CN109465464A - 一种制备氧化铝基金属陶瓷纳米复合粉末的方法 - Google Patents
一种制备氧化铝基金属陶瓷纳米复合粉末的方法 Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 93
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 66
- 239000002184 metal Substances 0.000 title claims abstract description 66
- 239000000919 ceramic Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 41
- 239000002243 precursor Substances 0.000 claims abstract description 39
- 238000010438 heat treatment Methods 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 14
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- 239000008103 glucose Substances 0.000 claims abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 7
- 239000010941 cobalt Substances 0.000 claims abstract description 4
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- 239000008139 complexing agent Substances 0.000 claims abstract description 3
- 239000002270 dispersing agent Substances 0.000 claims abstract description 3
- 239000000446 fuel Substances 0.000 claims abstract description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000011159 matrix material Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910003158 γ-Al2O3 Inorganic materials 0.000 claims description 3
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 description 21
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 13
- 238000000498 ball milling Methods 0.000 description 13
- 229910052593 corundum Inorganic materials 0.000 description 12
- 230000008569 process Effects 0.000 description 12
- 229910001845 yogo sapphire Inorganic materials 0.000 description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 238000005551 mechanical alloying Methods 0.000 description 7
- 239000004411 aluminium Substances 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000006479 redox reaction Methods 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
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- 239000007769 metal material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 229910001868 water Inorganic materials 0.000 description 2
- BMTAFVWTTFSTOG-UHFFFAOYSA-N Butylate Chemical group CCSC(=O)N(CC(C)C)CC(C)C BMTAFVWTTFSTOG-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 229910017709 Ni Co Inorganic materials 0.000 description 1
- 229910003267 Ni-Co Inorganic materials 0.000 description 1
- 229910003262 Ni‐Co Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- KGWWEXORQXHJJQ-UHFFFAOYSA-N [Fe].[Co].[Ni] Chemical compound [Fe].[Co].[Ni] KGWWEXORQXHJJQ-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000713 high-energy ball milling Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000009700 powder processing Methods 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000010415 tropism Effects 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B22F1/0003—
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- 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
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Abstract
本发明提供一种制备氧化铝基金属陶瓷纳米复合粉末的方法，包括如下步骤，a、前驱体粉末的制备：原料中氧化铝源和金属源的用量为使得最终制备得到的氧化铝基金属陶瓷纳米复合粉末中的包括铁、钴和镍中一种或两种的金属占复合粉末的质量百分含量为3～20％，尿素为反应燃料，葡萄糖为络合剂和分散剂，反应制备得到所述前驱体粉末；b、复合粉末产品的制备：将得到的前驱体粉末进行高温双步热处理，具体包括前驱体粉末先在空气中然后在还原气氛中各于600‑1000℃下保温处理0.5～3小时，得到所述产品。本发明为制备具有纳米金属弥散相‑纳米晶结构的氧化铝基金属陶瓷粉末提供了新的思路，具有生产周期短、成本低、操作方便等优点。
Description
技术领域
本发明属于陶瓷基复合材料研究领域，特别提供了一种制备氧化铝基金属陶瓷纳米复合粉末的方法。
背景技术
氧化铝基金属陶瓷材料是近年来受到国内外广泛关注与研究的一种新型材料。这种材料一般使用超细纳米金属相(Ni、Ni-Co、Fe-Ni等，尺寸低于500nm)均匀弥散分布到氧化铝陶瓷基体中，使其在保有氧化铝材料的高强度、高硬度、耐磨损、耐高温和化学稳定性高等优点同时，又因为加入金属弥散相能获得较好韧性，是一种非常重要的工具材料和结构材料。
氧化铝陶瓷基纳米复合材料中，金属弥散相的尺寸与分布是决定其力学性能的关键因素。首先，纳米金属弥散相的引入不仅可以抑制基体晶粒异常长大，使基体材料微观结构均匀化，使材料韧性提升；其次，部分金属弥散相可能包裹在氧化物基体的内部，形成了丰富的金属/氧化物界面，从而弱化了晶界的作用，使裂纹通过氧化物基体的晶界扩展的倾向性降低，使沿晶断裂转化为穿晶断裂，材料的韧性得到提升。最后，金属弥散相的均匀分布可以抑制晶界迁移而细化晶粒，精细化的微观组织能同时提高材料的强度和韧性。故对于氧化铝基金属陶瓷材料，金属弥散相分布越均匀，尺寸越细小，金属弥散强化氧化铝基纳米复合材料的力学性能越高。
氧化铝基金属陶瓷纳米复合材料主要采用粉末冶金的方法制造，成功制备高性能氧化铝基金属陶瓷纳米复合材料的关键是制得弥散相分布均匀的高质量氧化铝基金属陶瓷纳米复合粉末。现有制备氧化铝基金属陶瓷纳米复合粉末的方法主要是机械合金化法、反应球磨法和溶胶凝胶法等。
机械合金化法主要是将作为原料的Al2O3粉末(基体)和金属元素粉末(金属源)混合装罐在一定球料比和气氛保护的条件下进行高能球磨。在球磨的过程中，原料粉末承受冲击、剪切、摩擦、压缩等多种力的作用，经历扁平化、冷焊合、合金成分均匀化等过程，实现金属粉末颗粒合金化并在氧化物基体均匀弥散分布。机械合金化过程能够成功制备氧化铝基纳米复合材料，但是有其显著的缺点：首先，由于机械合金化过程中作为球磨介质的球和粉末原料剧烈碰撞，作为介质的磨球和罐体极易在机械合金化的过程中磨损而混入粉末原料中，最终粉末原料中引入杂质；其次，机械合金化过程中的高速碰撞容易使金属弥散相聚合长大，影响最终得到的块体材料性能；最后，机械合金化是一个高耗能、效率较低的过程，不利于粉末的大规模生产。
反应球磨法是机械合金化法的改良方法，Tohru Sekino等人(Journal of theAmerican Ceramic Society，1997，80(5):1139–1148)使用Al2O3粉末和硝酸盐(金属源)溶液为原料进行湿混球磨，使得氧化铝粉和硝酸盐混合均匀。球磨一定时间以后将得到的混合物在450℃左右加热使硝酸盐分解得到金属氧化物和Al2O3的混合粉末，最后将混合还原得到金属弥散强化氧化铝基纳米复合粉末。虽然反应球磨法工艺较复杂，但现有的研究成果显示，与机械合金化法相比，反应球磨法过程中作为弥散相的金属在基体颗粒上原位生成，可以将金属弥散相的尺寸从300nm降低至100nm以下，从而较大幅度的提升氧化铝基金属陶瓷纳米复合材料的力学性能。不可忽视的是，反应球磨法与机械合金化法有类似的缺点：粉末易被掺杂污染和批量化生产成本过高。具体地，因球磨中高速旋转的球和球磨罐都会磨损，球磨1000g时氧化铝陶瓷基纳米复合材料产品一般增重20g以上，这就无疑会给产品带来2％的杂质。且球磨时间长，能耗大，因而批量化生产成本过高。
溶胶-凝胶法的基本原理是将易于水解的金属化合物(无机盐或金属醇盐)在某种溶剂中与水或者其他物质发生反应，经水解与缩聚过程逐渐凝胶化，再经过煅烧和还原得到所需的材料。如E.D.Rodeghiero等人(Materials Science and Engineering A，1995，195：151-161)将异丙醇铝(Al(C3H7O)3)溶于乙醇，加热至沸腾后加入二水甲酸镍(Ni(CHO2)2·2H2O)的水溶液，接着将混合溶液在60℃以上超声处理30分钟得到溶胶，将溶胶倒入开放容器在室温下一段时间得到凝胶，将凝胶在100℃以下干燥研磨过筛得到前驱体粉末，最后将前驱体粉末在氢气气氛中1000℃保温得到目标金属陶瓷粉末。E.BREVAL等人(Journal of Materials Science，1992，27：1464-1468)将仲丁醇铝溶于异丙醇中形成溶液，将溶液搅拌15分钟后加入HNO3把pH值调整到2。在80℃搅拌1小时后加入硝酸镍(Ni(NO3)2·6H2O)形成溶胶，溶胶经过干燥若干时间以后形成凝胶。再将得到的凝胶在空气气氛中500℃煅烧得到前驱体粉末，最后将前驱体粉末在氢气气氛中1000℃保温4小时得到目标金属陶瓷粉末。由前面描述可知，溶胶-凝胶法制备过程复杂，且制备得到目标粉末中的弥散相金属粒径较大。因此，需要开发新的金属弥散强化氧化铝陶瓷基纳米复合粉末的制备工艺。
发明内容
本发明的目的在于提供一种制备氧化铝基金属陶瓷纳米复合粉末的方法，旨在开发一种高效、节能的方法制备具有超细金属弥散相的氧化铝基金属陶瓷纳米复合粉末。超细金属弥散相强化氧化铝陶瓷基纳米复合粉末的可设计性强、金属弥散相特别细小(5-20nm)。
本发明首先采用溶液燃烧合成法制备纳米复合氧化物前驱体粉末，接着将氧化物前驱体粉末在空气焙烧和在氢气中进行选择还原得到氧化铝基金属陶瓷纳米复合粉末。
因此，本发明提供一种制备氧化铝基金属陶瓷纳米复合粉末的方法，所述方法包括如下步骤，a、前驱体粉末的制备：原料中氧化铝源为Al(NO3)3·9H2O，金属源为Fe(NO3)3·9H2O、Ni(NO3)2·6H2O和Co(NO3)2·6H2O中的一种或两种，所述氧化铝源和金属源的用量为使得最终制备得到的氧化铝基金属陶瓷纳米复合粉末中的包括铁、钴和镍中一种或两种的金属占复合粉末的质量百分含量为3～20％，尿素为反应燃料，葡萄糖为络合剂和分散剂，氧化铝源、金属源、尿素和葡萄糖溶解于去离子水中得到混合溶液，加热所述混合溶液反应制备得到所述前驱体粉末；b、复合粉末产品的制备：将得到的前驱体粉末进行高温双步热处理，具体包括前驱体粉末先在空气中600-1000℃下保温处理0.5～3小时，然后在还原气氛中600-1000℃下保温处理0.5～3小时，得到纳米尺度的金属均匀分布在γ-Al2O3陶瓷基体中的所述氧化铝基金属陶瓷纳米复合粉末。
在一种具体的实施方式中，产品中纳米尺度的金属的粒径为5～20nm。
在一种具体的实施方式中，步骤a中尿素与原料硝酸铝的摩尔比为0.9～1.2：1，葡萄糖与原料硝酸铝的摩尔比为0.2～0.5：1。
在一种具体的实施方式中，步骤a中前驱体粉末制备的反应温度为120～350℃，优选为200～300℃。
在一种具体的实施方式中，步骤b中的还原气氛为氢气气氛。
在一种具体的实施方式中，步骤a中，加热5～10min至溶液剧烈反应时停止加热，等待1～2分钟后，反应结束得到前驱体粉末。
在一种具体的实施方式中，步骤b中，前驱体粉末先在空气中700-900℃下保温处理1～2小时，然后在还原气氛中700～900℃下保温处理1～2小时。
本发明还相应提供一种氧化铝基金属陶瓷纳米复合粉末，所述氧化铝基金属陶瓷纳米复合粉末为如上任意一种所述方法制备得到的。
本发明的优点和有益效果：
1、本发明中，无论是制备前驱体粉末的加热过程，还是高温双步热处理过程中都不需要搅拌，更不需涉及高能耗的球磨方式。反应设备使用加热后能及时排气的坩埚、烧杯、电热炉和马弗炉等常见设备即可。设备简单，操作方便。
2、本发明中的纳米复合粉末以氧化铝为基体，且具体是以晶型为γ型的γ-氧化铝为陶瓷基体，通过前驱体制备后的高温双步热处理得到，使得处理过程中无定形氧化铝悉数转化为γ-氧化铝。
3、本发明提供的氧化铝基金属陶瓷纳米复合粉末产品可用于代替“碳化钨和钴硬质合金”作为高硬度的耐磨材料。该产品结合了陶瓷材料的高硬度和金属材料的韧性，该产品例如在压片之后形成一种性能优异的硬质耐磨材料。
总的来说，本发明通过控制原料配比在液-液原子级混合的溶液中原位生成目标纳米复合粉末，为制备具有纳米金属弥散相-纳米晶结构的氧化铝基金属陶瓷粉末提供了新的思路，它具有生产周期短、成本低、操作方便等优点。超细金属颗粒不仅能细化氧化铝的晶粒，提高烧结活性，且能有效抑制其烧结过程中的晶粒长大，为获得高致密度、纳米金属弥散相分布均匀的超细晶氧化铝基金属陶瓷奠定了基础。
附图说明
图1为本发明的工艺流程图。
图2为氧化铝基金属陶瓷纳米复合粉末透射电子形貌图。
具体实施方式
本发明步骤a中前驱体粉末制备的反应温度为120～350℃，优选为200～300℃。步骤a中制备得到的前驱体粉末为氧化铁、氧化钴和氧化镍这三种氧化物中的任意一种或两种与氧化铝的混合物，前驱体制备过程中将原料混匀后加热到200～300℃，反应过程中可能会释放出氮气、二氧化碳和水蒸汽等气体。
本发明步骤b中的还原气氛例如为氢气气氛。本发明中，对前驱体的高温双步热处理包括空气热处理和氢气热处理两步，空气热处理中可能会将氧化铁、氧化钴和氧化镍焙烧为与氧化铝形成复合物，再在氢气下热处理，铁钴镍的氧化物将悉数还原为单质，而氧化铝不会被还原，但无定形氧化铝会转变成晶型的γ-氧化铝。若将前驱体粉末直接在氢气气氛中热处理，则无法形成γ-氧化铝基的金属陶瓷纳米复合粉末。
实施例1：10wt.％Ni-Al2O3纳米复合粉末的制备
称量0.0192molNi(NO3)2·6H2O、0.2molAl(NO3)3·9H2O、0.18mol尿素和0.05mol葡萄糖溶于去离子水中，在容器中搅拌均匀，得到混合溶液。混合溶液在可控温炉内搅拌加热，使水溶液蒸发。随着反应的进行，放出的热量使原料发生热解和剧烈的氧化还原反应，目标元素则转化为粒度极细的复合前驱体颗粒。对前驱体粉末进行双步热处理：第一步热处理为在空气中800℃保温时间为1小时，第二步热处理为在氢气中800℃保温1小时。最终得到10wt.％Ni-Al2O3纳米复合粉末。
本发明步骤a中，尿素与原料中硝酸铝的摩尔比在0.9～1.2之间，反应过程中生成大量气体可以防止前驱体粉末的团聚；葡萄糖的作用是络合反应体系中的金属离子、吸收部分反应产生的热量防止团聚，并加大气体产生量，产生分散粉末效果，进一步细化粉末，降低反应温度，葡萄糖与原料中硝酸铝的摩尔比在0.2～0.5之间。
本发明在步骤b高温双步热处理以后，前驱体粉末中Fe、Co、Ni的氧化物转化成金属或者固溶体合金，氧化铝在热处理以后发生晶化，由无定型Al2O3转化为γ-Al2O3，最终得到氧化铝基金属陶瓷纳米复合粉末。最终制得粉末的透射电镜形貌图(以Ni-Al2O3为例)如图2所示，5～10nm的超细Ni颗粒均匀分布在片状Al2O3粉末中。
实施例2：5wt.％(Ni50wt.％Co)-Al2O3纳米复合粉末的制备
称量0.0045molCo(NO3)2·6H2O、0.0045molNi(NO3)2·6H2O、0.2mol Al(NO3)3·9H2O、0.2mol尿素和0.06mol葡萄糖溶于去离子水中，在容器中搅拌均匀，得到混合溶液。混合溶液在可控温炉内搅拌加热，使水溶液蒸发。随着反应的进行，放出的热量使原料发生热解和剧烈的氧化还原反应，目标元素则转化为粒度极细的复合前驱体颗粒。对前驱体粉末进行双步热处理：第一步热处理为在空气中700℃保温时间为2小时，第二步热处理为在氢气中800℃保温1小时。最终得到5wt.％(Ni50wt.％Co)-Al2O3复合粉末。
实施例3：20wt.％(Fe50wt.％Ni)-Al2O3纳米复合粉末的制备
称量0.0228molFe(NO3)3·9H2O、0.0216molNi(NO3)2·6H2O、0.2mol Al(NO3)3·9H2O、0.22mol尿素和0.08mol葡萄糖溶于去离子水中，在容器中搅拌均匀，得到混合溶液。混合溶液在可控温炉内搅拌加热，使水溶液蒸发。随着反应的进行，放出的热量使原料发生热解和剧烈的氧化还原反应，目标元素则转化为粒度极细的复合前驱体颗粒。对前驱体粉末进行双步热处理：第一步热处理为在空气中900℃保温时间为2小时，第二步热处理为在氢气中900℃保温2小时。最终得到20wt.％(Fe50wt.％Ni)-Al2O3纳米复合粉末。
实施例4：15wt.％(Fe50wt.％Co)-Al2O3纳米复合粉末的制备
称量0.0161molFe(NO3)3·9H2O、0.0153molCo(NO3)2·6H2O、0.2mol Al(NO3)3·9H2O、0.24mol尿素和0.1mol葡萄糖溶于去离子水中，在容器中搅拌均匀，得到混合溶液。混合溶液在可控温炉内搅拌加热，使水溶液蒸发。随着反应的进行，放出的热量使原料发生热解和剧烈的氧化还原反应，目标元素则转化为粒度极细的复合前驱体颗粒。对前驱体粉末进行双步热处理：第一步热处理为在空气中850℃保温时间为2小时，第二步热处理为在氢气中850℃保温2小时。最终得到15wt.％(Fe50wt.％Co)-Al2O3复合粉末。
以上内容是结合具体的优选实施方式对本发明作的进一步详细说明，不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干简单推演和替换，都应当视为属于本发明的保护范围。
Claims (8)
1.一种制备氧化铝基金属陶瓷纳米复合粉末的方法，其特征在于，所述方法包括如下步骤，
a、前驱体粉末的制备：原料中氧化铝源为Al(NO3)3·9H2O，金属源为Fe(NO3)3·9H2O、Ni(NO3)2·6H2O和Co(NO3)2·6H2O中的一种或两种，所述氧化铝源和金属源的用量为使得最终制备得到的氧化铝基金属陶瓷纳米复合粉末中的包括铁、钴和镍中一种或两种的金属占复合粉末的质量百分含量为3～20％，尿素为反应燃料，葡萄糖为络合剂和分散剂，氧化铝源、金属源、尿素和葡萄糖溶解于去离子水中得到混合溶液，加热所述混合溶液反应制备得到所述前驱体粉末；
b、复合粉末产品的制备：将得到的前驱体粉末进行高温双步热处理，具体包括前驱体粉末先在空气中600-1000℃下保温处理0.5～3小时，然后在还原气氛中600-1000℃下保温处理0.5～3小时，得到纳米尺度的金属均匀分布在γ-Al2O3陶瓷基体中的所述氧化铝基金属陶瓷纳米复合粉末。
2.根据权利要求1所述的方法，其特征在于，产品中纳米尺度的金属的粒径为5～20nm。
3.根据权利要求1所述的方法，其特征在于，步骤a中尿素与原料硝酸铝的摩尔比为0.9～1.2：1，葡萄糖与原料硝酸铝的摩尔比为0.2～0.5：1。
4.根据权利要求1所述的方法，其特征在于，步骤a中前驱体粉末制备的反应温度为120～350℃，优选为200～300℃。
5.根据权利要求1所述的方法，其特征在于，步骤b中的还原气氛为氢气气氛。
6.根据权利要求1所述的方法，其特征在于，步骤a中，加热5～10min至溶液剧烈反应时停止加热，等待1～2分钟后，反应结束得到前驱体粉末。
7.根据权利要求1～6中任意一项所述的方法，其特征在于，步骤b中，前驱体粉末先在空气中700～900℃下保温处理1～2小时，然后在还原气氛中700～900℃下保温处理1～2小时。
8.一种氧化铝基金属陶瓷纳米复合粉末，其特征在于，所述氧化铝基金属陶瓷纳米复合粉末为如权利要求1～7中任意一项所述方法制备得到的。
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