CN111424270A - 铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法 - Google Patents
铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法 Download PDFInfo
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 159
- 239000010432 diamond Substances 0.000 title claims abstract description 159
- 239000002245 particle Substances 0.000 title claims abstract description 117
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 86
- 239000010949 copper Substances 0.000 title claims abstract description 86
- 238000000576 coating method Methods 0.000 title claims abstract description 70
- 239000011248 coating agent Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 43
- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 39
- 238000004372 laser cladding Methods 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 239000011651 chromium Substances 0.000 claims abstract description 51
- 238000007747 plating Methods 0.000 claims abstract description 33
- 229910052709 silver Inorganic materials 0.000 claims abstract description 32
- 239000004332 silver Substances 0.000 claims abstract description 31
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 30
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 239000011812 mixed powder Substances 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000002844 melting Methods 0.000 claims abstract description 7
- 230000008018 melting Effects 0.000 claims abstract description 7
- 238000007711 solidification Methods 0.000 claims abstract description 3
- 230000008023 solidification Effects 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 46
- 239000000843 powder Substances 0.000 claims description 40
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 28
- 229910052786 argon Inorganic materials 0.000 claims description 23
- 238000000498 ball milling Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 238000005253 cladding Methods 0.000 claims description 6
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- 238000009713 electroplating Methods 0.000 claims description 4
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- 238000005086 pumping Methods 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000001723 curing Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
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- 238000012986 modification Methods 0.000 abstract description 3
- 239000007769 metal material Substances 0.000 abstract description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 15
- 150000003839 salts Chemical class 0.000 description 13
- 239000000463 material Substances 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000005087 graphitization Methods 0.000 description 7
- 230000007935 neutral effect Effects 0.000 description 7
- 239000011208 reinforced composite material Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000004020 conductor Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 239000000956 alloy Substances 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- BUKHSQBUKZIMLB-UHFFFAOYSA-L potassium;sodium;dichloride Chemical compound [Na+].[Cl-].[Cl-].[K+] BUKHSQBUKZIMLB-UHFFFAOYSA-L 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000009749 continuous casting Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
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- 230000014759 maintenance of location Effects 0.000 description 1
- -1 on the other hand Substances 0.000 description 1
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Classifications
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
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- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
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- 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
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C23C18/1646—Characteristics of the product obtained
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
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- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
- B22F2007/042—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method
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- B22F9/00—Making metallic powder or suspensions thereof
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Abstract
本发明属于金属材料表面改性领域,公开了一种在铜及铜合金表面采用激光熔覆技术制备铜基金刚石颗粒增强复合涂层的方法。采用金属铬和银依次镀覆在金刚石颗粒表面,形成铬/银双镀层金刚石颗粒,将所述铬/银双镀层金刚石颗粒与紫铜粉进行混合配制金刚石/紫铜混合粉末,所述金刚石/紫铜混合粉末铺于铜合金基板,再铺上紫铜粉,进行烧结固化成型,然后采用激光熔覆的方法熔化预置的所述金刚石/紫铜混合粉末,凝固后形成铜基金刚石颗粒增强复合涂层。本发明采用双镀层预处理金刚石颗粒,有效避免了金刚石颗粒在加工中出现的结构损伤,同时解决了金刚石与铜基体的结合问题。
Description
技术领域
本发明涉及金属材料表面改性领域,尤其涉及一种铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法。
背景技术
铜及其合金具有优良的导电和导热性能,在电子封装、大型散热器件中得到广泛应用。然而,随着技术升级造成装备服役环境的愈发恶劣,要求散热器件不仅具备较高的导热导电性能,同时具备较高的耐磨性能,如钢铁生产行业中使用的钢铁连铸结晶器,承受着钢铁连铸生产中的超高温和强摩擦作用;电磁炮作为下一代先进动能杀伤武器,其导轨材料既要承受炮弹发射时热损耗而产生的高温,还要承受炮弹在导轨上运动时的高速摩擦作用。传统的单质铜及铜合金材料已经无法满足这些高技术装备的综合要求和高指标要求。因此铜基材料的表面复合化是其发展的必然趋势,亟需在铜合金表面制备出高耐磨性能的涂层材料,同时不降低铜合金表面与外界的热传导效率。
金刚石是自然界中导热性能最高的材料,导热系数约在2000W/(m·K)左右,同时金刚石的原子结构决定了它具备极高的硬度和较低的热膨胀系数,已被广泛应用在高摩擦工况的切割刀具表面。因此,如果能将金刚石颗粒作为弥散强化相与铜粉混合并在传统导热材料表面制备一种复合材料涂层,则会在确保材料整体导热性能不下降的情况下,极大地提升材料表面的耐磨性能。
目前,对于铜基金刚石颗粒增强复合材料及其激光熔覆涂层已经有一定的研究,例如:在《.铬包覆的金刚石颗粒增强铜基复合材料的热物理性能研究》中,朱聪旭等人通过混合熔盐法对金刚石表面进行镀铬处理,并采用放电等离子烧结技术制备了镀铬金刚石颗粒增强铜基复合材料,结果表明金刚石与铜基体的界面结合得到优化,复合材料的密度和热导率获得较大提升,放电等离子烧结工艺下较长的高温停留时间极易造成金刚石表面镀层厚度的增加,从而导致镀层出现开裂等现象,进而导致金刚石石墨化以及界面结合的恶化;在《激光熔覆/熔注法制备金属基金刚石复合涂层研究》中,吴佳采用激光熔覆技术在45钢表面分别制备了铁基和镍基的金刚石颗粒增强涂层,结果显示铁/镍基金刚石颗粒涂层的应用分别提升了基体表面60%和30%的耐磨性能,但是涂层内部的金刚石颗粒均发生了较大程度的石墨化相变,未镀覆的金刚石颗粒在激光的辐照下极易发生石墨化相变,且镍、铁等传统耐磨材料作为基体粉末在提高涂层耐磨性能的同时牺牲了涂层的导热性。然而,在铜基合金表面激光熔覆制备金刚石颗粒增强铜基涂层材料还存在较多困难,主要存在以下几个问题:
(1)铜基体导热系数很高,而且对于激光的反射率较高,不利于涂层与基体的熔化和界面有效结合;
(2)金刚石在激光照射的高温下易发生石墨化转变,原子结构遭到破坏从而丧失金刚石的物理性质,同时在有氧环境下,金刚石石墨化的温度会进一步降低;
(3)铜在高温下对氧含量较为敏感,易形成氧化物,造成铜基体与金刚石颗粒之间难以形成有效界面结合。
因此,本发明致力于优化激光熔覆工艺方案,以及开发金刚石颗粒界面优化的方法,提供了一种铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法。
发明内容
有鉴于现有技术的上述缺陷,本发明所要解决的技术问题是避免金刚石颗粒在加工中出现的石墨化转变而导致原子结构损伤,同时解决金刚石与铜基体的界面结合问题。
为实现上述目的,本发明提供了一种适用于铜合金表面的含铬/银双镀层的金刚石颗粒增强铜基复合材料涂层,采用金属铬和银依次镀覆在金刚石颗粒表面,形成铬/银的双镀层结构,一方面铬是强碳化物形成元素,可以与金刚石表面形成良好结合,另一方面,银在铜中有一定的固溶度,能够与铜形成有效连接,而且银具有更高的激光反射率,在激光熔覆过程中可减小金刚石颗粒对激光能量的吸收,从而有效保护金刚石颗粒避免石墨化。
具体地,铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法,包括以下步骤:
(1)超声清洗金刚石颗粒,在所述金刚石颗粒表面,通过电镀或化学镀的方法依次镀覆铬、银镀层,形成铬/银双镀层结构,得到铬/银双镀层金刚石颗粒,其中采用电镀或化学镀的方式在金刚石颗粒表面先后镀覆一层均匀的铬层和银层的目的是隔绝金刚石与氧气以及激光热源的直接接触,避免因氧化和过热引起的石墨化,同时改善金刚石颗粒与铜基体的结合;
(2)将所述铬/银双镀层金刚石颗粒与紫铜粉进行混合配制金刚石/紫铜混合粉末;
(3)将铜合金基板上铺上所述金刚石/紫铜混合粉末,再铺上紫铜粉,放入加热炉中进行烧结,使得所述金刚石/紫铜混合粉末在所述铜合金基板上初步固化成型,得到烧结预成型的铜合金基板;
(4)对所述烧结预成型的铜合金基板进行预热,在所述烧结预成型的铜合金基板表面采用激光熔覆的方法熔化预置的所述金刚石/紫铜混合粉末,凝固后形成铜基金刚石颗粒增强复合涂层。
进一步地,所述金刚石颗粒粒径为100~300目。
进一步地,所述步骤(1)金刚石表面电镀铬、银镀层时在通氩气的电阻炉或真空炉中进行反应烧结,烧结温度在700~950℃,保温时间为1~1.5h。
进一步地,所述步骤(1)包括:在镀铬过程中,采用电磁搅拌或超声波震荡金刚石颗粒,确保颗粒表面镀层均匀,制得表面镀层均匀的镀铬金刚石颗粒;将所述镀铬金刚石颗粒与化学镀银液进行混合,并加以超声振荡均匀分布所述金刚石颗粒,得到所述铬/银双镀层金刚石颗粒。
进一步地,所述步骤(2)中所述铬/银双镀层金刚石颗粒与所述紫铜粉按1:(3~5)的质量比混合,混合方式采用机械球磨方式,达到所述紫铜粉与所述金刚石颗粒的初步机械嵌合,球磨罐内抽真空或填充纯氩气氛,所述紫铜粉的粒径为200~325目。
进一步地,所述步骤(3)中所述金刚石/紫铜混合粉末的铺粉厚度为0.4~0.6mm,所述紫铜粉的铺粉厚度为0.35~0.4mm。
进一步地,所述步骤(3)在通惰性气体的电阻炉或真空炉中进行反应烧结,烧结温度在500~900℃,升温速率为10~30℃/min,保温时间为2~10min。
进一步地,所步骤(4)的烧结预成型的铜合金基板的预热温度为450~900℃,预热过程中持续通氩气保护,氩气流量为10~15L/min。
进一步地,所步骤(4)的激光熔覆采用半导体激光器作为热源,激光功率为0.8~1.8kW,扫描速度为3~7mm/s,光斑直径为7mm,氩气流量为15L/min。
进一步地,铜基金刚石颗粒增强复合涂层熔覆完成后,其冷却方式采用惰性气体冷却,气体流量为15~20L/min。
与现有技术相比,本发明的优点在于:
(1)本发明中的金刚石颗粒增强铜基复合材料涂层采用铬/银双镀层包覆金刚石表面,有效避免了金刚石与氧气的直接接触以及激光的直接辐照,抑制了金刚石颗粒的石墨化程度,改善了金刚石与铜基体的界面结合,显著提升了涂层的质量;
(2)本发明金刚石颗粒增强铜基复合材料涂层的激光熔覆工艺,采用预置粉末层铺的方式配合烧结预成型工艺,利用上层的纯铜粉将下层的金刚石粉层与外部空气进行隔离,进一步避免金刚石颗粒氧化;在优化的激光功率和扫描速度下,激光熔覆技术精准的热源调控有效地实现了金刚石结构的完好以及涂层结构的致密。
(3)本发明所涉及的复合材料涂层及其制备方法也可应用于其他导热材料(Al、Ag等)的表面修复,对于工程设备中难以替换的导热材料,可以直接在其表面实现修复再制造,不仅极大地节约了企业成本,而且相关寿命明显超过了修复前的材料本身。
本发明具有实际的应用前景,铬/银镀层有效地保护了金刚石颗粒在激光加工过程中的完整性,改善了金刚石与铜基体的界面结合,在保证涂层高导热性能的基础上进一步提高了耐磨性能,并且通过粉末的层铺处理以及烧结预成型处理,极大地降低了涂层材料在加工过程中的氧化和烧蚀,激光熔覆前的预热处理进一步提高了材料对激光的吸收率,保证了涂层与基体的有效冶金结合。
具体实施方式
以下介绍本发明的多个优选实施例,使其技术内容更加清楚和便于理解。本发明可以通过许多不同形式的实施例来得以体现,本发明的保护范围并非仅限于文中提到的实施例。
实施例一
(1)选取平均粒径为300目的金刚石颗粒,对金刚石颗粒依次进行丙酮和无水乙醇环境下的超声清洗,结束后取出并用去离子水洗至中性,其中,工作气压为常压,超声清洗时间为15min,清洗温度为20℃;
(2)将金刚石颗粒、Cr粉以及混合盐NaCl-KCl(质量比NaCl:KCl=1:1)配置混合原料,金刚石颗粒:Cr粉:混合盐的质量比为1:3:5~10,然后在通氩气的管式电阻炉中以5℃/min的升温速度加热至950℃并保温1h进行反应烧结,在高温下使熔盐中的Cr粉与金刚石表面反应形成Cr7C3/Cr层。随炉冷却后,将产物进行反复超声清洗和过筛处理,得到表面Cr包覆的金刚石颗粒;
(3)将镀Cr金刚石颗粒放置在无水乙醇中进行超声清洗15min,并用去离子水洗至中性后加入配置好的化学镀银液,通过超声振荡使金刚石颗粒均匀分布后,随即加入还原剂C6H12O6进行3min的镀覆反应,反应结束后取出并用去离子水冲洗至中性并烘干后,得到Cr/Ag双镀层金刚石颗粒;
(4)将Cr/Ag双镀层金刚石颗粒与粒径为325目的紫铜粉按照1:3的质量比混合,并进行机械球磨,球磨转速为250r/min,球磨时间为16h,球磨罐内抽真空,使得金刚石颗粒与铜之间达到初步的机械嵌合,得到金刚石/紫铜混合粉末;
(5)对紫铜基板进行除油除锈处理后,将金刚石/紫铜混合粉末铺入预先加工好的紫铜基板上,铺粉厚度为0.6mm,再将紫铜粉均匀铺在混合粉层上,铺粉厚度为0.4mm,最终实现紫铜基板-金刚石/紫铜混合粉末-紫铜粉的层铺粉结构;
(6)将已铺粉的铜合金基板放入真空/惰性气氛加热炉中加热至900℃,升温速率为30℃/min并保温2min,确保层铺粉末层达到初步的固化成型;
(7)预热铜合金基板至450℃,预热过程中持续通氩气保护,氩气流量为10l/min,并采用激光熔覆的方法,激光光斑直径为7mm,激光功率为1.8kW,扫描速度为7mm/s,持续通氩气保护,氩气流量为15L/min,将预置粉末层熔化制备成铜基金刚石颗粒增强复合材料涂层;
(8)铜基金刚石颗粒增强复合材料涂层熔覆完成后,在惰性汽体重冷却,惰性气体流量改为15L/min。
实施例二
(1)将平均粒径为200目的金刚石颗粒,对金刚石颗粒依次进行丙酮和无水乙醇环境下的超声清洗,结束后取出并用去离子水洗至中性,其中,工作气压为常压,超声清洗时间为15min,清洗温度为20℃;
(2)选取金刚石颗粒、Cr粉以及混合盐NaCl-KCl(质量比NaCl:KCl=1:1)配置混合原料,金刚石微粉:Cr粉:混合盐的质量比为1:4:5~10,然后在通氩气的管式电阻炉中以10℃/min的升温速度加热至700℃并保温1.5h进行反应烧结,在高温下使熔盐中的Cr粉与金刚石表面反应形成Cr7C3/Cr层。随炉冷却后,将产物进行反复超声清洗和过筛处理,得到表面Cr包覆的金刚石颗粒;
(3)将镀Cr金刚石粉放置在无水乙醇中进行超声清洗15min,并用去离子水洗至中性后加入配置好的化学镀银液,通过超声振荡使金刚石颗粒均匀分布后,随即加入还原剂C6H12O6进行3min的镀覆反应,反应结束后取出并用去离子水冲洗至中性并烘干后,得到Cr/Ag双镀层金刚石颗粒;
(4)将Cr/Ag双镀层金刚石颗粒与粒径为200目的紫铜粉按照1:4的质量比混合,并进行机械球磨,球磨转速为250r/min,球磨时间为16h,球磨罐内抽真空,使得金刚石颗粒与铜之间达到初步的机械嵌合,得到金刚石/紫铜混合粉末;
(5)对紫铜基板进行除油除锈处理后,将金刚石/紫铜混合粉末铺入预先加工好的紫铜基板上,铺粉厚度为0.4mm,再将紫铜粉均匀铺在金刚石/紫铜混合粉末层上,铺粉厚度为0.35mm,最终实现紫铜基板-金刚石/紫铜混合粉-紫铜粉的层铺粉结构;
(6)将已铺粉的铜合金基板放入真空/惰性气氛加热炉中加热至750℃,升温速率为15℃/min并保温5min,确保层铺粉末层达到初步的固化成型;
(7)预热铜合金基板至700℃,预热过程中持续通氩气保护,氩气流量为15L/min,并采用激光熔覆的方法,激光光斑直径为7mm,激光功率为1.5kW,扫描速度为5mm/s,持续通氩气保护,氩气流量为15L/min,将预置粉末层熔化制备成铜基金刚石颗粒增强复合材料涂层;
(8)铜基金刚石颗粒增强复合材料涂层熔覆完成后,在惰性汽体重冷却,惰性气体流量改为15L/min。
实施例三
(1)将平均粒径为100目的金刚石微粉,对金刚石微粉依次进行丙酮和无水乙醇环境下的超声清洗,结束后取出并用去离子水洗至中性,其中工作气压为常压,超声清洗时间为15min,清洗温度为20℃;
(2)选取金刚石颗粒、Cr粉以及混合盐NaCl-KCl(质量比NaCl:KCl=1:1)配置混合原料,金刚石颗粒:Cr粉:混合盐的质量比为1:5:5~10,然后在通氩气的管式电阻炉中以10℃/min的升温速度加热至800℃并保温1h进行反应烧结,在高温下使熔盐中的Cr粉与金刚石表面反应形成Cr7C3/Cr层,随炉冷却后,将产物进行反复超声清洗和过筛处理,得到表面Cr包覆的金刚石颗粒;
(3)将镀Cr金刚石粉放置在无水乙醇中进行超声清洗15min,并用去离子水洗至中性后加入配置好的化学镀银液,通过超声振荡使金刚石颗粒均匀分布后,随即加入还原剂C6H12O6进行3min的镀覆反应,反应结束后取出并用去离子水冲洗至中性并烘干后,得到Cr/Ag双镀层金刚石颗粒;
(4)将Cr/Ag双镀层金刚石颗粒与粒径为325目的紫铜粉按照1:5的质量比混合,并进行机械球磨,球磨转速为250r/min,球磨时间为16h,球磨罐内抽真空,使得金刚石颗粒与铜之间达到初步的机械嵌合;
(5)对紫铜基板进行除油除锈处理后,将混合后的金刚石/铜混合粉铺入预先加工好的紫铜基板上,铺粉厚度为0.6mm,再将紫铜粉均匀铺在混合粉层上,铺粉厚度为0.35mm,最终实现紫铜基板-金刚石/铜混合粉-紫铜粉的层铺结构;
(6)将已铺粉的铜合金基板放入真空/惰性气氛加热炉中加热至500℃,升温速率为10℃/min并保温10min,确保层铺粉末层达到初步的固化成型;
(7)预热铜合金基板至900℃,预热过程中持续通氩气保护,氩气流量为15L/min,并采用激光熔覆的方法,激光光斑直径为7mm,激光功率为0.8kW,扫描速度为3mm/s,持续通氩气保护,熔覆时氩气流量为10L/min,将预置粉末层熔化制备成铜基金刚石颗粒增强复合材料涂层;
(8)铜基金刚石颗粒增强复合材料涂层熔覆完成后,在惰性汽体重冷却,惰性气体流量改为15L/min。
表1和表2分别为不同实施例得到的复合涂层的硬度和热导率数值。本发明采用了不同的参数进行了完整的制备实验,得到的涂层表面平整且呈现银灰色光泽,与硬度较高的黄铜对比,涂层硬度显著提升2~3倍。与热导率与导热性能优异的紫铜对比,涂层热导率略有下降或相同。
表1实施例1~3得到的涂层的硬度值
表2实施例1~3得到的涂层的热导率
以上详细描述了本发明的较佳具体实施例。应当理解,本领域的普通技术无需创造性劳动就可以根据本发明的构思作出诸多修改和变化。因此,凡本技术领域中技术人员依本发明的构思在现有技术的基础上通过逻辑分析、推理或者有限的实验可以得到的技术方案,皆应在由权利要求书所确定的保护范围内。
Claims (10)
1.一种铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法,其特征在于,包括以下步骤:
(1)超声清洗金刚石颗粒,在所述金刚石颗粒表面,通过电镀或化学镀的方法依次镀覆铬、银镀层,形成铬/银双镀层结构,得到铬/银双镀层金刚石颗粒;
(2)将所述铬/银双镀层金刚石颗粒与紫铜粉进行混合配制金刚石/紫铜混合粉末;
(3)将铜合金基板上铺上所述金刚石/紫铜混合粉末,再铺上紫铜粉,放入加热炉中进行烧结,使得所述金刚石/紫铜混合粉末在所述铜合金基板上初步固化成型,得到烧结预成型的铜合金基板;
(4)对所述烧结预成型的铜合金基板进行预热,在所述烧结预成型的铜合金基板表面采用激光熔覆的方法熔化预置的所述金刚石/紫铜混合粉末,凝固后形成铜基金刚石颗粒增强复合涂层。
2.如权利要求1所述的铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法,其特征在于,所述金刚石颗粒粒径为100~300目。
3.如权利要求1所述的铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法,其特征在于,所述步骤(1)金刚石表面电镀铬、银镀层时在通氩气的电阻炉或真空炉中进行反应烧结,烧结温度为700~950℃,保温时间为1~1.5h。
4.如权利要求1-3任一项所述的铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法,其特征在于,所述步骤(1)包括:在镀铬过程中,采用电磁搅拌或超声波震荡所述金刚石颗粒,制得表面镀层均匀的镀铬金刚石颗粒;将所述镀铬金刚石颗粒与化学镀银液进行混合,并加以超声振荡所述镀铬金刚石颗粒,得到所述铬/银双镀层金刚石颗粒。
5.如权利要求1-3任一项所述的铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法,其特征在于,所述步骤(2)中所述铬/银双镀层金刚石颗粒与所述紫铜粉分按1:(3~5)的质量比混合,混合方式采用机械球磨方式,球磨罐内抽真空或填充纯氩气氛,所述紫铜粉的粒径为200~325目。
6.如权利要求1所述的铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法,其特征在于,所述步骤(3)中所述金刚石/紫铜混合粉末的铺粉厚度为0.4~0.6mm,所述紫铜粉的铺粉厚度为0.35~0.4mm。
7.如权利要求1-3或6任一项所述的铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法,其特征在于,所述步骤(3)在通惰性气体的电阻炉或真空炉中进行反应烧结,烧结温度在500~900℃,升温速率为10~30℃/min,保温时间为2~10min。
8.如权利要求1所述的铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法,其特征在于,所步骤(4)的烧结预成型的铜合金基板的预热温度为450~900℃,预热过程中持续通氩气保护,氩气流量为10~15L/min。
9.如权利要求1-3或8任一项所述的铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法,其特征在于,所步骤(4)的激光熔覆采用半导体激光器作为热源,激光功率为0.8~1.8kW,扫描速度为3~7mm/s,光斑直径为7mm,氩气流量为15L/min。
10.如权利要求1-3或6或8任一项所述的铜合金表面激光熔覆铜基金刚石颗粒增强复合涂层的方法,其特征在于,所述铜基金刚石颗粒增强复合涂层熔覆完成后,其冷却方式采用惰性气体冷却,气体流量为15~20L/min。
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