CN105861995B - ZrTiN-MoS2/Ti/Zr叠层涂层刀具及其制备工艺 - Google Patents
ZrTiN-MoS2/Ti/Zr叠层涂层刀具及其制备工艺 Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 82
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 35
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000011248 coating agent Substances 0.000 claims abstract description 52
- 230000007704 transition Effects 0.000 claims abstract description 33
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- 238000005461 lubrication Methods 0.000 claims abstract description 7
- 229910000997 High-speed steel Inorganic materials 0.000 claims abstract description 4
- 229910052582 BN Inorganic materials 0.000 claims abstract description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 3
- 239000010432 diamond Substances 0.000 claims abstract description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract 7
- 238000000151 deposition Methods 0.000 claims description 31
- 238000010891 electric arc Methods 0.000 claims description 29
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 26
- 238000007747 plating Methods 0.000 claims description 18
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- 238000000034 method Methods 0.000 claims description 13
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000007733 ion plating Methods 0.000 claims description 7
- 239000007888 film coating Substances 0.000 claims description 5
- 238000009501 film coating Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 238000010849 ion bombardment Methods 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 238000005477 sputtering target Methods 0.000 claims description 4
- 239000002344 surface layer Substances 0.000 claims description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000005520 cutting process Methods 0.000 abstract description 28
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- 239000002184 metal Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 description 13
- 239000000463 material Substances 0.000 description 11
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 5
- 239000011247 coating layer Substances 0.000 description 4
- 230000001050 lubricating effect Effects 0.000 description 4
- KRQUFUKTQHISJB-YYADALCUSA-N 2-[(E)-N-[2-(4-chlorophenoxy)propoxy]-C-propylcarbonimidoyl]-3-hydroxy-5-(thian-3-yl)cyclohex-2-en-1-one Chemical compound CCC\C(=N/OCC(C)OC1=CC=C(Cl)C=C1)C1=C(O)CC(CC1=O)C1CCCSC1 KRQUFUKTQHISJB-YYADALCUSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- -1 TiCN Inorganic materials 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 229910004211 TaS2 Inorganic materials 0.000 description 1
- 229910010037 TiAlN Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
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Abstract
本发明属于机械制造金属切削刀具领域，特别是涉及一种ZrTiN‑MoS2/Ti/Zr叠层涂层刀具及其制备工艺。其刀具基体材料为高速钢、硬质合金、立方氮化硼或金刚石，刀具表面为MoS2/Ti/Zr润滑涂层，且由基体到涂层表面依次为Ti过渡层、Ti/Zr过渡层、ZrTiN硬质涂层和MoS2/Ti/Zr润滑涂层交替的叠层复合结构。该刀具综合了ZrTiN多元硬质涂层、MoS2/Ti/Zr润滑涂层及叠层结构的优点，既可保持涂层较高的硬度，又可降低涂层的摩擦系数，使涂层刀具的切削性能有了显著地提高。叠层结构可使涂层刀具在涂层使用寿命周期中始终保持良好的减摩润滑性，延长润滑涂层的使用周期。
Description
技术领域
本发明属于机械制造金属切削刀具领域，特别是涉及一种ZrTiN-MoS2/Ti/Zr叠层涂层刀具及其制备工艺。
背景技术
根据涂层材料的性质，涂层刀具可分为两大类，即：“高硬度”涂层刀具和“润滑”涂层刀具。“高硬度”涂层刀具其主要优点是硬度高、耐磨性能好，典型的“高硬度”涂层材料有TiN、 TiCN、TiAlN和类金刚石等。“润滑”涂层刀具追求的目标是低摩擦系数，典型的“润滑”涂层材料为具有低摩擦系数的固体润滑材料(如：MoS2、WS2、TaS2等硫化物)。当前刀具涂层的发展趋势是：涂层成分趋于多元化和复合化。复合涂层可综合单涂层的优点，复合多涂层及其相关技术的出现，既可提高涂层与基体的结合强度，又兼顾多种单涂层的综合性能，使涂层刀具的性能显著提高。
中国专利(专利号ZL 2006 1 0068975.3)报道了“自润滑复合软涂层刀具及其制备方法”，它是采用中频磁控+多弧法镀膜方法制备的MoS2/Zr复合涂层刀具，刀具表面为MoS2层，MoS2层与刀具基体之间具有Ti过渡层。该刀具在无切削液冷却、润滑的切削过程中，能够在刀具表面能形成具有润滑作用的润滑膜，从而实现刀具自身的润滑功能，但是这种润滑涂层硬度较低而导致刀具涂层尤其是后刀面涂层的使用寿命不长。文献(ActaMaterials.2011,59(1): 68-74)报道了TiN硬涂层刀具切削加工时的作用机理及使用性能，但是这种硬涂层由于相对较高的摩擦系数，限制了其广泛使用。中国专利TiN+MoS2/Zr组合涂层刀具(专利号ZL 201110081977.7)采用中频磁控溅射与电弧镀复合镀膜方法制备的TiN+MoS2/Zr组合涂层刀具，但该组合涂层在干切削超硬材料时刀具使用寿命仍无法满足实际使用需要。中国专利梯度叠层涂层刀具及其制备方法(专利号ZL201110214393.2)制备的ZrTiN复合涂层刀具有较高的硬度和强度、优异的抗磨损和抗腐蚀性能，但是在切削有色金属材料时其表面摩擦系数较高，刀具使用寿命无法满足使用需要。
层状复合材料是近几年发展起来的材料增强增韧新技术，这种结构是通过模仿贝壳而来，因此又叫仿生叠层复合材料。自然界中贝壳的珍珠层是一种天然的层状结构材料，其断裂韧性却比普通单一均质结构高出3000倍以上。因此，通过模仿生物材料结构形式的层间设计，制备出的叠层复合涂层可以显著提高涂层的韧性、结合强度及减摩耐磨性等综合性能。
发明内容
本发明的目的在于克服上述现有涂层刀具技术的不足，结合多元硬质涂层、润滑涂层、多层结构的优点，提供一种ZrTiN-MoS2/Ti/Zr叠层涂层刀具及其制备工艺。
本发明是通过以下方式实现的：
ZrTiN-MoS2/Ti/Zr叠层涂层刀具，刀具基体材料为高速钢、硬质合金、立方氮化硼或金刚石，刀具表面为MoS2/Ti/Zr润滑涂层，且由基体到涂层表面依次为Ti过渡层、Ti/Zr过渡层、ZrTiN硬质涂层和MoS2/Ti/Zr润滑涂层交替的叠层复合结构。
所述ZrTiN-MoS2/Ti/Zr叠层涂层刀具的制备方法，其沉积方式为采用电弧镀与中频磁控溅射复合镀膜方法，包括1个Ti靶电弧靶，一个Zr靶电弧靶，2个MoS2中频溅射靶：电弧离子镀沉积Ti过渡层、Ti/Zr过渡层各5-6min，然后交替沉积厚度为30～40nm的ZrTiN硬质涂层(电弧离子镀)和厚度为10～20nm的MoS2/Ti/Zr润滑涂层(中频磁控溅射+电弧离子镀)，最后表面为MoS2/Ti/Zr润滑涂层。
具体包括以下步骤：
(1)前处理：将刀具基体表面抛光，去除表面杂质，然后依次放入酒精和丙酮中，超声清洗，经干燥后迅速放入镀膜机，抽真空至8.0×10-3Pa，加热至300℃，保温30～40min；
(2)离子清洗：通Ar气，其压力为1.5Pa，开启偏压电源，电压700V，占空比0.2，辉光放电清洗15min；降低偏压至500V，开启离子源离子清洗15min，开启Ti靶的电弧源，偏压300V，靶电流50A，离子轰击Ti靶1min；
(3)沉积Ti过渡层：Ar气压0.5～0.6Pa，偏压降至250V，Ti靶电流70A，沉积温度250℃，电弧镀Ti过渡层5～6min；
(4)沉积Ti/Zr过渡层：Ar气压0.5～0.6Pa，偏压250V，Ti靶电流80A，Zr靶电流90A，电弧镀Ti/Zr过渡层5～6min；
(5)沉积ZrTiN硬质涂层：开启N2，Ar气压0.5Pa，偏压220V，Ti靶的靶电流80A， Zr靶电流100A，N2气压为1.0Pa，沉积温度230～250℃，电弧镀ZrTiN硬质涂层3～4min；
(6)沉积MoS2/Ti/Zr润滑涂层：关闭N2，Ti靶电流60A，Zr靶电流80A，开启MoS2靶中频磁控溅射电源，电流1.5A，偏压调至200V，沉积温度250～270℃，复合沉积MoS2/Ti/Zr 润滑涂层3～4min；
(7)沉积ZrTiN硬质涂层：重复(5)；
(8)沉积MoS2/Ti/Zr润滑涂层：重复(6)；
(9)重复(5)、(6)、(5)…：交替沉积ZrTiN、MoS2/Ti/Zr…ZrTiN涂层共100min；
(10)沉积表层MoS2/Ti/Zr润滑涂层：重复(6)；
(11)后处理：关闭各电源、离子源及气体源，涂层结束。
与现有技术相比，本发明具有如下技术方案：
本发明所述涂层采用电弧镀与中频磁控溅射复合镀膜方法制备的ZrTiN-MoS2/Ti/Zr叠层涂层刀具，涂层是多层结构，其中基体上的Ti过渡层和Ti/Zr过渡层主要是提高涂层与刀具基体间的结合性能。该刀具综合了ZrTiN多元硬质涂层、MoS2/Ti/Zr润滑涂层及叠层结构的优点，既可保持涂层较高的硬度，又可降低涂层的摩擦系数，使涂层刀具的切削性能有了显著地提高。叠层结构可使涂层刀具在涂层使用寿命周期中始终保持良好的减摩润滑性，延长润滑涂层的使用周期。另外，叠层结构通过不同材料结构和成分组成的层间界面可以减缓涂层的过早剥落和裂纹的扩展。该涂层刀具进行切削时，由于表面MoS2/Ti/Zr涂层本身具有润滑作用，可以减小切削时的摩擦，降低切削力和切削温度；同时，ZrTiN高硬度涂层可提高 MoS2/Ti/Zr润滑涂层的整体强度，减缓由于MoS2/Ti/Zr涂层本身硬度较低而造成的刀具涂层过早磨损。与TiN+MoS2/Zr涂层刀具(专利号ZL 201110081977.7)相比，耐磨性提高了15-25％，涂层刀具使用寿命提高了20-35％；与ZrTiN复合涂层刀具(专利号201110214393.2)相比，表面摩擦系数降低35-40％，减摩耐磨性提高25-30％，涂层刀具使用寿命提高25％以上，且提高了涂层刀具的使用范围，可更广泛应用于包括有色金属在内的各种材料的切削加工。
附图说明
图1为本发明的软硬复合涂层刀具的涂层结构示意图。
图中：1为刀具基体、2为Ti过渡层、3为Ti/Zr过渡层、4为ZrTiN硬质涂层、5为MoS2/Ti/Zr 润滑涂层、6为ZrTiN与MoS2/Ti/Zr交替的涂层。
具体实施方式
下面给出本发明的最佳实施例：
实施例一
一种ZrTiN-MoS2/Ti/Zr叠层涂层刀具，该刀具为普通的铣刀片，其基体材料为：硬质合金YT15。沉积方式为采用电弧镀与中频磁控溅射复合镀膜方法制备组合涂层，包括1个Ti 靶电弧靶，一个Zr靶电弧靶，2个MoS2中频溅射靶：电弧离子镀沉积Ti、Ti/Zr过渡层、ZrTiN 硬质涂层，中频磁控溅射(MoS2)及电弧离子镀(Zr、Ti)复合沉积MoS2/Ti/Zr润滑涂层，其制备工艺为：
(1)前处理：将刀具基体表面抛光，去除表面油污、锈迹等杂质，然后依次放入酒精和丙酮中，超声清洗各30min，去除刀具表面油污和其它附着物，电吹风干燥充分后迅速放入镀膜机，抽真空至8.0×10-3Pa，加热至300℃，保温30～40min；
(2)离子清洗：通Ar气，其压力为1.5Pa，开启偏压电源，电压700V，占空比0.2，辉光放电清洗15min；降低偏压至500V，开启离子源离子清洗15min，开启Ti靶的电弧源，偏压300V，靶电流50A，离子轰击Ti靶1min；
(3)沉积Ti过渡层：Ar气压0.5～0.6Pa，偏压降至250V，Ti靶电流70A，沉积温度250℃，电弧镀Ti过渡层5～6min；
(4)沉积Ti/Zr过渡层：Ar气压0.5～0.6Pa，偏压250V，Ti靶电流80A，Zr靶电流90A，电弧镀Ti/Zr过渡层5～6min；
(5)沉积ZrTiN层：开启N2，Ar气压0.5Pa，偏压220V，Ti靶的靶电流80A，Zr靶电流100A，N2气压为1.0Pa，沉积温度230～250℃，电弧镀ZrTiN 3～4min；
(6)沉积MoS2/Ti/Zr层：关闭N2，Ti靶电流60A，Zr靶电流80A，开启MoS2靶中频磁控溅射电源，电流1.5A，偏压调至200V，沉积温度250～270℃，复合沉积MoS2/Ti/Zr 3～4min；
(7)沉积ZrTiN层：重复(5)；
(8)沉积MoS2/Ti/Zr层：重复(6)；
(9)重复(5)、(6)、(5)…：交替沉积ZrTiN、MoS2/Ti/Zr…ZrTiN涂层共100min；
(10)沉积表层MoS2/Ti/Zr层：重复(6)；
(11)后处理：关闭各电源、离子源及气体源，涂层结束。
实施例二
一种ZrTiN-MoS2/Ti/Zr叠层涂层刀具，该刀具为普通麻花钻，其刀具基体材料为：高速钢W18Cr4V。其沉积方式为采用电弧镀与中频磁控溅射复合镀膜方法制备组合涂层，包括1 个Ti靶电弧靶，一个Zr靶电弧靶，2个MoS2中频溅射靶：电弧离子镀沉积Ti、Ti/Zr过渡层、ZrTiN硬质涂层，中频磁控溅射(MoS2)及电弧离子镀(Zr、Ti)复合沉积MoS2/Ti/Zr 润滑涂层，其制备工艺为：
(1)前处理：将刀具基体表面抛光，去除表面油污、锈迹等杂质，然后依次放入酒精和丙酮中，超声清洗各30min，去除刀具表面油污和其它附着物，电吹风干燥充分后迅速放入镀膜机，抽真空至8.0×10-3Pa，加热至300℃，保温30～40min；
(2)离子清洗：通Ar气，其压力为1.5Pa，开启偏压电源，电压700V，占空比0.2，辉光放电清洗15min；降低偏压至500V，开启离子源离子清洗15min，开启Ti靶的电弧源，偏压300V，靶电流50A，离子轰击Ti靶1min；
(3)沉积Ti过渡层：Ar气压0.5～0.6Pa，偏压降至250V，Ti靶电流70A，沉积温度250℃，电弧镀Ti过渡层5～6min；
(4)沉积Ti/Zr过渡层：Ar气压0.5～0.6Pa，偏压250V，Ti靶电流80A，Zr靶电流90A，电弧镀Ti/Zr过渡层5～6min；
(5)沉积ZrTiN层：开启N2，Ar气压0.5Pa，偏压220V，Ti靶的靶电流80A，Zr靶电流100A，N2气压为1.0Pa，沉积温度230～250℃，电弧镀ZrTiN 3～4min；
(6)沉积MoS2/Ti/Zr层：关闭N2，Ti靶电流60A，Zr靶电流80A，开启MoS2靶中频磁控溅射电源，电流1.5A，偏压调至200V，沉积温度250～270℃，复合沉积MoS2/Ti/Zr 3～4min；
(7)沉积ZrTiN层：重复(5)；
(8)沉积MoS2/Ti/Zr层：重复(6)；
(9)重复(5)、(6)、(5)…：交替沉积ZrTiN、MoS2/Ti/Zr…ZrTiN涂层共100min；
(10)沉积表层MoS2/Ti/Zr层：重复(6)；
(11)后处理：关闭各电源、离子源及气体源，涂层结束。
Claims (1)
1.一种ZrTiN-MoS2/Ti/Zr叠层涂层刀具的制备工艺，刀具基体材料为高速钢、硬质合金、立方氮化硼或金刚石，刀具表面为MoS2/Ti/Zr润滑涂层，且由基体到涂层表面依次为Ti过渡层、Ti/Zr过渡层、ZrTiN硬质涂层和MoS2/Ti/Zr润滑涂层交替的叠层复合结构；其特征在于，沉积方式为采用电弧镀与中频磁控溅射复合镀膜方法，包括1个Ti靶电弧靶，一个Zr靶电弧靶，2个MoS2中频溅射靶：电弧离子镀沉积Ti过渡层、Ti/Zr过渡层各5-6min，然后交替沉积厚度为30～40nm的ZrTiN硬质涂层和厚度为10～20nm的MoS2/Ti/Zr润滑涂层，最后表面为MoS2/Ti/Zr润滑涂层，具体包括以下步骤：
(1)前处理：将刀具基体表面抛光，去除表面杂质，然后依次放入酒精和丙酮中，超声清洗，经干燥后迅速放入镀膜机，抽真空至8.0×10-3Pa，加热至300℃，保温30～40min；
(2)离子清洗：通Ar气，其压力为1.5Pa，开启偏压电源，电压700V，占空比0.2，辉光放电清洗15min；降低偏压至500V，开启离子源离子清洗15min，开启Ti靶的电弧源，偏压300V，靶电流50A，离子轰击Ti靶1min；
(3)沉积Ti过渡层：Ar气压0.5～0.6Pa，偏压降至250V，Ti靶电流70A，沉积温度250℃，电弧镀Ti过渡层5～6min；
(4)沉积Ti/Zr过渡层：Ar气压0.5～0.6Pa，偏压250V，Ti靶电流80A，Zr靶电流90A，电弧镀Ti/Zr过渡层5～6min；
(5)沉积ZrTiN硬质涂层：开启N2，Ar气压0.5Pa，偏压220V，Ti靶的靶电流80A，Zr靶电流100A，N2气压为1.0Pa，沉积温度230～250℃，电弧镀ZrTiN硬质涂层3～4min；
(6)沉积MoS2/Ti/Zr润滑涂层：关闭N2，Ti靶电流60A，Zr靶电流80A，开启MoS2靶中频磁控溅射电源，电流1.5A，偏压调至200V，沉积温度250～270℃，复合沉积MoS2/Ti/Zr润滑涂层3～4min；
(7)沉积ZrTiN硬质涂层：重复(5)；
(8)沉积MoS2/Ti/Zr润滑涂层：重复(6)；
(9)重复(5)、(6)、(5)···：交替沉积ZrTiN、MoS2/Ti/Zr···ZrTiN涂层共100min；
(10)沉积表层MoS2/Ti/Zr润滑涂层：重复(6)；
(11)后处理：关闭各电源、离子源及气体源，涂层结束。
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