corundum crucible to 1573-1773K along with the furnace in the air atmosphere, continuously carrying out heat treatment for 1-2 h to ensure that the raw material powder is fully melted and reacted at high temperature, and then directly taking out the raw material powder and cooling the raw material powder to room temperature to obtain Sm modified borosilicate glass;
step 3, grinding to prepare powder: and grinding the Sm modified borosilicate glass block into powder for repairing the SiC coating of the carbon/carbon composite material.
A method for repairing a carbon/carbon composite SiC coating by laser cladding by using the modified glass material is characterized by comprising the following steps: setting the laser power at 300-500W, the spot diameter at 2-5 mm, the scanning speed at 5-10 mm/s, and the thickness of the preset layer at 0.2-0.5 mm.
Advantageous effects
According to the modified glass material for repairing the carbon/carbon composite SiC coating based on the laser cladding method and the preparation and use methods, borosilicate glass is modified by the rare earth element samarium, so that the absorption rate of the material on a laser wave band covered by a fiber laser is remarkably improved, the cladding quality of the modified borosilicate glass can be improved, and the oxidation resistance of a repaired carbon/carbon composite SiC coating sample is improved; on the other hand, the energy loss of the laser can be effectively reduced, and the development targets of environmental protection and cost saving are achieved.
As can be seen from FIG. 1, the modified borosilicate glass powder of the present invention has an absorbance significantly higher than that before the modification, wherein the absorbance is a characteristic parameter of the absorbance, and the wavelength range of the fiber laser used in the experiment is 900-1200nm. As can be seen from the figure, the absorptivity of the Sm modified borosilicate glass powder is obviously improved.
As can be seen in fig. 2, the cross-sectional profiles of the borosilicate glass coating before and after modification are shown. Wherein (a) is a borosilicate glass coating after cladding, the power is 300W, the scanning speed is 7mm/s, and the diameter of a light spot is 4mm; (b) The coating is a Sm modified borosilicate glass coating after cladding, the power is 300W, the scanning speed is 8mm/s, and the diameter of a light spot is 4mm. As can be seen from the figure, the glass coating prepared by using the modified powder has a more compact structure, the hole defects are obviously reduced, and the scanning speed can be properly increased on the premise of ensuring certain laser power, so that the laser processing time is shortened, the energy consumption is reduced, and the experimental expectation is completely met.
Drawings
FIG. 1: results of absorption rate test of borosilicate glass powder before and after modification
FIG. 2: (a) Cross-sectional profile of borosilicate glass coating before modification and after modification (b)
Detailed Description
The invention will now be further described with reference to the following examples, and the accompanying drawings:
example 1:
1) Respectively weighing SiO with the mol percentage content of 70 percent 2 Powder, 20% of B 2 O 3 Powder, 9% Al 2 O 3 Powder and 1 percent of Sm 2 O 3 Ball milling the powder for 3h, and mixing uniformly for later use;
2) Placing the mixed raw material powder into a corundum crucible, placing the corundum crucible into a muffle furnace, heating the corundum crucible and the muffle furnace to 1573K in the air atmosphere, continuously performing heat treatment for 2 hours to enable the raw material powder to be fully melted and reacted at high temperature, and then directly taking out the raw material powder and cooling the raw material powder to room temperature to obtain Sm modified borosilicate glass;
3) In order to facilitate the subsequent repair and use, the Sm modified borosilicate glass block body which is formed by melting is ground into powder;
4) The fiber laser is used for cladding the damaged area of the C/C composite SiC coating on the modified glass powder, and the modification effect of the rare earth element Sm on the borosilicate glass coating is detected through process parameter comparison and coating morphology observation. Wherein, the laser power is set to be 300W, the spot diameter is 4mm, the scanning speed is 7mm/s, the thickness of the preset layer is 0.4mm, single-pass scanning is adopted, and no lap joint exists.
Example 2:
1) Respectively weighing SiO with the mol percentage of 70 percent 2 Powder, 20% of B 2 O 3 Powder, 5% Al 2 O 3 Powder and 5% of Sm 2 O 3 Ball milling the powder for 3h, and mixing uniformly for later use;
2) Placing the mixed raw material powder into a corundum crucible, placing the corundum crucible into a muffle furnace, heating the corundum crucible and the muffle furnace to 1573K in the air atmosphere, continuously carrying out heat treatment for 2 hours to ensure that the raw material powder is fully melted and reacted at high temperature, and then directly taking out the raw material powder and cooling the raw material powder to room temperature to obtain Sm modified borosilicate glass;
3) In order to facilitate the subsequent repair and use, the Sm modified borosilicate glass block body which is formed by melting is ground into powder;
4) The fiber laser is used for cladding the damaged area of the C/C composite SiC coating on the modified glass powder, and the modification effect of the rare earth element Sm on the borosilicate glass coating is detected through process parameter comparison and coating morphology observation. Wherein, the laser power is set to be 300W, the spot diameter is 4mm, the scanning speed is 8mm/s, the thickness of the preset layer is 0.4mm, and single-channel scanning without lap joint is adopted.
Example 3:
1) Respectively weighing SiO with 65 mol percent 2 Powder, 20% of B 2 O 3 Powder, 5% Al 2 O 3 Powder and 10 percent of Sm 2 O 3 Ball milling the powder for 3h, and mixing uniformly for later use;
2) Placing the mixed raw material powder into a corundum crucible, placing the corundum crucible into a muffle furnace, heating the corundum crucible and the muffle furnace to 1573K in the air atmosphere, continuously carrying out heat treatment for 2 hours to ensure that the raw material powder is fully melted and reacted at high temperature, and then directly taking out the raw material powder and cooling the raw material powder to room temperature to obtain Sm modified borosilicate glass;
3) In order to facilitate subsequent repair and use, the Sm modified borosilicate glass block body which is subjected to melt molding is ground into powder;
4) The fiber laser is used for cladding the damaged area of the C/C composite SiC coating on the modified glass powder, and the modification effect of the rare earth element Sm on the borosilicate glass coating is detected through process parameter comparison and coating morphology observation. Wherein, the laser power is 300W, the spot diameter is 4mm, the scanning speed is 10mm/s, the thickness of the preset layer is 0.4mm, and single-channel scanning without lap joint is adopted.

Claims (1)

1. A method for repairing a carbon/carbon composite SiC coating by laser cladding by using a modified glass material is characterized by comprising the following steps: the modified glass material adopts rare earth element samarium Sm to modify borosilicate glass, so that the absorption rate of a laser band covered by the fiber laser is improved; the material comprises the following components: siO with molar percentage of 65 to 80 percent 2 Powder and 15 to 20 percent of B 2 O 3 Powder, 4 to 10 percent of Al 2 O 3 Powder and 1 to 10 percent of Sm 2 O 3 Pulverizing;
the method comprises the following steps:
step 1, raw material preparation: siO with the mol percentage of 65-80 percent 2 Powder, 15-20% of B 2 O 3 Powder, 4-10% of Al 2 O 3 Mixing the powder with 1-10% of Sm 2 O 3 Ball milling the powder and mixing uniformly;
step 2, melting and forming: placing the mixed raw material powder into a corundum crucible, placing the corundum crucible into a muffle furnace, heating to 1573-1773K along with the furnace in the air atmosphere, continuously heating for 1-2 h to enable the raw material powder to be fully melted and reacted at high temperature, and then directly taking out the raw material powder and cooling to room temperature to obtain Sm modified borosilicate glass;
step 3, grinding to prepare powder: grinding the Sm modified borosilicate glass block into powder for repairing a carbon/carbon composite SiC coating;
step 4, cladding repair: carrying out cladding on a damaged area of a C/C composite SiC coating on modified glass powder by using a fiber laser, and inspecting the modification effect of the rare earth element Sm on the borosilicate glass coating by comparing process parameters and observing the appearance of the coating, wherein the laser power is set to be 300-500W, the diameter of a light spot is 2-5 mm, the scanning speed is 5-10 mm/s, and the thickness of a preset layer is 0.2-0.5 mm.
CN202011360860.8A 2020-11-27 2020-11-27 Carbon/carbon composite material SiC coating repairing modified glass material based on laser cladding method and preparation and use methods Active CN112341000B (en)

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CN1974452A (en) * 2005-07-06 2007-06-06 肖特股份有限公司 Thin flat glass for display purposes and method of cutting the thin flat glass into display sheets
CN102503585A (en) * 2011-11-23 2012-06-20 陕西科技大学 Method for preparing carbon/carbon composite antioxidant phosphate rare-earth glass coating
CN102674902A (en) * 2012-05-15 2012-09-19 陕西科技大学 Preparation method of C-AlPO4-mullite/glass layer gradient composite antioxidation coating
CN103827056A (en) * 2011-09-06 2014-05-28 赫拉克勒斯公司 Method for forming smooth glaze-like coating on substrate made of ceramic matrix composite material containing sic, and part made of ceramic matrix composite material provided with such coating
CN108975953A (en) * 2018-08-29 2018-12-11 中国科学院上海硅酸盐研究所 A kind of C/SiC composite material surface laser melting coating combines by force the preparation method of glass film layers

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FR2932176B1 (en) * 2008-06-06 2012-02-03 Snecma Propulsion Solide METHOD FOR PRODUCING A SELF-HEATING LAYER ON A PIECE OF COMPOSITE C / C MATERIAL
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Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004175605A (en) * 2002-11-26 2004-06-24 Tokai Carbon Co Ltd Oxidation-resistant c/c composite material and its manufacturing process
CN1974452A (en) * 2005-07-06 2007-06-06 肖特股份有限公司 Thin flat glass for display purposes and method of cutting the thin flat glass into display sheets
CN103827056A (en) * 2011-09-06 2014-05-28 赫拉克勒斯公司 Method for forming smooth glaze-like coating on substrate made of ceramic matrix composite material containing sic, and part made of ceramic matrix composite material provided with such coating
CN102503585A (en) * 2011-11-23 2012-06-20 陕西科技大学 Method for preparing carbon/carbon composite antioxidant phosphate rare-earth glass coating
CN102674902A (en) * 2012-05-15 2012-09-19 陕西科技大学 Preparation method of C-AlPO4-mullite/glass layer gradient composite antioxidation coating
CN108975953A (en) * 2018-08-29 2018-12-11 中国科学院上海硅酸盐研究所 A kind of C/SiC composite material surface laser melting coating combines by force the preparation method of glass film layers

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