CN114524673A - 一种高体积密度的氧化锆耐火材料的制备工艺 - Google Patents
一种高体积密度的氧化锆耐火材料的制备工艺 Download PDFInfo
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 307
- 239000011819 refractory material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 119
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 238000005469 granulation Methods 0.000 claims abstract description 37
- 230000003179 granulation Effects 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 238000002844 melting Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 24
- 230000008018 melting Effects 0.000 claims abstract description 24
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 20
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910002076 stabilized zirconia Inorganic materials 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000003825 pressing Methods 0.000 claims abstract description 14
- 229910021532 Calcite Inorganic materials 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000007664 blowing Methods 0.000 claims description 20
- 238000007873 sieving Methods 0.000 claims description 17
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 claims description 17
- 239000002002 slurry Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 239000011812 mixed powder Substances 0.000 claims description 15
- 239000003381 stabilizer Substances 0.000 claims description 15
- 229910052726 zirconium Inorganic materials 0.000 claims description 15
- 239000007921 spray Substances 0.000 claims description 14
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 13
- 229910052593 corundum Inorganic materials 0.000 claims description 12
- 238000011049 filling Methods 0.000 claims description 12
- 238000003723 Smelting Methods 0.000 claims description 11
- 239000002270 dispersing agent Substances 0.000 claims description 11
- 238000010891 electric arc Methods 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 10
- 239000010431 corundum Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000007670 refining Methods 0.000 claims description 6
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 5
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 5
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 5
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 5
- 238000001238 wet grinding Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- NWBJYWHLCVSVIJ-UHFFFAOYSA-N N-benzyladenine Chemical compound N=1C=NC=2NC=NC=2C=1NCC1=CC=CC=C1 NWBJYWHLCVSVIJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 3
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 18
- 230000007547 defect Effects 0.000 abstract description 7
- 238000013461 design Methods 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000009413 insulation Methods 0.000 description 5
- 239000000155 melt Substances 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 3
- 238000009991 scouring Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- -1 zirconium ions Chemical class 0.000 description 2
- 238000005452 bending Methods 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
一种高体积密度的氧化锆耐火材料的制备工艺,包括如下步骤:(1)电熔氧化锆粉体的制备;(2)钇稳氧化锆造粒粉的制备;(3)混料:将上述电熔氧化锆粉体、钇稳氧化锆造粒粉与SiC、纳米η‑Al2O3加入到高速混炼机中混合搅拌均匀;(4)压制成坯:经冷等静压机在120‑150Mpa的压力条件下压制成生坯;(5)烧结成型。本发明所述的高体积密度的氧化锆耐火材料的制备工艺,工艺步骤设计合理,通过高纯方解石、热处理完善电熔氧化锆粉体晶格发育和改善颗粒表面性能、消除缺陷,以电熔氧化锆粉体、钇稳氧化锆造粒粉为主,添加SiC、纳米η‑Al2O3,结合了电熔氧化锆粉体、钇稳氧化锆造粒粉的优点,耐火性能优良,具有更高的体积密度、更小的显气孔率,制备方法简单。
Description
技术领域
本发明属于氧化锆制品技术领域,具体涉及一种高体积密度的氧化锆耐火材料的制备工艺。
背景技术
二氧化锆熔点高达2715℃,以其为主要原料制备的氧化锆耐火材料具有高温下化学性质稳定、使用温度超高(可达2400℃以上)、氧化或还原气氛下均可使用等诸多优点,是目前可工业化生产和应用的最为成熟的超高温领域用耐火材料。
目前,氧化锆耐火材料按照隔热性能基本可分为3大类:(1)氧化锆纤维制品;(2)高纯氧化锆空心球隔热制品;(3)重质氧化锆制品。其中,氧化锆重质制品所使用的颗粒料主要物质是氧化锆电熔颗,该类氧化锆电熔颗粒是通过电熔氧化锆熔液冷却后破碎制得,氧化锆重质制品具有结构强度高、抗渗透、抗冲刷、使用温度更高,缺点是热导率偏高、隔热效果略差,主要用于2000℃以上高温反应衬。
此外,电熔氧化锆粉体容易在冷却的过程中出现结晶缺陷,比如晶格中的空位、晶面位错、玻璃态等,这造成了电熔氧化锆粉体性能不稳定,同时机械破碎氧化锆耐火制品工艺会导致氧化锆颗粒的表面粗糙,颗粒形状不规则、且颗粒尺寸分布不均匀,在成型过程中不易于制备高密度坯体,从而在烧结时影响其致密化过程,体积密度下降。因此,需要研发出一种高体积密度的氧化锆耐火材料的制备工艺,以来解决上述技术问题。
中国专利申请号为CN201911386761.4公开一种基于氧化锆的耐火材料及其制备方法,包括氧化锆、氧化硅、氧化铝、稳定剂、结合剂等原料,主要通过混料、成坯、烧结成型三步法制备成型,没有氧化锆耐火材料的体积密度、显气孔率进行进一步的改进。
发明内容
发明目的:为了克服以上不足,本发明的目的是提供一种高体积密度的氧化锆耐火材料的制备工艺,工艺步骤设计合理,通过高纯方解石、热处理完善电熔氧化锆粉体晶格发育和改善颗粒表面性能、消除缺陷,以电熔氧化锆粉体、钇稳氧化锆造粒粉为主,添加SiC、纳米η-Al2O3,结合了电熔氧化锆粉体、钇稳氧化锆造粒粉的优点,耐火性能优良,具有更高的体积密度、更小的显气孔率,制备方法简单,前景广泛。
本发明的目的是通过以下技术方案实现的:
一种高体积密度的氧化锆耐火材料的制备工艺,包括如下步骤:
(1)电熔氧化锆粉体的制备:将电熔单斜锆、稳定剂高纯方解石通过搅拌机混合均匀,得到混合粉;将上述混合粉放入三相电弧炉进行熔炼,待混合粉在三相电弧炉完全熔融后,精炼0.5-1h,得到熔融体,将上述熔融体经熔融喷吹制得氧化锆空心球,收集喷吹好的氧化锆空心球进行研磨至325目,得到稳定氧化锆粉体;将上述氧化锆粉体置于刚玉坩埚中放入热处理炉中,热处理炉以8-10℃/min升温至1100-1200℃,保温3-5h,关闭热处理炉,随炉冷却后取出粉体,将粉体在行星球磨机中以400-500r/min的速率进行湿磨5-6h,过325目筛,烘干后得到电熔氧化锆粉体;
(2)钇稳氧化锆造粒粉的制备:将氧化钇稳定氧化锆粉末、去离子水、分散剂在行星球磨机中以300-400r/min的速率进行球墨制成浆料,向上述浆料加入粘结剂,通过搅拌机搅拌4-6h,然后采用喷雾造粒机喷雾造粒,过325目筛,得到钇稳氧化锆造粒粉;
(3)混料:将上述电熔氧化锆粉体、钇稳氧化锆造粒粉与SiC、纳米η-Al2O3加入到高速混炼机中混合搅拌均匀,过325目筛;
(4)压制成坯:采用控制体积填料法向模具中填料,经冷等静压机在120-150Mpa的压力条件下压制成生坯;
(5)烧结成型:将成型好的生坯在恒温烘箱中,在100-120℃烘干8-12h,然后将生坯置于升降炉中,以8-10℃/min升温至的速率升温至1500-1600℃,并且保温4-6h,然后关闭升降炉,样品随炉冷却,得到氧化锆耐火材料。
本发明所述的高体积密度的氧化锆耐火材料的制备工艺,工艺步骤设计合理,采用熔融喷吹工艺制备的电熔氧化锆粉体经历了由高温熔体向固态氧化锆空心球的急冷过程,因而其晶粒长大的过程受到抑制,所得粉体的晶粒较小,所述电熔氧化锆粉体的组成有两部分,一部分是由高纯方解石的钙离子取代锆离子形成置换固溶体,通过引入氧空位来降低四方相氧化锆晶格内部的库伦斥力,提高其稳定性,并将四方相保存至室温状态,另一部分是无离子掺杂的纯氧化锆晶格,由于其晶粒尺寸小于相变临界尺寸,可在室温保持亚稳四方相。
本发明通过热处理除去亚稳四方相,热处理可以完善晶格发育和改善颗粒表面性能,消除缺陷,使电熔氧化锆粉体颗粒形状更规则、且颗粒尺寸更分布均匀,在成型过程中有利于制备高密度坯体,解决了现有技术中电熔氧化锆粉体在后续热处理中发生体积膨胀效应导致的烧结过程中开裂的问题,提高了体积密度。
通过氧化钇稳定氧化锆粉末、去离子水、分散剂、粘结剂制浆然后经喷雾造粒机喷雾造粒,得到烧结活性高的钇稳氧化锆造粒粉。
所述氧化锆耐火材料以电熔氧化锆粉体、钇稳氧化锆造粒粉为主,结合电熔氧化锆粉体强度高、抗渗透、抗冲刷、使用温度高和钇稳氧化锆造粒粉烧结活性高、高温烧成过程发生自身烧结收缩、在制品内部形成大量闭口缩孔或闭口微型气孔、热导率低,隔热效果好的优点,通过添加SiC、纳米η-Al2O3,以SiC氧化后的SiO2为硅源、纳米η-Al2O3为铝源形成莫来石晶体,均匀分布于氧化锆耐火材料中,有利于氧化锆耐火材料具有更高的体积密度、更小的显气孔率,由于钇稳氧化锆造粒粉内含有粘结剂,因此在混料时不再外加结合剂。
进一步的,上述的高体积密度的氧化锆耐火材料的制备工艺,所述步骤(1)中,所述电熔单斜锆、稳定剂高纯方解石均为325目,所述稳定剂为高纯方解石;所述熔融喷吹采用压缩空气喷吹并且压力为8-10公斤。
进一步的,上述的高体积密度的氧化锆耐火材料的制备工艺,所述步骤(1)中,所述电熔单斜锆、稳定剂的质量比为96-97:3-4。
进一步的,上述的高体积密度的氧化锆耐火材料的制备工艺,所述步骤(2)中,所述氧化钇稳定氧化锆粉末中包括质量比为94.74:5.23:0.035:0.0022的氧化锆、氧化钇、三氧化二铁、氧化钛;所述分散剂为聚丙烯酸铵、聚丙烯酸钠、柠檬酸铵、DS005、CE-64和丙三醇中的一种或者多种的混合;所述粘结剂为聚乙烯醇、聚乙二醇、羧甲基纤维素钠、B-1000和B-1022中的一种或者多种的混合。
进一步的,上述的高体积密度的氧化锆耐火材料的制备工艺,所述步骤(2)中,所述氧化钇稳定氧化锆粉末、去离子水、分散剂、粘结剂的质量比为100-110:120-130:0.2-0.3:1.5-2.5。
进一步的,上述的高体积密度的氧化锆耐火材料的制备工艺,所述步骤(3)中,所述电熔氧化锆粉体、钇稳氧化锆造粒粉、SiC、纳米η-Al2O3的质量比为20-30:50-60:5-10:2-5。
进一步的,上述的高体积密度的氧化锆耐火材料的制备工艺,所述SiC采用1500#SiC,粒径为10μm;所述纳米η-Al2O3的纯度为99.5%,粒径为20nm。
与现有技术相比,本发明具有如下的有益效果:
(1)本发明所述的高体积密度的氧化锆耐火材料的制备工艺,工艺步骤设计合理,采用熔融喷吹工艺制备的电熔氧化锆粉体经历了由高温熔体向固态氧化锆空心球的急冷过程,因而其晶粒长大的过程受到抑制,所得粉体的晶粒较小,所述电熔氧化锆粉体的组成有两部分,一部分是由高纯方解石的钙离子取代锆离子形成置换固溶体,通过引入氧空位来降低四方相氧化锆晶格内部的库伦斥力,提高其稳定性,并将四方相保存至室温状态,另一部分是无离子掺杂的纯氧化锆晶格,由于其晶粒尺寸小于相变临界尺寸,可在室温保持亚稳四方相;
(2)本发明所述的高体积密度的氧化锆耐火材料的制备工艺,通过热处理除去亚稳四方相,热处理可以完善晶格发育和改善颗粒表面性能,消除缺陷,使电熔氧化锆粉体颗粒形状更规则、且颗粒尺寸更分布均匀,在成型过程中有利于制备高密度坯体,解决了现有技术中电熔氧化锆粉体在后续热处理中发生体积膨胀效应导致的烧结过程中开裂的问题,提高了体积密度;
(3)本发明所述的高体积密度的氧化锆耐火材料的制备工艺,以电熔氧化锆粉体、钇稳氧化锆造粒粉为主,结合电熔氧化锆粉体强度高、抗渗透、抗冲刷、使用温度高和钇稳氧化锆造粒粉烧结活性高、高温烧成过程发生自身烧结收缩、在制品内部形成大量闭口缩孔或闭口微型气孔、热导率低,隔热效果好的优点,通过添加SiC、纳米η-Al2O3,以SiC氧化后的SiO2为硅源、纳米η-Al2O3为铝源形成莫来石晶体,均匀分布于氧化锆耐火材料中,有利于氧化锆耐火材料具有更高的体积密度、更小的显气孔率。
具体实施方式
下面将实施例结合具体实验数据,对本发明实施例中的技术方案进行清楚、完整的描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通的技术人员在没有做出创造性劳动的前提下所获得的所有其它实施例,都属于本发明的保护范围。
以下实施例1、实施例2、实施例3、对比例1提供了一种高体积密度的氧化锆耐火材料的制备工艺。
其中,所述电熔单斜锆、稳定剂高纯方解石均为325目;所述氧化钇稳定氧化锆粉末中包括质量比为94.74:5.23:0.035:0.0022的氧化锆、氧化钇、三氧化二铁、氧化钛;所述分散剂为聚丙烯酸铵、聚丙烯酸钠、柠檬酸铵、DS005、CE-64和丙三醇中的一种或者多种的混合;所述粘结剂为聚乙烯醇、聚乙二醇、羧甲基纤维素钠、B-1000和B-1022中的一种或者多种的混合;所述SiC采用1500#SiC,粒径为10μm;所述纳米η-Al2O3的纯度为99.5%,粒径为20nm。
实施例1
高体积密度的氧化锆耐火材料的制备工艺,包括如下步骤:
(1)电熔氧化锆粉体的制备:电熔单斜锆、稳定剂的质量比为96.5:3.5,将电熔单斜锆、稳定剂高纯方解石通过搅拌机混合均匀,得到混合粉;将上述混合粉放入三相电弧炉进行熔炼,待混合粉在三相电弧炉完全熔融后,精炼1h,得到熔融体,将上述熔融体经熔融喷吹制得氧化锆空心球,所述熔融喷吹采用压缩空气喷吹并且压力为8公斤,收集喷吹好的氧化锆空心球进行研磨至325目,得到稳定氧化锆粉体;将上述氧化锆粉体置于刚玉坩埚中放入热处理炉中,热处理炉以10℃/min升温至1150℃,保温4h,关闭热处理炉,随炉冷却后取出粉体,将粉体在行星球磨机中以450r/min的速率进行湿磨6h,过325目筛,烘干后得到电熔氧化锆粉体;
(2)钇稳氧化锆造粒粉的制备:所述氧化钇稳定氧化锆粉末、去离子水、CE-64、10wt%PVA溶液的质量比为100:125:0.22:1.8,将氧化钇稳定氧化锆粉末、去离子水、CE-64在行星球磨机中以300r/min的速率进行球墨制成浆料,向上述浆料加入10wt%PVA溶液,通过搅拌机搅拌5h,然后采用喷雾造粒机喷雾造粒,过325目筛,得到钇稳氧化锆造粒粉;
(3)混料:所述电熔氧化锆粉体、钇稳氧化锆造粒粉、SiC、纳米η-Al2O3的质量比为30:50:10:5,将上述电熔氧化锆粉体、钇稳氧化锆造粒粉与SiC、纳米η-Al2O3加入到高速混炼机中混合搅拌均匀,过325目筛;
(4)压制成坯:采用控制体积填料法向模具中填料,经冷等静压机在130Mpa的压力条件下压制成生坯;
(5)烧结成型:将成型好的生坯在恒温烘箱中,在110℃烘干12h,然后将生坯置于升降炉中,以10℃/min升温至的速率升温至1550℃,并且保温5h,然后关闭升降炉,样品随炉冷却,得到氧化锆耐火材料。
实施例2
高体积密度的氧化锆耐火材料的制备工艺,包括如下步骤:
(1)电熔氧化锆粉体的制备:电熔单斜锆、稳定剂的质量比为97:3,将电熔单斜锆、稳定剂高纯方解石通过搅拌机混合均匀,得到混合粉;将上述混合粉放入三相电弧炉进行熔炼,待混合粉在三相电弧炉完全熔融后,精炼45min,得到熔融体,将上述熔融体经熔融喷吹制得氧化锆空心球,所述熔融喷吹采用压缩空气喷吹并且压力为10公斤,收集喷吹好的氧化锆空心球进行研磨至325目,得到稳定氧化锆粉体;将上述氧化锆粉体置于刚玉坩埚中放入热处理炉中,热处理炉以9℃/min升温至1200℃,保温3.5h,关闭热处理炉,随炉冷却后取出粉体,将粉体在行星球磨机中以400r/min的速率进行湿磨5h,过325目筛,烘干后得到电熔氧化锆粉体;
(2)钇稳氧化锆造粒粉的制备:所述氧化钇稳定氧化锆粉末、去离子水、分散剂(聚丙烯酸钠和DS005的混合物,聚丙烯酸钠和DS005的质量比为3:2)、10wt%羧甲基纤维素钠溶液的质量比为100:130:0.3:1.6,将氧化钇稳定氧化锆粉末、去离子水、分散剂在行星球磨机中以300-400r/min的速率进行球墨制成浆料,向上述浆料加入10wt%羧甲基纤维素钠溶液,通过搅拌机搅拌6h,然后采用喷雾造粒机喷雾造粒,过325目筛,得到钇稳氧化锆造粒粉;
(3)混料:所述电熔氧化锆粉体、钇稳氧化锆造粒粉、SiC、纳米η-Al2O3的质量比为30:55:6:4,将上述电熔氧化锆粉体、钇稳氧化锆造粒粉与SiC、纳米η-Al2O3加入到高速混炼机中混合搅拌均匀,过325目筛;
(4)压制成坯:采用控制体积填料法向模具中填料,经冷等静压机在120Mpa的压力条件下压制成生坯;
(5)烧结成型:将成型好的生坯在恒温烘箱中,在120℃烘干12h,然后将生坯置于升降炉中,以8℃/min升温至的速率升温至1580℃,并且保温5h,然后关闭升降炉,样品随炉冷却,得到氧化锆耐火材料。
实施例3
高体积密度的氧化锆耐火材料的制备工艺,包括如下步骤:
(1)电熔氧化锆粉体的制备:电熔单斜锆、稳定剂的质量比为96.2:3.8,将电熔单斜锆、稳定剂高纯方解石通过搅拌机混合均匀,得到混合粉;将上述混合粉放入三相电弧炉进行熔炼,待混合粉在三相电弧炉完全熔融后,精炼1h,得到熔融体,将上述熔融体经熔融喷吹制得氧化锆空心球,所述熔融喷吹采用压缩空气喷吹并且压力为9公斤,收集喷吹好的氧化锆空心球进行研磨至325目,得到稳定氧化锆粉体;将上述氧化锆粉体置于刚玉坩埚中放入热处理炉中,热处理炉以9℃/min升温至1180℃,保温4h,关闭热处理炉,随炉冷却后取出粉体,将粉体在行星球磨机中以450r/min的速率进行湿磨6h,过325目筛,烘干后得到电熔氧化锆粉体;
(2)钇稳氧化锆造粒粉的制备:所述氧化钇稳定氧化锆粉末、去离子水、分散剂(聚丙烯酸钠和DS005的混合物,聚丙烯酸钠和DS005的质量比为1:1)、10wt%PVA溶液的质量比为100:125:0.25:2,将氧化钇稳定氧化锆粉末、去离子水、分散剂在行星球磨机中以400r/min的速率进行球墨制成浆料,向上述浆料加入10wt%PVA溶液,通过搅拌机搅拌5h,然后采用喷雾造粒机喷雾造粒,过325目筛,得到钇稳氧化锆造粒粉;
(3)混料:所述电熔氧化锆粉体、钇稳氧化锆造粒粉、SiC、纳米η-Al2O3的质量比为30:50:6:3,将上述电熔氧化锆粉体、钇稳氧化锆造粒粉与SiC、纳米η-Al2O3加入到高速混炼机中混合搅拌均匀,过325目筛;
(4)压制成坯:采用控制体积填料法向模具中填料,经冷等静压机在120Mpa的压力条件下压制成生坯;
(5)烧结成型:将成型好的生坯在恒温烘箱中,在110℃烘干12h,然后将生坯置于升降炉中,以8℃/min升温至的速率升温至1590℃,并且保温5h,然后关闭升降炉,样品随炉冷却,得到氧化锆耐火材料。
对比例1
氧化锆耐火材料的制备工艺,包括如下步骤:
(1)电熔氧化锆粉体的制备:将电熔单斜锆放入三相电弧炉进行熔炼,待完全熔融后,精炼1h,得到熔融体,将上述熔融体经熔融喷吹制得氧化锆空心球,所述熔融喷吹采用压缩空气喷吹并且压力为9公斤,收集喷吹好的氧化锆空心球进行研磨至325目,得到电熔氧化锆粉体;
(2)钇稳氧化锆造粒粉的制备:所述氧化钇稳定氧化锆粉末、去离子水、分散剂(聚丙烯酸钠和DS005的混合物,聚丙烯酸钠和DS005的质量比为1:1)、10wt%PVA溶液的质量比为100:125:0.25:2,将氧化钇稳定氧化锆粉末、去离子水、分散剂在行星球磨机中以400r/min的速率进行球墨制成浆料,向上述浆料加入10wt%PVA溶液,通过搅拌机搅拌5h,然后采用喷雾造粒机喷雾造粒,过325目筛,得到钇稳氧化锆造粒粉;
(3)混料:所述电熔氧化锆粉体、钇稳氧化锆造粒粉的质量比为3:5,将上述电熔氧化锆粉体、钇稳氧化锆造粒粉加入到高速混炼机中混合搅拌均匀,过325目筛;
(4)压制成坯:采用控制体积填料法向模具中填料,经冷等静压机在120Mpa的压力条件下压制成生坯;
(5)烧结成型:将成型好的生坯在恒温烘箱中,在110℃烘干12h,然后将生坯置于升降炉中,以8℃/min升温至的速率升温至1590℃,并且保温5h,然后关闭升降炉,样品随炉冷却,得到氧化锆耐火材料。
效果验证:
将上述实施例1、实施例2、实施例3、对比例1得到的氧化锆耐火材料分别制备成试样1、试样2、试样3、试样4,对试样1、试样2、试样3、试样4进行性能检测。
1、体积密度、显气孔率:按GB/T2997-2015标准计算。具体如下:(1)试样在空气中的质量测定:将待测试样1-4分别置于干燥箱中110℃保温24h进行烘干处理后,将试样1-4表面的细颗粒去除,测每个试样的质量(m1)。之后将试样1-4置于真空装置中,在内压<0.08MPa时,衡压保持5min,然后注入浸渍液没过试样1-4为止,并继续衡压保持30min,使试样1-4充分饱和;(2)饱和试样表观质量测定:试样1-4浸泡30min后将其放进带溢流嘴的容器中,待示数稳定后称量试样1-4的悬浮质量(m2);(3)饱和试样质量测定:将试样1-4从浸渍液中取出,用饱和湿毛巾擦去试样1-4表面液滴,然后测定饱和试样1-4在空气中的质量(m3)。测试数据见表1。
其计算公式为:
体积密度=m1×(在实验温度下浸渍液体的密度)/m3-m2
显气孔率=(m3-m1)/(m3-m2)×100%
2、常温抗折强度:按GB/T6569—2006标准测定,室温下待测试样1-4在三点弯曲装置上被加压而不折断时能承受的极限应力。本实验所使用的设备为显数电动抗折仪。跨距为4cm,加荷速度为0.5mm/min。测试数据见表1。
表1性能测试结果
本发明具体应用途径很多,以上所述仅是本发明的优选实施方式。应当指出,以上实施例仅用于说明本发明,而并不用于限制本发明的保护范围。对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进,这些改进也应视为本发明的保护范围。
Claims (7)
1.一种高体积密度的氧化锆耐火材料的制备工艺,其特征在于,包括如下步骤:
(1)电熔氧化锆粉体的制备:将电熔单斜锆、稳定剂高纯方解石通过搅拌机混合均匀,得到混合粉;将上述混合粉放入三相电弧炉进行熔炼,待混合粉在三相电弧炉完全熔融后,精炼0.5-1h,得到熔融体,将上述熔融体经熔融喷吹制得氧化锆空心球,收集喷吹好的氧化锆空心球进行研磨至325目,得到稳定氧化锆粉体;将上述氧化锆粉体置于刚玉坩埚中放入热处理炉中,热处理炉以8-10℃/min升温至1100-1200℃,保温3-5h,关闭热处理炉,随炉冷却后取出粉体,将粉体在行星球磨机中以400-500r/min的速率进行湿磨5-6h,过325目筛,烘干后得到电熔氧化锆粉体;
(2)钇稳氧化锆造粒粉的制备:将氧化钇稳定氧化锆粉末、去离子水、分散剂在行星球磨机中以300-400r/min的速率进行球墨制成浆料,向上述浆料加入粘结剂,通过搅拌机搅拌4-6h,然后采用喷雾造粒机喷雾造粒,过325目筛,得到钇稳氧化锆造粒粉;
(3)混料:将上述电熔氧化锆粉体、钇稳氧化锆造粒粉与SiC、纳米η-Al2O3加入到高速混炼机中混合搅拌均匀,过325目筛;
(4)压制成坯:采用控制体积填料法向模具中填料,经冷等静压机在120-150Mpa的压力条件下压制成生坯;
(5)烧结成型:将成型好的生坯在恒温烘箱中,在100-120℃烘干8-12h,然后将生坯置于升降炉中,以8-10℃/min升温至的速率升温至1500-1600℃,并且保温4-6h,然后关闭升降炉,样品随炉冷却,得到氧化锆耐火材料。
2.根据权利要求1所述的高体积密度的氧化锆耐火材料的制备工艺,其特征在于,所述步骤(1)中,所述电熔单斜锆、稳定剂高纯方解石均为325目;所述熔融喷吹采用压缩空气喷吹并且压力为8-10公斤。
3.根据权利要求1所述的高体积密度的氧化锆耐火材料的制备工艺,其特征在于,所述步骤(1)中,所述电熔单斜锆、稳定剂的质量比为96-97:3-4。
4.根据权利要求1所述的高体积密度的氧化锆耐火材料的制备工艺,其特征在于,所述步骤(2)中,所述氧化钇稳定氧化锆粉末中包括质量比为94.74:5.23:0.035:0.0022的氧化锆、氧化钇、三氧化二铁、氧化钛;所述分散剂为聚丙烯酸铵、聚丙烯酸钠、柠檬酸铵、DS005、CE-64和丙三醇中的一种或者多种的混合;所述粘结剂为聚乙烯醇、聚乙二醇、羧甲基纤维素钠、B-1000和B-1022中的一种或者多种的混合。
5.根据权利要求1所述的高体积密度的氧化锆耐火材料的制备工艺,其特征在于,所述步骤(2)中,所述氧化钇稳定氧化锆粉末、去离子水、分散剂、粘结剂的质量比为100-110:120-130:0.2-0.3:1.5-2.5。
6.根据权利要求1所述的高体积密度的氧化锆耐火材料的制备工艺,其特征在于,所述步骤(3)中,所述电熔氧化锆粉体、钇稳氧化锆造粒粉、SiC、纳米η-Al2O3的质量比为20-30:50-60:5-10:2-5。
7.根据权利要求1所述的高体积密度的氧化锆耐火材料的制备工艺,其特征在于,所述SiC采用1500#SiC,粒径为10μm;所述纳米η-Al2O3的纯度为99.5%,粒径为20nm。
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