CN114014652A - 低温烧结氧化锆陶瓷及其制备工艺 - Google Patents
低温烧结氧化锆陶瓷及其制备工艺 Download PDFInfo
- Publication number
- CN114014652A CN114014652A CN202111314291.8A CN202111314291A CN114014652A CN 114014652 A CN114014652 A CN 114014652A CN 202111314291 A CN202111314291 A CN 202111314291A CN 114014652 A CN114014652 A CN 114014652A
- Authority
- CN
- China
- Prior art keywords
- zirconia
- temperature
- low
- ceramic
- sintered
- 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.)
- Pending
Links
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 272
- 239000000919 ceramic Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 33
- 239000002270 dispersing agent Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 44
- 239000002002 slurry Substances 0.000 claims description 33
- 235000015895 biscuits Nutrition 0.000 claims description 28
- 239000007921 spray Substances 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000005469 granulation Methods 0.000 claims description 17
- 238000000227 grinding Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- 238000000498 ball milling Methods 0.000 claims description 16
- 230000003179 granulation Effects 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000292 calcium oxide Substances 0.000 claims description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims description 2
- 238000009766 low-temperature sintering Methods 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 7
- 239000002131 composite material Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 238000001035 drying Methods 0.000 description 11
- 238000003756 stirring Methods 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 8
- 229910001928 zirconium oxide Inorganic materials 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- 239000004576 sand Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000011268 mixed slurry Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000013001 point bending Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 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 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000009690 centrifugal atomisation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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
- C04B35/48—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
- C04B35/486—Fine ceramics
- C04B35/488—Composites
-
- 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
- C04B35/486—Fine ceramics
- C04B35/488—Composites
- C04B35/4885—Composites with aluminium 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
- C04B35/622—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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62695—Granulation or pelletising
-
- 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
- C04B2235/65—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
- C04B2235/6562—Heating rate
-
- 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
- C04B2235/6567—Treatment time
-
- 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
本发明涉及氧化锆陶瓷技术领域,具体涉及一种低温烧结氧化锆陶瓷及其制备工艺。所述的低温烧结氧化锆陶瓷,包括以下质量分数的原料制成:92%~98%氧化锆烧成料,2%~8%的烧结助剂;分散剂的加入质量为氧化锆烧成料和烧结助剂总质量和的0.02%~0.04%。本发明提供一种低温烧结氧化锆陶瓷,成本低、强度高、韧性好,制备工艺简单易操作。本发明还提供其制备工艺。
Description
技术领域
本发明涉及氧化锆陶瓷技术领域,具体涉及一种低温烧结氧化锆陶瓷及其制备工艺。
背景技术
氧化锆陶瓷是近年来逐渐发展起来的一类新型陶瓷。由于在粉体合成、成型工艺、烧结技术等方面取得的成就,氧化锆陶瓷的研究和应用获得了快速发展。氧化锆陶瓷不仅在化工、冶金、机械、能源、环保等领域得到广泛应用,而且在航空航天、生物医学、国防建设等尖端技术领域也展现出广阔的应用前景,氧化锆陶瓷已成为新材料家族中的重要组成部分。国内外制备氧化锆陶瓷的报道很多,但大都是在高温下制得的,在相对较低的温度下制备高强度、高韧性的氧化锆陶瓷却少之又少。
CN105367056B专利公开了氧化锆陶瓷造粒粉的制备方法,将氧化锆粉体、分散剂、表面活性剂、抗菌剂及去离子水混合后球磨制成浆料,加入粘结剂,喷雾造粒,得到氧化锆陶瓷造粒粉,通过在制备过程中分别加入分散剂及粘结剂,能够使得到的氧化锆陶瓷造粒粉形状规则,提高了造粒粉的压制性能,但所用表面活性剂成本高,重金属添加剂产生环境污染问题。
CN111825467A专利公开了一种利用喷雾造粒机制备纳米氧化锆的方法,采用凝胶-造粒的方式,通过喷雾造粒机的加热干燥特性,将配置好的凝胶系及锆源溶液,然后将凝胶颗粒浸泡于氨水中,烘干凝胶,煅烧,获得纳米锆粉,过程中先凝胶后反应也从源头上克服了纳米粉体团聚的问题,但制造凝胶过程复杂,凝胶需要保持在0-5℃的温度进行操作,增加了操作难度,且喷雾造粒时的温度较低,制备的氧化锆粉体含水量较大,影响后期生坯的加工性能。
CN111825467A专利公开了一种低成本氧化锆增韧氧化铝陶瓷造粒粉的制备方法,以氧化钇稳定的氧化锆粉料、微晶氧化铝粉料和结合剂为主要原料,以水为分散介质,在室温条件下球磨混料后得到均匀的混合浆体;再将混合浆体转移到搅拌桶中,加入粘结剂,搅拌后得到混合均匀的浆液;然后浆液经过压力雾化或离心雾化在喷雾造粒塔中进行喷雾造粒获得造粒粉,喷雾造粒工艺和采用的设备简单,成本低,制备的氧化锆增韧氧化铝陶瓷造粒粉纯度高,但氧化锆增韧氧化铝陶瓷,主要原料为60%~80%的氧化铝,且喷雾造粒时进出塔温度较高,由此制备的粉体含水量较低,后期成型比较困难。
发明内容
本发明要解决的技术问题是提供一种低温烧结氧化锆陶瓷,成本低、强度高、韧性好,制备工艺简单易操作。本发明还提供其制备工艺。
本发明所述的低温烧结氧化锆陶瓷,包括以下质量分数的原料制成:92%~98%氧化锆烧成料,2%~8%的烧结助剂;分散剂的加入质量为氧化锆烧成料和烧结助剂总质量和的0.02%~0.04%。
烧结助剂为氧化镁、氧化铝、氧化钙、氧化铋一种多种。
分散剂为丙烯酸、聚乙烯醇、聚乙二醇中的一种。
所述的低温烧结氧化锆陶瓷的制备工艺,包括以下步骤:
(1)溶解氧化锆烧成料,加入烧结助剂和分散剂混合,调节粘度,得到氧化锆料浆;
(2)将氧化锆料浆球磨,喷雾造粒,得到氧化锆粉体;
(3)将氧化锆粉体经预成型、高压脱模后,得到陶瓷素坯;
(4)将陶瓷素坯低温烧结,得到氧化锆陶瓷。
溶解氧化锆烧成料质量浓度为70%~80%的水溶液;烧结助剂溶液的质量浓度为0.15%~0.4%;分散剂溶液的质量浓度为0.02%~0.04%。
用氨水溶液调节粘度至10~15Pa.s。
球磨时间为50min~70min,球磨粒度研磨至0.50μm~0.60μm。
喷雾造粒的工艺条件为:进风温度为180℃~195℃,出风温度为80℃~95℃,转速为9000r/min~10000r/min。
预成型压力为100~150kg/cm2,并保压10s~30s,然后高压脱模,经打磨后,得到陶瓷素坯。
陶瓷素坯的低温烧结工艺包括:陶瓷素坯将以1.5℃/min~5℃/min的升温速率升温至1260℃~1360℃,保温2~8h。
具体地,所述的低温烧结氧化锆陶瓷的制备工艺,包括以下步骤:
(1)溶解氧化锆烧成料为浓度为70%~80%的水溶液,加入烧结助剂溶液的质量浓度为0.15%~0.4%,加入分散剂溶液的质量浓度为0.02%~0.04%,混合,通过加入氨水的量来调节料浆的PH,进而达到调节其粘度的目的,得到氧化锆料浆;
(2)将氧化锆料浆进行搅拌球磨,磨研50min~70min,然后用砂磨机研磨所述浆体粒度至0.50μm~0.60μm;然后喷雾造粒,喷雾造粒在喷雾干燥机中进行,喷雾造粒的工艺条件为:进风温度为180℃~195℃,出风温度为80℃~95℃,转速为9000r/min~10000r/min,干燥得到氧化锆粉体;
(3)将氧化锆粉体预成型,压力为100~150kg/cm2,并保压10s~30s,然后高压脱模,经打磨后,得到陶瓷素坯;
(4)将陶瓷素坯以1.5℃/min~5℃/min的升温速率升温至1260℃~1360℃之间进行烧结,保温2h~8h,得到氧化锆陶瓷。
本发明的低温烧结氧化锆陶瓷的制备工艺,采用氧化锆烧结料,进行水溶解,与分散剂和烧结助剂进行混合,然后经过搅拌球磨,喷雾造粒干燥制得氧化锆粉体,制备的粉体进行低温烧结即可制得复杂陶瓷构件。
与现有技术相比,本发明具有以下的有益效果:
(1)本发明的低温烧结氧化锆陶瓷的制备工艺,操作简单,通过喷雾造粒制备氧化锆粉体,粉体颗粒均匀近乎球形,将所制备粉体进一步成型,烧结体质地均匀、强度高,适用于制备精密复杂的结构件;
(2)本发明的低温烧结氧化锆陶瓷的制备工艺,在低烧结温度下(1245℃~1345℃)操作,节能减耗;
(3)本发明所述的低温烧结氧化锆陶瓷,综合性能优越,密度在6.04g/cm3以上,三点抗弯强度≥700Mpa,维氏硬度≥1200,烧结体中氧化锆含量为88-98mol%。
具体实施方式
本发明提供了一种低温烧结氧化锆陶瓷及其制备工艺,本领域技术人员可以借鉴本文内容,适当改进工艺参数实现。特别需要指出的是,所有类似的替换和改动对本领域技术人员来书是显而易见的,它们都属于本发明保护的范围。本发明的制备方法已经通过较佳实施例进行了描述,相关人员明显能在不脱离本发明内容、精神和范围内对本发明的制备方法进行改动和适当变更与组合,来实现和应用本发明技术。
为了进一步说明本发明,以下结合实施例对本发明提供的低温烧结氧化锆陶瓷及其制备工艺进行详细描述。以下实施例中的氧化锆烧成料,均采用市售材料。
实施例1
所述的低温烧结氧化锆陶瓷的制备工艺,包括以下步骤:
(1)将氧化锆烧成料溶解到纯水中,配成溶质含量为70%的水溶液,得到氧化锆料浆;氧化锆烧成料质量百分数为92%,氧化镁的质量百分数为8%,聚乙烯醇的质量为氧化锆烧成料和氧化镁总质量的0.02%,调节粘度为10Pa.s,得到氧化锆料浆;
(2)将氧化锆料浆进行搅拌球磨,磨研60min,然后用砂磨机研磨所述浆体粒度至0.50μm;然后喷雾造粒,进风温度为180℃,出风温度为85℃,转速为9300r/min,200℃干燥得到氧化锆粉体,粉体含水量为0.5%;
(3)将氧化锆粉体预成型,压力为100kg/cm2,并保压10s,然后高压脱模,经打磨后,得到陶瓷素坯;
(4)将陶瓷素坯以2℃/min的升温速率升温至1280℃进行烧结,保温2h,得到氧化锆陶瓷。
实施例2
所述的低温烧结氧化锆陶瓷的制备工艺,包括以下步骤:
(1)将氧化锆烧成料溶解到纯水中,配成溶质含量为75%的水溶液,得到氧化锆料浆;氧化锆烧成料质量百分数为95%,氧化铝的质量百分数为5%,聚乙二醇的质量为氧化锆烧成料和氧化铝总质量的0.02%,调节粘度为15Pa.s,得到氧化锆料浆;
(2)将氧化锆料浆进行搅拌球磨,磨研65min,然后用砂磨机研磨所述浆体粒度至0.53μm;然后喷雾造粒,进风温度为185℃,出风温度为90℃,转速为9500r/min,200℃干燥得到氧化锆粉体,粉体含水量为0.8%;
(3)将氧化锆粉体预成型,压力为120kg/cm2,并保压15s,然后高压脱模,经打磨后,得到陶瓷素坯;
(4)将陶瓷素坯以3℃/min的升温速率升温至1300℃进行烧结,保温3h,得到氧化锆陶瓷。
实施例3
所述的低温烧结氧化锆陶瓷的制备工艺,包括以下步骤:
(1)将氧化锆烧成料溶解到纯水中,配成溶质含量为78%的水溶液,得到氧化锆料浆;氧化锆烧成料质量百分比为96%,氧化钙的质量百分比为4%,丙烯酸树脂的质量为氧化锆烧成料和氧化钙总质量的0.04%,调节粘度为12Pa.s,得到氧化锆料浆;
(2)将氧化锆料浆进行搅拌球磨,磨研70min,然后用砂磨机研磨所述浆体粒度至0.55μm;然后喷雾造粒,进风温度为190℃,出风温度为90℃,转速为9800r/min,200℃干燥得到氧化锆粉体,粉体含水量为0.8%;
(3)将氧化锆粉体预成型,压力为130kg/cm2,并保压20s,然后高压脱模,经打磨后,得到陶瓷素坯;
(4)将陶瓷素坯以1.8℃/min的升温速率升温至1320℃进行烧结,保温3h,得到氧化锆陶瓷。
实施例4
所述的低温烧结氧化锆陶瓷的制备工艺,包括以下步骤:
(1)将氧化锆烧成料溶解到纯水中,配成溶质含量为72%的水溶液,得到氧化锆料浆;氧化锆烧成料质量百分比为98%,氧化钙的质量百分比为2%,丙烯酸树脂的质量为氧化锆烧成料和氧化钙总质量的0.02%,调节粘度为12Pa.s,得到氧化锆料浆;
(2)将氧化锆料浆进行搅拌球磨,磨研60min,然后用砂磨机研磨所述浆体粒度至0.56μm;然后喷雾造粒,进风温度为188℃,出风温度为86℃,转速为10000r/min,200℃干燥得到氧化锆粉体,粉体含水量为0.9%;
(3)将氧化锆粉体预成型,压力为150kg/cm2,并保压30s,然后高压脱模,经打磨后,得到陶瓷素坯;
(4)将陶瓷素坯以2.2℃/min的升温速率升温至1340℃进行烧结,保温2h,得到氧化锆陶瓷。
对比例1
一种的氧化锆陶瓷的制备工艺,包括以下步骤:
(1)将氧化锆烧成料溶解到纯水中,配成溶质含量为70%的水溶液,得到氧化锆料浆;氧化锆烧成料质量百分数为90%,氧化镁的质量百分数为10%,聚乙烯醇的质量为氧化锆烧成料和氧化镁的总质量的0.02%;
(2)将氧化锆料浆进行搅拌球磨,磨研60min,然后用砂磨机研磨所述浆体粒度至0.50μm;然后喷雾造粒,进风温度为180℃,出风温度为85℃,转速为9300r/min,200℃干燥得到氧化锆粉体,粉体含水量为0.8%;
(3)将氧化锆粉体预成型,压力为100kg/cm2,并保压10s,然后高压脱模,经打磨后,得到陶瓷素坯;
(4)将陶瓷素坯以2℃/min的升温速率升温至1430℃之间进行烧结,保温2h,得到氧化锆陶瓷。
对比例2
一种的氧化锆陶瓷的制备工艺,包括以下步骤:
(1)将氧化锆烧成料溶解到纯水中,配成溶质含量为75%的水溶液,得到氧化锆料浆;氧化锆烧成料质量百分比为95%,烧结助剂为氧化钇,质量百分比为5%,分散剂为0.03%的聚乙醇胺;
(2)将氧化锆料浆进行搅拌球磨,磨研65min,然后用砂磨机研磨所述浆体粒度至0.53μm;然后喷雾造粒,进风温度为185℃,出风温度为90℃,转速为9500r/min,干燥得到氧化锆粉体,粉体含水量为0.9%;
(3)将氧化锆粉体成型为陶瓷素坯,预成型压力为120kg/cm2,并保压15s,然后高压脱模,经打磨后,得到陶瓷素坯;
(4)将陶瓷素坯以3℃/min的升温速率升温至1530℃之间进行烧结,保温3h,得到氧化锆陶瓷。
对比例3
一种的氧化锆陶瓷的制备工艺,包括以下步骤:
(1)将氧化锆烧成料和硝酸钇源混合,配制成0.5mol/L的溶液A;
(2)将溶液A冷却至0-5℃,称取丙烯酰胺和N,N'-亚甲基双丙烯酰胺,投入溶液A中溶解,得到溶液B,并保持冷却在0~5℃的温度内;
(3)将溶液B打入喷雾造粒塔内进行凝胶反应,得到粒径为50μm的圆形颗粒,塔内的干燥温度为150℃;
(4)将颗粒浸泡在过量的氨水中2个小时,将浸泡后的颗粒进行滤出式清洗,重复多次浸泡和清洗,直至滤出液中的离子含量少于20ppm,所述氨水浓度为25%;
(5)将经过多次浸泡和清洗后的颗粒在110℃下烘干,水分含量为3.8%;
(6)将烘干后的颗粒在800℃下煅烧4小时,得到纳米氧化锆粉;
(7)将氧化锆粉体成型为陶瓷素坯,预成型压力为120kg/cm2,并保压15s,然后高压脱模,经打磨后,得到陶瓷素坯;
(8)将陶瓷素坯以3℃/min的升温速率升温至1430℃之间进行烧结,保温3h,得到氧化锆陶瓷。
将以上实施例1-4制备的低温烧结氧化锆陶瓷和对比例1-3制得的氧化锆陶瓷,进行性能检测:
密度检测方法为GB4472-84排水法;
三点抗弯强度检测方法为GB/T232-2010三点弯曲法;
维氏硬度检测方法为GB/T4340.1-2009维氏硬度计;
氧化锆含量检测方法为GB2590.1-81X射线荧光光谱分析法
检测结果如表1所示:
表1检测结果与检测标准
当然,上述内容仅为本发明的较佳实施例,不能被认为用于限定对本发明的实施例范围。本发明也并不仅限于上述举例,本技术领域的普通技术人员在本发明的实质范围内所做出的均等变化与改进等,均应归属于本发明的专利涵盖范围内。
Claims (10)
1.一种低温烧结氧化锆陶瓷,其特征在于:包括以下质量分数的原料制成:92%~98%氧化锆烧成料,2%~8%的烧结助剂;分散剂的加入质量为氧化锆烧成料和烧结助剂总质量和的0.02%~0.04%。
2.根据权利要求1所述的低温烧结氧化锆陶瓷,其特征在于:烧结助剂为氧化镁、氧化铝、氧化钙、氧化铋一种多种。
3.根据权利要求1所述的低温烧结氧化锆陶瓷,其特征在于:分散剂为丙烯酸、聚乙烯醇、聚乙二醇中的一种。
4.一种权利要求1-3任一项所述的低温烧结氧化锆陶瓷的制备工艺,其特征在于:包括以下步骤:
(1)溶解氧化锆烧成料,加入烧结助剂和分散剂混合,调节粘度,得到氧化锆料浆;
(2)将氧化锆料浆球磨,喷雾造粒,得到氧化锆粉体;
(3)将氧化锆粉体经预成型、高压脱模后,得到陶瓷素坯;
(4)将陶瓷素坯低温烧结,得到氧化锆陶瓷。
5.根据权利要求4所述的低温烧结氧化锆陶瓷的制备工艺,其特征在于:溶解氧化锆烧成料质量浓度为70%~80%的水溶液;烧结助剂溶液的质量浓度为0.15%~0.4%;分散剂溶液的质量浓度为0.02%~0.04%。
6.根据权利要求4所述的低温烧结氧化锆陶瓷的制备工艺,其特征在于:用氨水溶液调节粘度至10~15Pa.s。
7.根据权利要求4所述的低温烧结氧化锆陶瓷的制备工艺,其特征在于:球磨时间为50min~70min,球磨粒度研磨至0.50μm~0.60μm。
8.根据权利要求4所述的低温烧结氧化锆陶瓷的制备工艺,其特征在于:喷雾造粒的工艺条件为:进风温度为180℃~195℃,出风温度为80℃~95℃,转速为9000r/min~10000r/min。
9.根据权利要求4所述的低温烧结氧化锆陶瓷的制备工艺,其特征在于:预成型压力为100~150kg/cm2,并保压10s~30s,然后高压脱模,经打磨后,得到陶瓷素坯。
10.根据权利要求4所述的低温烧结氧化锆陶瓷的制备工艺,其特征在于:陶瓷素坯的低温烧结工艺包括:陶瓷素坯将以1.5℃/min~5℃/min的升温速率升温至1260℃~1360℃,保温2~8h。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111314291.8A CN114014652A (zh) | 2021-11-08 | 2021-11-08 | 低温烧结氧化锆陶瓷及其制备工艺 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202111314291.8A CN114014652A (zh) | 2021-11-08 | 2021-11-08 | 低温烧结氧化锆陶瓷及其制备工艺 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN114014652A true CN114014652A (zh) | 2022-02-08 |
Family
ID=80062315
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202111314291.8A Pending CN114014652A (zh) | 2021-11-08 | 2021-11-08 | 低温烧结氧化锆陶瓷及其制备工艺 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN114014652A (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114656260A (zh) * | 2022-04-22 | 2022-06-24 | 烟台核晶陶瓷新材料有限公司 | 一种医用高透氧化锆陶瓷烧结体的制备方法及应用 |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002104874A (ja) * | 2000-09-28 | 2002-04-10 | Tosoh Corp | ジルコニア球状焼結体の製造方法 |
CN1458119A (zh) * | 2003-04-30 | 2003-11-26 | 天津大学 | 抽油泵多元系氧化锆增韧陶瓷柱塞的制备方法 |
JP2009269812A (ja) * | 2008-04-09 | 2009-11-19 | Tosoh Corp | 透光性ジルコニア焼結体及びその製造方法並びに用途 |
CN104261821A (zh) * | 2014-09-12 | 2015-01-07 | 李正国 | 一种超耐磨氧化锆陶瓷挤头的制造工艺 |
CN106699174A (zh) * | 2017-02-10 | 2017-05-24 | 山东国瓷功能材料股份有限公司 | 高强度氧化锆烧结体用粉体及其应用 |
CN106830929A (zh) * | 2017-02-10 | 2017-06-13 | 山东国瓷功能材料股份有限公司 | 白色氧化锆烧结体及其制备方法和应用 |
CN108147814A (zh) * | 2018-01-25 | 2018-06-12 | 山东国瓷功能材料股份有限公司 | 一种低温烧结氧化锆陶瓷的方法 |
CN108341668A (zh) * | 2018-04-20 | 2018-07-31 | 内蒙古科技大学 | 一种黑色氧化锆陶瓷及其制备方法 |
CN109503185A (zh) * | 2018-11-14 | 2019-03-22 | 安徽致磨新材料科技有限公司 | 纳米氧化铝增韧增强的氧化锆陶瓷材料及其产品成型方法 |
US20190210927A1 (en) * | 2016-08-31 | 2019-07-11 | Shandong Sinocera Functional Material Co., Ltd. | High-light trasmittance zirconia sintered body, preparation method therefor and use thereof |
-
2021
- 2021-11-08 CN CN202111314291.8A patent/CN114014652A/zh active Pending
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002104874A (ja) * | 2000-09-28 | 2002-04-10 | Tosoh Corp | ジルコニア球状焼結体の製造方法 |
CN1458119A (zh) * | 2003-04-30 | 2003-11-26 | 天津大学 | 抽油泵多元系氧化锆增韧陶瓷柱塞的制备方法 |
JP2009269812A (ja) * | 2008-04-09 | 2009-11-19 | Tosoh Corp | 透光性ジルコニア焼結体及びその製造方法並びに用途 |
CN104261821A (zh) * | 2014-09-12 | 2015-01-07 | 李正国 | 一种超耐磨氧化锆陶瓷挤头的制造工艺 |
US20190210927A1 (en) * | 2016-08-31 | 2019-07-11 | Shandong Sinocera Functional Material Co., Ltd. | High-light trasmittance zirconia sintered body, preparation method therefor and use thereof |
CN106699174A (zh) * | 2017-02-10 | 2017-05-24 | 山东国瓷功能材料股份有限公司 | 高强度氧化锆烧结体用粉体及其应用 |
CN106830929A (zh) * | 2017-02-10 | 2017-06-13 | 山东国瓷功能材料股份有限公司 | 白色氧化锆烧结体及其制备方法和应用 |
CN108147814A (zh) * | 2018-01-25 | 2018-06-12 | 山东国瓷功能材料股份有限公司 | 一种低温烧结氧化锆陶瓷的方法 |
CN108341668A (zh) * | 2018-04-20 | 2018-07-31 | 内蒙古科技大学 | 一种黑色氧化锆陶瓷及其制备方法 |
CN109503185A (zh) * | 2018-11-14 | 2019-03-22 | 安徽致磨新材料科技有限公司 | 纳米氧化铝增韧增强的氧化锆陶瓷材料及其产品成型方法 |
Non-Patent Citations (1)
Title |
---|
周张健等: "《无机非金属材料工艺学》", 31 January 2010, 中国轻工业出版社 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114656260A (zh) * | 2022-04-22 | 2022-06-24 | 烟台核晶陶瓷新材料有限公司 | 一种医用高透氧化锆陶瓷烧结体的制备方法及应用 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN113831136B (zh) | 一种固相烧结碳化硅制品及其制备方法 | |
CN107759218B (zh) | 一种氧化钇稳定氧化锆陶瓷及其制备方法 | |
CN111204802B (zh) | 黑色钇稳定氧化锆粉体的制备方法 | |
CN108546118B (zh) | 一种氧化钇稳定氧化锆粉体及其制备方法和陶瓷 | |
CN108002828B (zh) | 一种等离子喷涂用ysz陶瓷造粒粉及其制备方法 | |
CN110668813A (zh) | 一种纳米氧化锆造粒粉末的制备方法 | |
CN108911753A (zh) | 一种高韧性无压烧结碳化硼陶瓷制备方法 | |
CN115368122B (zh) | 一种改性硅藻土多孔陶瓷浆料及陶瓷粉体 | |
CN112500159B (zh) | 高韧性高强度黑色氧化锆陶瓷材料的制备方法 | |
CN105294138A (zh) | 一种双峰氧化铝微粉及其制备方法 | |
CN101648814A (zh) | 一步固相反应法制备高性能陶瓷的方法 | |
CN113200567A (zh) | 一种高烧结活性氧化锆粉体及其制备方法 | |
CN109592982A (zh) | 一种碳化硼核中子吸收材料及制备方法 | |
CN111233468B (zh) | 结构件用钇稳定锆粉的制备方法 | |
CN113105252A (zh) | 一种制备氮化硅陶瓷的烧结助剂及其应用、氮化硅陶瓷的制备方法 | |
CN104909725A (zh) | 一种无指甲纹缺陷的氧化铝瓷球制备方法 | |
CN114014652A (zh) | 低温烧结氧化锆陶瓷及其制备工艺 | |
CN110078120A (zh) | 一种基于超临界分散焙烧的氧化钇稳定氧化锆粉体的制备方法 | |
CN109336590B (zh) | 氧化镁部分稳定氧化锆、氧化镁部分稳定氧化锆陶瓷及其制备方法和应用 | |
CN112174662A (zh) | 一种滴定法制备锆铝复合球的方法 | |
CN103482981A (zh) | 一种多孔氮化硅陶瓷材料的制备方法 | |
CN111718186B (zh) | 颗粒尺寸可调的zta陶瓷微珠的制备方法 | |
CN113800909A (zh) | 一种高熵稀土钽酸盐空心球粉体及制备方法 | |
CN103060762A (zh) | 钼铌合金靶材的生产工艺 | |
CN103664167B (zh) | 一种片状AlON/四方相ZrO2复合材料的制备方法 |
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 | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220208 |