EP0190179A1 - Verfahren zur verbesserung des farbeindrucks von titannitridschichten - Google Patents
Verfahren zur verbesserung des farbeindrucks von titannitridschichtenInfo
- Publication number
- EP0190179A1 EP0190179A1 EP19850903273 EP85903273A EP0190179A1 EP 0190179 A1 EP0190179 A1 EP 0190179A1 EP 19850903273 EP19850903273 EP 19850903273 EP 85903273 A EP85903273 A EP 85903273A EP 0190179 A1 EP0190179 A1 EP 0190179A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- coating
- titanium nitride
- nitride layers
- improving
- hydrocarbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 238000000034 method Methods 0.000 title claims abstract description 28
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 title claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000576 coating method Methods 0.000 claims abstract description 19
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 14
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 7
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000011248 coating agent Substances 0.000 claims description 14
- 239000004215 Carbon black (E152) Substances 0.000 claims description 9
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000000151 deposition Methods 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 230000008021 deposition Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 150000002835 noble gases Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000010939 rose gold Substances 0.000 description 1
- 229910001112 rose gold Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
Classifications
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the layer
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
-
- G—PHYSICS
- G04—HOROLOGY
- G04B—MECHANICALLY-DRIVEN CLOCKS OR WATCHES; MECHANICAL PARTS OF CLOCKS OR WATCHES IN GENERAL; TIME PIECES USING THE POSITION OF THE SUN, MOON OR STARS
- G04B37/00—Cases
- G04B37/22—Materials or processes of manufacturing pocket watch or wrist watch cases
Definitions
- the invention relates to a method for improving the color impression of titanium nitride layers by means of plasma-supported coating methods, in particular by means of
- Magnetron nuts using a process gas consisting of an inert gas and nitrogen.
- Decorative hard material coatings made of titanium nitride on substrates made of any material such as plastic, ceramic, metal or metal alloy can be deposited using physical coating methods such as magnetron sputtering or ion plating.
- the color scale of such layers ranges from white to yellow to rose gold. Compared to pure gold layers, however, gold-colored titanium nitride layers are generally perceived as cold. This fact is very disruptive when using titanium nitride for decorative applications, especially as a gold substitute.
- the color impression of the titanium nitride layers can be influenced by varying the process conditions such as bias voltage and temperature.
- the morphology of the layer is also changed.
- the temperature is higher, so the layers show an undesirably stalky appearance.
- Titanium nitride layers are desired that have the outstanding physical and chemical properties of titanium nitride such as great hardness and thus high scratch resistance and corrosion resistance and also show a warm gold color.
- the subjective impression of a warm gold color is created e.g. B. by increasing the red value or by reducing the proportion of green, ie the black haze of the layer. This is not achieved by simply increasing the nitrogen content in the titanium nitride layer, since the associated increase in the red value always goes hand in hand with a decrease in the yellow content. Therefore, reddish-brown layers are increasingly obtained.
- the object of the invention is to increase the red value of titanium nitride layers by a simple variation of the coating conditions, or to reduce the proportion of green without influencing the yellow value of the layer. Furthermore, the process should not cause any change in the physical and chemical properties, in particular the corrosion resistance and the scratch resistance of the titanium nitride.
- This object is achieved in that carbon is introduced into the reaction space between a target and a substrate to be coated and. that the coating is carried out at substrate temperatures of less than 250 ° C, and that the properties of the layer depend on the substrate temperature and
- Bias voltage and the color impression can be adjusted via the carbon content. Preferred embodiments of the method according to the invention are described in subclaims 2 to 11.
- the titanium nitride layers are deposited in a manner known per se by plasma-assisted deposition methods in a vacuum coating apparatus, preferably by magnetron sputtering.
- a hydrocarbon is admitted to the process gases argon and nitrogen which are usually used. All saturated and unsaturated substituted or unsubstituted hydrocarbons with 1 to 6, preferably 1 to 3, carbon atoms are suitable.
- the reaction conditions, in particular the bias voltage and the temperature of the substrate, are set to values favorable for advantageous properties of use of the layer, such as adhesion, homogeneity and unity.
- the red value of the deposited titanium nitride layers depends sensitively on the flow rate of the hydrocarbon introduced into the apparatus.
- low substrate temperatures of less than 250 ° C, preferably 20 to 200 ° C, are used.
- the flow rates of the hydrocarbons added to influence the color impression are between about 0.05 and 1 cm 3 / min.
- carbon is supplied by using a titanium carbide target instead of a pure titanium target.
- a titanium carbide target instead of a pure titanium target.
- noble gases preferably argon
- nitrogen are used as process gases.
- the flow rate of the nitrogen can also be continuously reduced or increased from about the middle of the total coating time or towards the end of the coating, as a result of which the layer only has the desired color on the surface.
- the coating is typically carried out at a residual gas pressure of less than 2.10 -6 torr.
- Deposition rates are between 1 0 and 20 ⁇ / sec. , preferably 1 5 ⁇ / sec.
- the argon flow rate is e.g. B. 1 0, 5 to 1 3, 5 cm 3 / min. who have favourited Sticks toff flow rate e.g. B. 2 to 1 0 cm 3 / min.
- the flow rate of the hydrocarbon can be between 0.05 and 1 cm 3 / min. vary.
- a gold-colored titanium nitride layer is obtained by reactive magnetron sputtering of a pure titanium target on a stainless steel workpiece.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Physical Vapour Deposition (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3425467 | 1984-07-11 | ||
| DE19843425467 DE3425467A1 (de) | 1984-07-11 | 1984-07-11 | Verfahren zur verbesserung des farbeindrucks von titannitrid-schichten |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP0190179A1 true EP0190179A1 (de) | 1986-08-13 |
Family
ID=6240323
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP19850903273 Withdrawn EP0190179A1 (de) | 1984-07-11 | 1985-07-04 | Verfahren zur verbesserung des farbeindrucks von titannitridschichten |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP0190179A1 (enrdf_load_stackoverflow) |
| DE (1) | DE3425467A1 (enrdf_load_stackoverflow) |
| WO (1) | WO1986000649A1 (enrdf_load_stackoverflow) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039354C (zh) * | 1989-08-21 | 1998-07-29 | 巴尔策斯有限公司 | 带有固溶体涂镀层的工件及其生产方法、生产设备和应用 |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3890319C2 (de) * | 1987-04-23 | 1994-08-25 | Nisshin Steel Co Ltd | Dekorative Platte als Baumaterial |
| CA1296289C (en) * | 1987-06-30 | 1992-02-25 | Inco Limited | Process for producing gold-colored coinage |
| DE3726731A1 (de) * | 1987-08-11 | 1989-02-23 | Hartec Ges Fuer Hartstoffe Und | Verfahren zum aufbringen von ueberzuegen auf gegenstaende mittels magnetfeldunterstuetzter kathodenzerstaeubung im vakuum |
| DE4020595A1 (de) * | 1990-06-28 | 1992-01-09 | Patent Treuhand Ges Fuer Elektrische Gluehlampen Mbh | Elektrische lampe mit lichtreflektierender schicht |
| DE4205017A1 (de) * | 1992-02-19 | 1993-08-26 | Leybold Ag | Verfahren zur erzeugung einer dekorativen goldlegierungsschicht |
| CN108505004A (zh) * | 2018-05-04 | 2018-09-07 | 武汉理工大学 | 带有彩色TiN涂层的不锈钢刀具制备方法 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1951362B2 (de) * | 1969-10-11 | 1971-12-02 | W.C. Heraeus Gmbh, 6450 Hanau | Verfahren zum ueberziehen einer schreibfeder mit einer schicht aus hartstoff |
| BE787599A (fr) * | 1971-08-16 | 1973-02-16 | Battelle Memorial Institute | Vitrage filtrant antisolaire et isolant thermique |
| CH624817B (de) * | 1979-09-04 | Balzers Hochvakuum | Verfahren zur herstellung goldfarbener ueberzuege. |
-
1984
- 1984-07-11 DE DE19843425467 patent/DE3425467A1/de active Granted
-
1985
- 1985-07-04 WO PCT/EP1985/000324 patent/WO1986000649A1/de unknown
- 1985-07-04 EP EP19850903273 patent/EP0190179A1/de not_active Withdrawn
Non-Patent Citations (1)
| Title |
|---|
| See references of WO8600649A1 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039354C (zh) * | 1989-08-21 | 1998-07-29 | 巴尔策斯有限公司 | 带有固溶体涂镀层的工件及其生产方法、生产设备和应用 |
Also Published As
| Publication number | Publication date |
|---|---|
| DE3425467A1 (de) | 1986-01-23 |
| DE3425467C2 (enrdf_load_stackoverflow) | 1988-06-30 |
| WO1986000649A1 (en) | 1986-01-30 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
| AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AT BE CH DE FR GB IT LI LU NL SE |
|
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN |
|
| 18D | Application deemed to be withdrawn |
Effective date: 19860612 |
|
| RIN1 | Information on inventor provided before grant (corrected) |
Inventor name: STEININGER, HELMUT Inventor name: ETZKORN, HEINZ-WERNER |