CN111689764A - 一种低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法 - Google Patents

一种低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法 Download PDF

Info

Publication number
CN111689764A
CN111689764A CN202010639185.6A CN202010639185A CN111689764A CN 111689764 A CN111689764 A CN 111689764A CN 202010639185 A CN202010639185 A CN 202010639185A CN 111689764 A CN111689764 A CN 111689764A
Authority
CN
China
Prior art keywords
powder
defocusing
ceramic
forming
melting
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202010639185.6A
Other languages
English (en)
Other versions
CN111689764B (zh
Inventor
熊志伟
张凯
廖文和
刘婷婷
邹志永
闫志隆
陈丹
陈香媛
顾明飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing University of Science and Technology
Original Assignee
Nanjing University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing University of Science and Technology filed Critical Nanjing University of Science and Technology
Priority to CN202010639185.6A priority Critical patent/CN111689764B/zh
Publication of CN111689764A publication Critical patent/CN111689764A/zh
Application granted granted Critical
Publication of CN111689764B publication Critical patent/CN111689764B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00—Products made by additive manufacturing
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/057—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on calcium oxide
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/45—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on copper oxide or solid solutions thereof with other oxides
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
    • C04B35/505—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds based on yttrium oxide
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
    • C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
    • C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
    • C04B35/5615—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides based on titanium silicon carbides
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
    • C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
    • C04B35/5618—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides based on titanium aluminium carbides
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3229—Cerium oxides or oxide-forming salts thereof
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3826—Silicon carbides
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • C04B2235/3839—Refractory metal carbides
    • C04B2235/3843—Titanium carbides
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C04B2235/6026—Computer aided shaping, e.g. rapid prototyping
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/665—Local sintering, e.g. laser sintering
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

本发明涉及一种低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，采用以下步骤：准备陶瓷材料的粉末或粉末混合物；CAD模型的设计导入及切层；使用辊子对制备好的陶瓷材料的粉末或粉末混合物进行铺粉和压粉工序，得到粉层胚体；控制成形缸升降，将粉层胚体置于离焦状态；通过熔化热源将所述粉层胚体的特定区域加热至最高温度，熔化冷却后凝固致密一体化；判断所有切层是否完成；回收粉末原料，取出成形件。本方法充分利用低成本的不规则陶瓷粉末，可节约原料成本；通过离焦打印优化了熔池的温度场分布，减小了温度梯度。采用本发明解决了SLM陶瓷粉末要求高、加工条件苛刻、工艺及后处理复杂繁琐、零件制备成本高且性能不足等问题。

Description

一种低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法
技术领域
本发明涉及增材制造技术领域，具体涉及一种低成本激光选区熔化(SelectiveLaser Melting,SLM)用陶瓷粉末制备及其离焦成形方法。
背景技术
陶瓷及陶瓷基复合材料具有质量轻、耐高温、低热导、绝缘性和化学稳定性等优良性质，在航空航天、电子器件、生物医疗及建筑建材等领域获得广泛应用。陶瓷增材制造技术是一种先进的新兴制造技术，具有客制化定制、高设计自由度以及绿色环保等优势，能够实现复杂结构陶瓷部件的快速设计，获得了广泛关注和快速发展，有望推动陶瓷材料制造与应用技术的新一轮技术变革。
陶瓷激光选区熔化技术(SLM)利用高能量激光束逐层选择性熔化陶瓷粉末，通过逐层铺粉，逐层融化凝固堆积的方式，制造三维实体复杂零部件，该技术突破了传统制造工艺的去除成形思路，无需任何模具和脱脂烧结过程，直接成形，是制造效率最高、最具发展潜力的直接增材制造技术。
现阶段陶瓷SLM一般使用橡胶刮刀铺粉，为得到均匀的陶瓷粉层，对所使用的原料粉末要求较高，需要陶瓷粉体具有较高的球形度、流动性、纯度和较窄的粒度分布范围等等。目前，国内外有关SLM陶瓷的研究报道均采用雾化造粒法产生的球形粉末为原料，然而这种陶瓷球形粉末制备是通过粘结剂将很多小颗粒团聚在一起，粉体纯度低且制备成本高；另外陶瓷材料对应力和裂纹敏感，激光束辐照引起熔池区域产生高温度梯度，使得成形件在激热激冷的过程中反复受到热冲击并产生裂纹，就有了成形件性能不好的隐患，现阶段通过高温预热的方法不仅对设备要求高，工艺复杂，效率极低且不能完全抑制裂纹，限制了该技术的研究发展。
发明内容
为解决现有技术中存在的问题，本发明提供的一种低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，充分利用低成本的不规则陶瓷粉末的吸光性和透光性、结合离焦打印方法优化了熔池的温度场分布，减小了温度梯度，有效降低了加工成本和门槛，抑制了缺陷的产生，提高了成形效率和质量。
为实现上述目的，本发明提供的技术方案是：
一种低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，包括以下步骤：
(a)准备陶瓷材料的粉末或粉末混合物，其中包括设计粉末或粉末混合物的尺寸及粉末混合物的组分；
(b)CAD模型的设计导入及切层；
(c)使用辊子对制备好的陶瓷材料的粉末或粉末混合物进行铺粉和压粉工序，得到粉层胚体；
(d)控制成形缸升降，将粉层胚体置于离焦状态；
(e)通过熔化热源将所述粉层胚体的特定区域加热至最高温度，熔化冷却后凝固致密一体化；
(f)判断所有切层是否完成，否，则进入步骤(c)，是，则进入步骤(g)；
(g)回收粉末原料，取出成形件。
其中，步骤(a)中陶瓷材料的粉末或粉末混合物的准备包括如下步骤：
A1、原料设计：选择单一陶瓷粉末或复合陶瓷粉末原料，所述原料的粒度中位径D50的范围为0.5～50μm；
A2、湿法球磨混粉：选择酒精为媒介，将原料按球料比3:1～6:1置于氧化锆球磨罐中，磨球材质为氧化铝，直径为2～10mm，在100～200r/min的转速下，球磨2～4h；
A3、干燥：对球磨后收集的粉末浆料从球磨罐中与磨球分离，在真空干燥箱中以80～110℃干燥3～6h，干燥箱气压为5000～10000Pa；
A4、筛粉：使用300目筛网对干燥后的粉末进行筛分后得到粉末混合物，其中，所述的粉末粒度范围为0～55μm；
A5、调节通透性：将筛分后的粉末置于惰性气体保护条件下进行退火处理，加热温度为700～1000℃，保温时间0.5～72h，保温后空冷，惰性气体为氩气。
步骤(a)中的陶瓷粉末是单一陶瓷粉末或复合陶瓷粉末，所述的单一陶瓷粉末纯度≥99wt％；所述的复合陶瓷粉末为Al2O3、Y2O3、La2O3、Gd2O3、Er2O3、Eu2O3、CaO、MgO、CuO、CeO2、TiO2、SiO2、ZrO2、SiC、TiC、Ti2AlC3、Ti2SiC3中的两种以上的混合。
所述步骤(b)中切层厚度为25～60μm，扫描策略包括岛形、之字形或单向线性扫描。
所述步骤(c)中铺粉和压粉工艺包括如下步骤：
C1、基板选择：以高纯烧制陶瓷板作为基板材料固定于成形缸，基板致密度为60～99.9％；
C2、送粉：将原料装入粉料缸，送入成形缸；
C3、铺粉工艺：控制成形缸升降，调整粉层厚度，铺粉时开启辊子选转；其中粉层厚度为2～6个切层厚度，辊子旋转方向与铺粉方向保持一致；
C4、压粉工艺：上升基板，调整铺粉层底部与辊子的相对位置，间距为单个CAD零部件模型切层厚度并压粉，压粉过程中开启辊子旋转，辊子旋转方向与压粉方向相反。
所述步骤(d)中激光加工平面为离焦状态，其中，取向选择为正向离焦或负向离焦，离焦量的取值范围为0～5mm，通过升降成形缸对离焦取向和离焦量进行控制。
所述步骤(e)中，熔化热源为电弧、等离子体或电子束。
所述熔化热源为激光束时，激光器输出为连续激光或超快脉冲激光，其中，连续激光波长为400～1080nm，激光功率为20～200W，超快激光波长为1028nm，脉宽为1～1000ps，脉冲频率为1～500KHz，每个脉冲能量为2～100μJ，振镜扫描速度为20～400mm/s。
基板预热温度为100～1200℃，成形密封舱体内温度保持在28℃。
所述熔化热源为电弧、等离子体时，粉末的铺设和扫描操作环境氧气含量为0～1000ppm，其余为惰性气体；所述熔化热源为电子束时，粉末的铺设和扫描操作环境为真空环境。
与现有技术相比，本发明的有益效果是：
(1)本发明充分利用了低成本的不规则陶瓷粉末，原料成本低、利用率高及适用原始材料种类不受限制，粉末混合制备工艺简单，操作方便，成本低廉；创新地引入退火工艺，通过对陶瓷粉末中晶体结构内点缺陷浓度的调节，实现了对陶瓷粉末通透性的控制，制备出高通透性、低散射率的陶瓷粉末，有利于优化熔池温度场均匀分布，减小温度梯度，从而抑制缺陷的产生。
(2)本发明的铺粉压粉工艺充分利用了不规则小尺寸粉末蓬松、高表面能从而可压实且晶体取向各异性的特点，将辊子替代橡胶刮刀，既减少了铺粉对粉末球形度苛刻条件的依赖作用，提升了铺粉粉层的均匀平整度，也极大的提升了铺粉胚体的堆积密度和内聚力，有效的遏制了粉末飞溅，使得粉末与激光的耦合作用效率和稳定性得到提升；
(3)本发明利用陶瓷粉末具有一定透明度的性质，采用离焦的激光选区熔化工艺方法，降低了低热导率对粉末胚体吸收激光的限制作用，有效降低了粉末表面的过热，使得粉末在三维空间内受热更加均匀，利用了离焦大光斑的预热作用，进而实现多种陶瓷材料粉末的激光选区熔化稳定成形，形成超细贝壳组织的制备；
(4)本发明通过调整超快脉冲激光重复频率区间控制相互作用机制为融化机制，利用超快脉冲激光与陶瓷材料相互作用的非线性多光子吸收效应，加热过程具有热吸收效率高、热影响区域小等优势，在不损伤基材的前提下可以实现无裂纹陶瓷复杂部件的成形。
附图说明
图1为本发明中方法的流程图。
图2为采用本发明压粉离焦工艺制备高通透Al2O3-ZrO2共晶陶瓷成形件示意图。
图3为采用本发明压粉离焦工艺制备高通透Al2O3-ZrO2共晶陶瓷成形件微观组织示意图。
图4为采用本发明离焦工艺制备高通透Al2O3-ZrO2共晶陶瓷成形件微观组织示意图。
图5为采用本发明压粉工艺制备高通透Al2O3-ZrO2共晶陶瓷成形件微观组织示意图。
图6为采用本发明压粉离焦工艺制备低通透Al2O3-ZrO2共晶陶瓷成形件微观组织示意图。
具体实施方式
下面结合具体实施例对本发明作进一步详细的说明。以下实施例仅用于说明本发明而不用于限制本发明的范围。
实施例1
结合图1所示，具体制备过程为：
选用纯度为99.5％的氧化铝和氧化锆为原料粉末进行尺寸8×8×8mm的小方块的选区激光熔化制备。氧化铝粉末粒度中值为0.78μm、粉末呈现不规则的片状；氧化锆粉末粒度中值为1μm、粉末呈现不规则多面体状。选取氧化铝氧化锆质量比为61.5:38.5，选取氧化铝磨球使得球料质量比为3:1，并以酒精为媒介在200r/min下混合均匀，取高能球磨得到的陶瓷浆料在100℃、10KPa的环境下干燥2小时后进行筛粉，将筛分后粉末置于氩气气氛下进行退火处理，加热温度为700℃，保温时间72h，保温后空冷。选取99.9％致密度的烧制氧化铝板作为小方块激光选区熔化加工的基板。将模型切层，设置扫描路径间距为75μm，层厚为50μm，接着将退火处理后得到的陶瓷粉末装入粉料缸中，并将成形室内部冲入氩气作为保护气，使得氧含量降为10ppm。控制基板由焦平面下降150μm，即使得氧含铝基板与辊子间距为150μm，接着注入粉末，利用辊子将粉末从右往左均匀的铺覆到整个成形基板的上面，得到均匀的陶瓷铺粉层，其中粉末层厚度为150μm，铺粉时调整辊子旋转方向与铺粉方向一致。控制基板上升100μm，保持辊子旋转方向不变，切换辊子运动方向，利用辊子卷粉作用将粉末从左往右均匀的压覆到整个成形基板的上面，得到均匀致密的陶瓷压粉层，其中粉末层厚度为50μm。控制基板上升3mm，采用波长为1070nm的红外连续激光作为能量源，设置激光的主要参数为：功率100W，扫描速度为90mm/s，扫描模式为之字形，对离焦后的压粉层进行扫描处理，使其熔化后冷凝固结为固态层。重复步骤(c)～(d)，进行逐层的粉末铺设操作和激光扫描操作，直至完成尺寸为8×8×8mm的小方块的选区激光熔化制备，最终获得如图2和图3所示的成形件。
另外，在本实施例中，虽然第一热源选用了连续激光作为热源，但是，在其他实施例中，也可以选用其他热源作为第一热源进行粉末层的第一次熔化成形扫描处理，例如超快脉冲激光、电弧、等离子体或电子束，特别的，在选用电子束作为热源时，需保证铺粉和扫描的环境为真空环境，选用电弧或等离子体作为热源时，需保证铺粉和扫描的环境为惰性气氛环境。
优选的，在本实施例中，为了保证粉末熔化凝固成形质量，需要避免超快脉冲激光与陶瓷材料相互作用的非线性效应而产生烧蚀、等离子体或气化等机制，因此需控制脉冲激光参数在低能量和高重复频率区间内，相互作用为热效应融化机制，从而提高成形件最终的质量。
对比例1
采用与实施例1相同的方法对氧化铝氧化锆共晶陶瓷进行8×8×8mm的小方块的选区激光熔化制备，其区别仅在于：未实施步骤(c)的铺粉压粉工序，直接铺粉得到致密度低的粉层，并最终获得如图4所示表面形貌的成形件。实施例1由于压粉工艺，粉层均匀平整，铺粉胚体的堆积密度和内聚力得到提升，有效的遏制了粉末飞溅，使得粉末与激光的耦合作用效率和稳定性得到提升，因此试件中裂纹得到抑制，熔道更加稳定均匀。
对比例2
采用与实施例1相同的方法对氧化铝氧化锆共晶陶瓷进行8×8×8mm的小方块的选区激光熔化制备，其区别仅在于：未实施步骤(d)的离焦工序，而是使用连续红外激光直接定焦熔化，并最终获得如图5所示表面形貌的成形件。实施例1由于离焦工艺，降低了低热导率对粉末胚体吸收激光的限制作用，有效降低了粉末表面的过热，抑制了飞溅的同时使得粉末在三维空间内受热更加均匀，利用了离焦大光斑的预热作用，实现了裂纹抑制和熔道稳定。
对比例3
采用与实施例1相同的方法对氧化铝氧化锆共晶陶瓷进行8×8×8mm的小方块的选区激光熔化制备，其区别仅在于：未实施步骤(a)的粉末退火处理工艺，仅使用低通透性的筛分后陶瓷粉末，连续红外激光单能量源离焦成形，并最终获得如图6所示表面形貌的成形件。实施例1由于施加72小时700℃的退火处理，降低氧化铝氧化锆粉末中晶体氧缺位的浓度，提升粉末的通透性，有利于优化熔池温度场均匀分布，减小温度梯度，从而抑制缺陷的产生。
以上所述，仅是本发明的较佳实施例，并非对本发明作任何形式上的限制，任何熟悉本专业的技术人员，在不脱离本发明技术方案范围内，依据本发明的技术实质，对以上实施例所作的任何简单的修改、等同替换与改进等，均仍属于本发明技术方案的保护范围之内。

Claims (10)

1.一种低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，其特征在于：包括以下步骤：
(a)准备陶瓷材料的粉末或粉末混合物，其中包括设计粉末或粉末混合物的尺寸及粉末混合物的组分；
(b)CAD模型的设计导入及切层；
(c)使用辊子对制备好的陶瓷材料的粉末或粉末混合物进行铺粉和压粉工序，得到粉层胚体；
(d)控制成形缸升降，将粉层胚体置于离焦状态；
(e)通过熔化热源将所述粉层胚体的特定区域加热至最高温度，熔化冷却后凝固致密一体化；
(f)判断所有切层是否完成，否，则进入步骤(c)，是，则进入步骤(g)；
(g)回收粉末原料，取出成形件。
2.根据权利要求1所述的低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，其特征在于：步骤(a)中陶瓷材料的粉末或粉末混合物的准备包括如下步骤：
A1、原料设计：选择单一陶瓷粉末或复合陶瓷粉末原料，所述原料的粒度中位径D50的范围为0.5～50μm；
A2、湿法球磨混粉：选择酒精为媒介，将原料按球料比3:1～6:1置于氧化锆球磨罐中，磨球材质为氧化铝，直径为2～10mm，在100～200r/min的转速下，球磨2～4h；
A3、干燥：对球磨后收集的粉末浆料从球磨罐中与磨球分离，在真空干燥箱中以80～110℃干燥3～6h，干燥箱气压为5000～10000Pa；
A4、筛粉：使用300目筛网对干燥后的粉末进行筛分后得到粉末混合物，其中，所述的粉末粒度范围为0～55μm；
A5、调节通透性：将筛分后的粉末置于惰性气体保护条件下进行退火处理，加热温度为700～1000℃，保温时间0.5～72h，保温后空冷，惰性气体为氩气。
3.根据权利要求1所述的低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，其特征在于：步骤(a)中的陶瓷粉末是单一陶瓷粉末或复合陶瓷粉末，所述的单一陶瓷粉末纯度≥99wt％；所述的复合陶瓷粉末为Al2O3、Y2O3、La2O3、Gd2O3、Er2O3、Eu2O3、CaO、MgO、CuO、CeO2、TiO2、SiO2、ZrO2、SiC、TiC、Ti2AlC3、Ti2SiC3中的两种以上的混合。
4.根据权利要求1所述的低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，其特征在于：所述步骤(b)中切层厚度为25～60μm，扫描策略包括岛形、之字形或单向线性扫描。
5.根据权利要求1所述的低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，其特征在于：所述步骤(c)中铺粉和压粉工艺包括如下步骤：
C1、基板选择：以高纯烧制陶瓷板作为基板材料固定于成形缸，基板致密度为60～99.9％；
C2、送粉：将原料装入粉料缸，送入成形缸；
C3、铺粉工艺：控制成形缸升降，调整粉层厚度，铺粉时开启辊子选转；其中粉层厚度为2～6个切层厚度，辊子旋转方向与铺粉方向保持一致；
C4、压粉工艺：上升基板，调整铺粉层底部与辊子的相对位置，间距为单个CAD零部件模型切层厚度并压粉，压粉过程中开启辊子旋转，辊子旋转方向与压粉方向相反。
6.根据权利要求1所述的低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，其特征在于：所述步骤(d)中激光加工平面为离焦状态，其中，取向选择为正向离焦或负向离焦，离焦量的取值范围为0～5mm，通过升降成形缸对离焦取向和离焦量进行控制。
7.根据权利要求1所述的低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，其特征在于：所述步骤(e)中，熔化热源为电弧、等离子体或电子束。
8.根据权利要求7所述的低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，其特征在于：所述熔化热源为激光束时，激光器输出为连续激光或超快脉冲激光，其中，连续激光波长为400～1080nm，激光功率为20～200W，超快激光波长为1028nm，脉宽为1～1000ps，脉冲频率为1～500KHz，每个脉冲能量为2～100μJ，振镜扫描速度为20～400mm/s。
9.根据权利要求8所述的低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，其特征在于：基板预热温度为100～1200℃，成形密封舱体内温度保持在28℃。
10.根据权利要求7所述的低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法，其特征在于：所述熔化热源为电弧、等离子体时，粉末的铺设和扫描操作环境氧气含量为0～1000ppm，其余为惰性气体；所述熔化热源为电子束时，粉末的铺设和扫描操作环境为真空环境。
CN202010639185.6A 2020-07-06 2020-07-06 一种低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法 Active CN111689764B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010639185.6A CN111689764B (zh) 2020-07-06 2020-07-06 一种低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010639185.6A CN111689764B (zh) 2020-07-06 2020-07-06 一种低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法

Publications (2)

Publication Number Publication Date
CN111689764A true CN111689764A (zh) 2020-09-22
CN111689764B CN111689764B (zh) 2022-05-31

Family

ID=72485248

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010639185.6A Active CN111689764B (zh) 2020-07-06 2020-07-06 一种低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法

Country Status (1)

Country Link
CN (1) CN111689764B (zh)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113798501A (zh) * 2021-08-10 2021-12-17 西安理工大学 纳米Al2O3增强3D打印铝基复合材料及制备方法
CN117921026A (zh) * 2024-03-27 2024-04-26 广东工业大学 一种使用lpbf工艺增材制造超薄零部件的离焦调控成形方法

Citations (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1648802A (zh) * 2004-12-03 2005-08-03 清华大学 一种电子束选区同步烧结工艺及三维分层制造设备
DE102008021507A1 (de) * 2008-04-30 2009-11-05 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zur Herstellung von keramischen Objekten mittels selektiven Laserschmelzens
CN101700977A (zh) * 2009-10-30 2010-05-05 武汉理工大学 一种快速制备MgAlON透明陶瓷粉末的方法
CN102432302A (zh) * 2011-09-08 2012-05-02 大连理工大学 一种激光束近净成形陶瓷结构的方法
CN104526836A (zh) * 2014-12-19 2015-04-22 南京工业大学 一种基于选择性激光熔化技术的固体无机物粉末3d打印方法
US20150251247A1 (en) * 2004-03-16 2015-09-10 Evonik Degussa Gmbh Method and device for producing three-dimensional objects using laser technology and for applying an absorber using an inkjet method
DE102015205316A1 (de) * 2015-03-24 2016-09-29 Siemens Aktiengesellschaft Verfahren zum Erzeugen eines Bauteiles aus einer Superlegierung mit einem pulverbettbasierten additiven Herstellungsverfahren und Bauteil aus einer Superlegierung
CN107973607A (zh) * 2016-10-21 2018-05-01 南京理工大学 一种无粘结剂的陶瓷浆料激光选区熔化/烧结成形方法
CN108080621A (zh) * 2017-11-21 2018-05-29 北京科技大学 低成本激光选区熔化用钛粉、其制备方法及钛材制备方法
CN109047762A (zh) * 2018-08-31 2018-12-21 江苏大学 一种激光选区熔化与激光切割复合的增材制造方法
CN109440051A (zh) * 2018-11-27 2019-03-08 陈涛 一种氧化铝陶瓷涂层及其制备方法
CN109434118A (zh) * 2018-10-30 2019-03-08 华中科技大学 一种非晶增强金属基复合材料的制备与成形方法
CN109761608A (zh) * 2019-03-07 2019-05-17 江苏师范大学 一种基于直写成型3d打印技术制备棒状复合透明陶瓷的方法
CN109887769A (zh) * 2019-01-18 2019-06-14 西安交通大学 基于选区激光成型的梯度功能钨铜材料电触头及制备方法
CN110683769A (zh) * 2019-10-25 2020-01-14 赣州中瓷科技有限公司 一种增强的钙硼硅微晶玻璃复合材料及其制备方法
CN111278618A (zh) * 2017-10-27 2020-06-12 佳能株式会社 陶瓷造型物的制造方法

Patent Citations (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150251247A1 (en) * 2004-03-16 2015-09-10 Evonik Degussa Gmbh Method and device for producing three-dimensional objects using laser technology and for applying an absorber using an inkjet method
CN1648802A (zh) * 2004-12-03 2005-08-03 清华大学 一种电子束选区同步烧结工艺及三维分层制造设备
DE102008021507A1 (de) * 2008-04-30 2009-11-05 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zur Herstellung von keramischen Objekten mittels selektiven Laserschmelzens
CN101700977A (zh) * 2009-10-30 2010-05-05 武汉理工大学 一种快速制备MgAlON透明陶瓷粉末的方法
CN102432302A (zh) * 2011-09-08 2012-05-02 大连理工大学 一种激光束近净成形陶瓷结构的方法
CN104526836A (zh) * 2014-12-19 2015-04-22 南京工业大学 一种基于选择性激光熔化技术的固体无机物粉末3d打印方法
DE102015205316A1 (de) * 2015-03-24 2016-09-29 Siemens Aktiengesellschaft Verfahren zum Erzeugen eines Bauteiles aus einer Superlegierung mit einem pulverbettbasierten additiven Herstellungsverfahren und Bauteil aus einer Superlegierung
CN107973607A (zh) * 2016-10-21 2018-05-01 南京理工大学 一种无粘结剂的陶瓷浆料激光选区熔化/烧结成形方法
CN111278618A (zh) * 2017-10-27 2020-06-12 佳能株式会社 陶瓷造型物的制造方法
CN108080621A (zh) * 2017-11-21 2018-05-29 北京科技大学 低成本激光选区熔化用钛粉、其制备方法及钛材制备方法
CN109047762A (zh) * 2018-08-31 2018-12-21 江苏大学 一种激光选区熔化与激光切割复合的增材制造方法
CN109434118A (zh) * 2018-10-30 2019-03-08 华中科技大学 一种非晶增强金属基复合材料的制备与成形方法
CN109440051A (zh) * 2018-11-27 2019-03-08 陈涛 一种氧化铝陶瓷涂层及其制备方法
CN109887769A (zh) * 2019-01-18 2019-06-14 西安交通大学 基于选区激光成型的梯度功能钨铜材料电触头及制备方法
CN109761608A (zh) * 2019-03-07 2019-05-17 江苏师范大学 一种基于直写成型3d打印技术制备棒状复合透明陶瓷的方法
CN110683769A (zh) * 2019-10-25 2020-01-14 赣州中瓷科技有限公司 一种增强的钙硼硅微晶玻璃复合材料及其制备方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
潘裕柏: "《稀土陶瓷材料》", 31 May 2016, 北京：冶金工业出版社, pages: 106 - 107 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113798501A (zh) * 2021-08-10 2021-12-17 西安理工大学 纳米Al2O3增强3D打印铝基复合材料及制备方法
CN117921026A (zh) * 2024-03-27 2024-04-26 广东工业大学 一种使用lpbf工艺增材制造超薄零部件的离焦调控成形方法

Also Published As

Publication number Publication date
CN111689764B (zh) 2022-05-31

Similar Documents

Publication Publication Date Title
US9944021B2 (en) Additive manufacturing 3D printing of advanced ceramics
Juste et al. Shaping of ceramic parts by selective laser melting of powder bed
KR101935446B1 (ko) 세라믹 입자 혼합물, 및 그러한 혼합물로부터 세라믹 부품의 제조방법
CN111689764B (zh) 一种低成本激光选区熔化用陶瓷粉末制备及其离焦成形方法
JP5384564B2 (ja) 多孔質焼結体
JP7362718B2 (ja) 造形方法および造形用の粉末材料
CN102513707B (zh) 一种激光切割陶瓷的方法
EP2784045A1 (en) Selective laser sintering/melting process
AU2010283737A2 (en) Ceramic or glass-ceramic article and methods for producing such article
CA2451495A1 (en) Thermal barrier coating material, method of production thereof, and gas turbine member and gas turbine applying said thermal barrier coating material
TW201609378A (zh) 透明尖晶石物件及用以製造該物件之薄帶成型方法
KR101384968B1 (ko) 통기성 자기용 소지 조성물 및 이를 이용한 통기성 자기의 제조방법
TWI546272B (zh) 陶瓷粉體與其形成方法及雷射燒結成型方法
US20220306540A1 (en) Method for preparing infrared radiation ceramic material
CN102924087A (zh) 一种立方氮化硼-碳化硅复相陶瓷材料的制备方法及其产品
WO2021172128A1 (ja) 焼結体の製造方法
JP5685152B2 (ja) 多孔質発熱体
WO2017053850A2 (en) Additive manufacturing 3d printing of advanced ceramics
CN113264767A (zh) 一种氧化铝/gap共晶陶瓷及其制备方法
Fan et al. Advances and Challenges in Direct Additive Manufacturing of Dense Ceramic Oxides
JP2019181930A (ja) セラミックス粉体、セラミックス粉体の製造方法およびセラミックス粉体を用いたセラミックス構造物の製造方法
KUWANA et al. Fabrication of carbon-decorated Al2O3 composite powders using cellulose nanofiber for selective laser sintering
KR20170077972A (ko) 고강도 도자기의 제조방법
CN107686341B (zh) 一种陶瓷产品及其制备方法
Gan et al. Selective Laser Melting Of Spodumene: An Exploratory Study

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant