CN1020476C - 钛上镀氮化物层的方法 - Google Patents

钛上镀氮化物层的方法 Download PDF

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CN1020476C
CN1020476C CN90110418A CN90110418A CN1020476C CN 1020476 C CN1020476 C CN 1020476C CN 90110418 A CN90110418 A CN 90110418A CN 90110418 A CN90110418 A CN 90110418A CN 1020476 C CN1020476 C CN 1020476C
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titanium
ammonia
temperature
workpiece
pressure
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CN1057866A (zh
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弗里德里克·普莱斯尔
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Evonik Operations GmbH
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Degussa GmbH
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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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/24—Nitriding

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  • Mechanical Engineering (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
  • Chemically Coating (AREA)
  • Physical Vapour Deposition (AREA)
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Abstract

一种在钛和钛合金上镀覆氮化物层的实用方法。通过在氨气氛中加压氮化，在短时间内得到20μm厚度的覆层。为此，必需使温度为500-1000℃，压力为0.2-10MPa。

Description

本发明涉及在由钛和钛合金构成的工件上，通过在加压和500℃以上温度下，用氨或含氨气体混合物对工件进行热化学处理的氮化物层镀覆方法。
作为结构材料，钛比钢具有某些优点，即比重小、耐腐蚀及强度高。另一方面，则由于其硬度较低而需要进行表面处理来提高耐磨性。这种表面处理通常是形成碳化钛或氮化钛层。迄今，对由钛和钛合金构成的工件进行氮化的已知方法包括，使用高能气体或电磁场。这些方法非常昂贵，而且只能用于几何形状简单的工件。
在联邦德国专利说明书DE-PS1796212中，提到了在氨气氛中，于较高温度和常压下，通过生成氮化物层的钛表面硬化方法。
尽管这一方法旨在制备相当厚的硬覆层，但由于牵涉到氢扩散使工件中心部分变脆，而根本不合实用。
EP-A-0105835提及一种在钛和钛合金构成的工件上制备氮化物层的方法，该方法是在高压釜中，将这类工件暴露于压力至少10MPa和温度至少200℃的氨气氛来进行的。在此情况下，氨必须很纯。这种氮化，优先在90-130MPa压力及930-1000℃温度下进行。该方法的缺点是，由于使用高压釜和很纯的氨而非常昂贵，并且在三小时或三小时以上的时间后，仅能得到20μm厚的覆层。
因而，本发明的目的是要研制一种在由钛和钛合金构成的工件上，于加压和500℃以上温度下，通过用氨或含氨气体混合物对这些工件进行热化学处理，来镀覆氮化物层的方法，该方法不但经济，而且可以在相当短的时间内形成20μm或更厚的氮化物层。
按照本发明，通过在500-1000℃温度及0.2-10MPa压力下（在该情况下氨分压至少必须为0.2MPa）进行处理而达到了这一目的。
温度为700-950℃和压力为0.5-7MPa（在此情况下氨分压要须至少为0.2MPa）已被证明特别有利。
使用这种加压处理，可以在箱式炉中向任何形状和尺寸的钛和钛合金部件提供20μm或20μm以上足够厚的氮化物层。意外的是，根本不需极其纯的气体，正常商业级的氨即已足够。此外，可以将氮与氨混合，在该情况下，进行氮化处理仅需要至少为0.2MPa的氨分压。
在广泛的压力范围内，所生成的氮化钛层厚度，取决于温度和处理的持续时间。处理后的表面为金色，并使硬度显著提高。在压力高于6MPa范围时，覆层的厚度几乎与压力无关。
曲线图表明，纯钛工件上氮化钛层的生成量，是含氨气氛压力和温度的函数。
甚至在500℃温度时，例如在2MPa（＝20巴）绝对压力下，1小时后测得10μm厚的TiN层。在880℃下，此时生成20μm的纯TiN层。
在6MPa（＝60巴）压力时，例如若将样品在880℃下保持1小时，则生成30μm的TiN层。
压力进一步增至9MPa（＝90巴）时，压力对TiN层厚度的影响减小。厚度增加不再成线性。在甚至更高的压力下，由于迅速形成致密的TiN层，只有氮透过该层的扩散才是决定时间的因素。
按处理纯钛的同样方法，也可以将钛合金，例如TiAl6V4氮化。
这些镀覆方法，根本不需高压釜，而处理却可以在标准工业箱式炉中进行。

Claims (2)

1、在由钛和钛合金构成的工件上，通过在加压和温度高于500℃时，用氨或氨-氮气体混合物对此种工件进行热化学处理的氮化物层镀覆方法，其特征在于，该处理在500-1000℃温度和0.2-10MPa下进行，同时氨分压须至少为0.2MPa。
2、权利要求1所述的氮化物层镀覆方法，其特征在于，该处理在700-950℃温度和0.5-7MPa压力下进行，同时氨分压须至少为0.2MPa。
CN90110418A 1990-07-04 1990-12-20 钛上镀氮化物层的方法 Expired - Fee Related CN1020476C (zh)

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DE4021286A DE4021286C1 (zh) 1990-07-04 1990-07-04
DEP4021286.6 1990-07-04

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JP (1) JPH0649924B2 (zh)
CN (1) CN1020476C (zh)
AT (1) ATE135058T1 (zh)
AU (1) AU627960B2 (zh)
BR (1) BR9101899A (zh)
CZ (1) CZ279472B6 (zh)
DE (2) DE4021286C1 (zh)
ES (1) ES2085320T3 (zh)
NO (1) NO905209L (zh)
PL (1) PL166281B1 (zh)
PT (1) PT98195A (zh)
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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN100537805C (zh) * 2007-10-30 2009-09-09 沈阳宝鼎化工设备制造有限公司 耐磨、耐腐蚀备件及其表面处理工艺

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WO2000063454A1 (de) * 1999-04-15 2000-10-26 Vacuumschmelze Gmbh Korrosionsfreie eisen-nickel-legierung für fehlerstromschutzschalter und uhrenlaufwerke
JP4684383B2 (ja) * 2000-04-03 2011-05-18 株式会社アライドマテリアル 耐酸化層を有する高融点金属材料及びその製造方法
JP2001295023A (ja) * 2000-04-06 2001-10-26 Allied Material Corp 表面硬化層を有する高融点金属材料およびその製造方法
US9580790B2 (en) 2006-12-22 2017-02-28 Iap Research, Inc. System and method for surface hardening of refractory metals
US10031113B2 (en) 2007-02-28 2018-07-24 Waters Technologies Corporation Liquid-chromatography apparatus having diffusion-bonded titanium components
JP5977669B2 (ja) * 2012-12-28 2016-08-24 株式会社セブン・セブン 真空断熱二重容器の製造方法

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US2804410A (en) * 1953-10-27 1957-08-27 Nat Lead Co Method for nitriding titanium surfaces
CH650532A5 (de) * 1982-09-07 1985-07-31 Ver Drahtwerke Ag Verfahren zur bildung einer haerteschicht im bauteil aus elementen der vierten, fuenften oder sechsten nebengruppen des periodischen systems oder deren legierungen.

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100537805C (zh) * 2007-10-30 2009-09-09 沈阳宝鼎化工设备制造有限公司 耐磨、耐腐蚀备件及其表面处理工艺

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ATE135058T1 (de) 1996-03-15
ES2085320T3 (es) 1996-06-01
NO905209D0 (no) 1990-11-30
AU6760290A (en) 1992-01-09
CN1057866A (zh) 1992-01-15
DE4021286C1 (zh) 1991-02-21
CZ279472B6 (cs) 1995-05-17
DE59010178D1 (de) 1996-04-11
NO905209L (no) 1992-01-06
EP0464265B1 (de) 1996-03-06
PL166281B1 (pl) 1995-04-28
CS198891A3 (en) 1992-02-19
EP0464265A1 (de) 1992-01-08
RU1836484C (ru) 1993-08-23
JPH0649924B2 (ja) 1994-06-29
PT98195A (pt) 1992-04-30
PL290931A1 (en) 1992-10-05
TW208721B (zh) 1993-07-01
AU627960B2 (en) 1992-09-03
JPH04232247A (ja) 1992-08-20
BR9101899A (pt) 1992-01-14

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