CN106893954B - 一种Co基非晶合金粉末及其制备工艺 - Google Patents
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- 229910000808 amorphous metal alloy Inorganic materials 0.000 title claims abstract description 32
- 239000000843 powder Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 12
- 239000000654 additive Substances 0.000 claims abstract description 11
- 230000000996 additive effect Effects 0.000 claims abstract description 11
- 238000009713 electroplating Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 6
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 6
- 238000007747 plating Methods 0.000 claims abstract description 6
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000008139 complexing agent Substances 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 5
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 4
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 17
- 238000000576 coating method Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 238000005275 alloying Methods 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical group C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims description 3
- 229940081974 saccharin Drugs 0.000 claims description 3
- 235000019204 saccharin Nutrition 0.000 claims description 3
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 3
- 238000004448 titration Methods 0.000 claims description 3
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 150000001735 carboxylic acids Chemical class 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- 239000003792 electrolyte Substances 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical class O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- HIRWGWMTAVZIPF-UHFFFAOYSA-N nickel;sulfuric acid Chemical compound [Ni].OS(O)(=O)=O HIRWGWMTAVZIPF-UHFFFAOYSA-N 0.000 claims 1
- 239000000956 alloy Substances 0.000 abstract description 16
- 229910045601 alloy Inorganic materials 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 4
- 238000012216 screening Methods 0.000 abstract description 3
- 229910052702 rhenium Inorganic materials 0.000 abstract description 2
- 229940044175 cobalt sulfate Drugs 0.000 abstract 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 abstract 2
- 238000010297 mechanical methods and process Methods 0.000 abstract 1
- 238000000053 physical method Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000001154 acute effect Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 239000006247 magnetic powder Substances 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000005280 amorphization Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000005300 metallic glass Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000005480 shot peening Methods 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/04—Amorphous alloys with nickel or cobalt as the major constituent
-
- B22F1/0003—
-
- 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
- B22F9/002—Making metallic powder or suspensions thereof amorphous or microcrystalline
-
- 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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
-
- 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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Powder Metallurgy (AREA)
- Electroplating Methods And Accessories (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Laminated Bodies (AREA)
Abstract
一种Co基非晶合金粉末及其制备工艺,具体成分为Co40‑95wt%,合金元素为可以与Co一起电沉积的元素,如P、Ni、Fe、Cr、Mo、W、Re等中的一种或多种元素的组合。制备工艺,包括以下步骤:(1)金属基板被镀表面的预处理;(2)电镀液组成;硫酸钴、氯化钴或两者的混合物0.5‑3mol/L(优选1.5‑2mol/L),酸0.2‑0.8mol/L、络合剂0.5‑5g/L、合金元素添加剂0.2‑2mol/L、添加剂0‑2g/L,水余量;(3)非晶合金镀层的制备;(4)采用机械或物理的方法使非晶合金镀层脱落;(5)非晶合金颗粒的球磨;(6)筛分成不同粗细的Co基非晶合金粉末。
Description
技术领域
本发明涉及一种非晶合金粉末,尤其是涉及一种Co基非晶合金粉末及其制备工艺。
背景技术
随着电子电力、通信工业的发展,电子元器件向小型化、高频化和大电流方向发
展,而且对电子设备的电磁兼容性能的要求也越来越高,传统的非晶带材铁芯、软磁铁氧体
及金属磁粉芯等不能满足需求,应用受到限制。主要表现在:(1) 非晶带材铁芯在高频工作
时感应涡流导致损耗很大,限制其在高频领域的应用;(2) 软磁铁氧体高频损耗低,但是饱和磁感应强度和磁导率低,不能满足小型化和大电流的发展需求;(3) 金属磁粉芯存在着高频损耗高、直流叠加特性差或者价格昂贵等问题,限制了其应用范围。非晶磁性粉末由于其优异的软磁性能,可以满足各种电子元器件稳定化、小型化、高频化、大电流、高功率的需求,能极大促进汽车、电子、航空航天领域等高新技术行业的发展。
由于长程无序、短程有序的结构,使非晶粉末具有很多独特的性能。钴基非晶合金粉末除具有优异的磁性能,还具有耐高温、耐燃气腐蚀、耐磨、耐蚀等性能,在电子、涂层和硬质合金中得到广泛应用。而一些特殊场合对粉末性能提出更高的要求。
到目前为止,非晶合金粉末的制备工艺主要有水雾法、气雾法以及使用非晶薄带破碎制粉的工艺。水雾法具有大的冷却速率,可满足制备非晶态粉末的要求。然而,在水雾化过程中,所获得的粉末易形成氧化物,氧含量高,再者当熔融金属凝固时,产生的水蒸气会覆盖在熔融金属的表面,该水蒸气膜的存在将导致熔融的核心金属冷却强度降低,从而使粉末中心部分不能获得非晶态结构的问题,影响器件性能。气雾法由于冷却强度受限,只能制备非晶形成能力强的非晶合金粉末,且生产成本高。直接破碎法的优点在于对物料的选择性不强,材料利用率高,但需对非晶薄带进行脆化退火,很容易由于退火不均造成薄带内部晶化转变的不均匀,而且在破碎后容易产生带有锐角的粉末颗粒,为粉末的后续加工带来困难。这后两类方法都需要材料具有较强的非晶形成能力。
发明内容
基于上述问题,本发明提供了一种Co基非晶合金粉末及其制备工艺,该方法能够制备非晶合金材料组元的构成及比例选择范围更广的Co基非晶态合金粉末。
本发明的Co基非晶合金粉末,具体合金成分为Co40-95 wt %,合金元素为可以与Co一起电沉积的元素,如P、Ni、Fe、Cr、Mo、W、Re等中的一种或多种元素的组合。
本发明Co基非晶合金粉末的制备工艺,包括以下步骤:
(1)金属基板被镀表面的预处理:金属基板被镀表面预先采用机械加光,再经碱性溶液脱脂;
(2)电镀液组成;硫酸钴、氯化钴或两者的混合物0.5-3mol/L(优选1.5-2mol/L),酸0.2-0.8mol/L、络合剂0.5-5g/L、合金元素添加剂0.2-2mol/L、添加剂0-2g/L,水余量;
上所述合金元素添加剂中,铁以硫酸亚铁或氯化亚铁(需配有还原剂)、铬以铬酐、钼以钼酸钠、镍以硫酸镍或氯化镍、钨以钨酸钠、磷以亚磷酸或可溶性次磷酸盐、Re以Re可溶盐的形式添加;
上述酸包括硼酸、磷酸、羧酸等;
上述络合剂包括酒石酸、十二烷基苯磺酸钠、十二烷基硫酸钠、柠檬酸盐等;
上述添加剂为糖精、对甲苯磺酸胺等;
(3)非晶合金镀层的制备:预处理后的金属基板接入电镀槽阴极,阳极采用石墨或不锈钢,电镀时搅拌电镀液,电镀电源可采用恒电位电源或脉冲电源,电极的电流密度为200-1000mA/mm2(优选500-800mA/mm2),电解液温度为20-60℃,滴定强酸溶液使Ph值不大于1;
(4)采用机械或物理的方法,如轧制压延、喷丸、刮擦等方法使非晶合金镀层脱落;
(5)非晶合金颗粒的球磨,将剥落的非晶颗粒在真空或惰性气体保护条件下进行球磨,球磨可采用球磨机、行星式球磨机等,球磨时间为2-24h,球料比为3-10:1;
(6)筛分成不同粗细的Co基非晶合金粉末。
与现有技术相比,本发明具有以下优点:
1.与气雾法和直接破碎法相比,本工艺具有设备投资少、工艺简单,对非晶合金形成能力要求不高等特点;
2.与水雾法相比,粉末不会产生氧化和部分非晶化的问题;
3.与直接破碎法相比,由于采用PH值较小条件下沉积,致使镀层内产生了较大的内应力和较多孔隙,镀层无需脆化退火破碎,且也不会产生带有锐角的粉末颗粒;
4.相比常规电镀而言,因为对镀层应力和表面质量没有要求,因此可采用更大的电流密度,既提高了非晶合金镀层的制备速度,也有利于获得更疏松和具有更大内应力的非晶合金镀层,从而更易对非晶合金镀层进行机械剥离;
5.本方法无需考虑对材料的非晶形成能力,可通过调整电镀液各主要成分的浓度配比,可获得不同构成和比例的Co基非晶合金粉末,因此,本方法的适用性更为广泛,可操作性更强,可满足不同场合的性能要求。
具体实施方式
以下结合实施例对本发明作进一步说明。
实施例1 Co-P非晶合金粉末的制备
本实施例非晶合金粉末Co含量的92.3wt%,P含量为复合镀层的7.7wt%。
其制备工艺,包括以下步骤:
(1)金属基板表面的预处理:金属基板选用45号钢板,被镀基板表面经机械加工,然后在20wt%氢氧化钠溶液清洗10min去除油脂;
(2)电镀液组成:氯化钴0.3mol/L,硫酸钴2mol/L,硼酸40g/L,次磷酸钠0.65mol/L,酒石酸0.8g/L,糖精0.4g/L,水余量;
(3)非晶合金镀层的制备:预处理后的镀件接入电镀槽阴极,阳极采用石墨,搅拌电镀液,滴定盐酸溶液使Ph值为0.8,电极的电流密度为450mA/mm2,电镀液温度为60℃;
(4)非晶合金镀层的剥离:采用轧制压延法剥离镀层;
(5)非晶合金颗粒的球磨,采用行星球磨机球磨,非晶合金粉末充氩气保护,球磨5h,球料比为5:1;
(6)非晶合金粉末的筛分,采用200目和400目筛子分筛,其中大于200目粉末所占比例为36%,200-400目粉末所占比例为47%,小于400目粉末所占比例为17%。
实施例2 Co-Fe-P非晶合金粉末的制备
本实施例Co-Fe-P非晶合金粉末的制备,粉末Co含量79.6wt%,Fe含量为13.2wt%,P含量为7.2wt%。
其制备工艺,包括以下步骤:
(1)金属基板表面的预处理:金属基板选用45号钢板,被镀基板表面经机械加工,然后在20wt%氢氧化钠溶液清洗10min去除油脂;
(2)电镀液组成;氯化钴0.2mol/L,硫酸镍1.8mol/L,氯化亚铁0.35mol/L,磷酸50ml/L,亚磷酸0.65mol/L,碘化钾1g/L、酒石酸1g/L,对甲苯磺酸胺0.6g/L,水余量;
(3)非晶合金镀层的制备:预处理后的金属基板接入电镀槽阴极,阳极采用石墨,机械搅拌电镀液,电极的电流密度为650mA/mm2,滴定盐酸溶液使Ph值为0.8,电镀液温度为50℃;
(4)非晶合金镀层的剥离:采用刮擦法剥离镀层;
(5)非晶合金颗粒的球磨,采用行星球磨机球磨,非晶合金粉末充氩气保护球磨8h,球料比为3:1;
(6)非晶合金粉末的筛分,采用200目和400目筛子分筛,其中大于200目粉末所占比例为33%,200-400目粉末所占比例为42%,小于400目粉末所占比例25%。
Claims (1)
1.一种Co基非晶合金粉末的制备工艺,其特征在于,包括以下步骤:
(1)金属基板被镀表面的预处理;
(2)电镀液组成:硫酸钴、氯化钴或两者的混合物1.5-2mol/L、酸0.2-0.8mol/L、络合剂0.5-5g/L、合金元素添加剂0.2-2mol/L、添加剂0-2g/L、水适量;
上述合金元素添加剂中,铁以硫酸亚铁或氯化亚铁、铬以铬酐、钼以钼酸钠、镍以硫酸镍或氯化镍、钨以钨酸钠、磷以亚磷酸或可溶性次磷酸盐、Re以Re可溶盐的形式添加,其中铁元素添加剂需配有还原剂;
上述酸包括硼酸、磷酸、羧酸;
上述络合剂包括酒石酸、十二烷基苯磺酸钠、十二烷基硫酸钠、柠檬酸盐;
上述添加剂为糖精、对甲苯磺酸胺;
(3)非晶合金镀层的制备:预处理后的金属基板接入电镀槽阴极,阳极采用石墨或不锈钢,电镀时搅拌电镀液,电镀电源可采用恒电位电源或脉冲电源,电极的电流密度为500-800mA/mm2,电解液温度为20-60℃,滴定强酸溶液使pH值不大于1;
(4)采用物理的方法使非晶合金镀层脱落;
(5)非晶合金颗粒的球磨;
(6)筛分成不同粗细的Co基非晶合金粉末。
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