CN111893439A - Method for preparing personal ornaments with titanium nitride hard coating - Google Patents
Method for preparing personal ornaments with titanium nitride hard coating Download PDFInfo
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- CN111893439A CN111893439A CN202010803647.3A CN202010803647A CN111893439A CN 111893439 A CN111893439 A CN 111893439A CN 202010803647 A CN202010803647 A CN 202010803647A CN 111893439 A CN111893439 A CN 111893439A
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- titanium nitride
- substrate sample
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- hard coating
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
-
- 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
-
- 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
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a preparation method of a personal ornament with a titanium nitride hard coating, which comprises the following steps: step 1: carrying out ultrasonic cleaning on a substrate sample, blowing dry moisture on the surface of the substrate sample by using high-pressure nitrogen, putting the substrate sample into a dryer, and putting the substrate sample into a vacuum coating chamber after the sample is completely dried; step 2: the vacuum coating chamber is preheated by a diffusion pump, then is vacuumized, and is further heated by a heater; and step 3: cleaning and etching the surface of the matrix sample by using argon ions; and 4, step 4: the titanium is evaporated and ionized and is plated on the substrate sample. The titanium nitride prepared by the invention has uniform coating thickness, compact structure and no defect, the coating is tightly combined with the matrix, the crystal grains are uniform, compact columnar crystals are formed, the titanium nitride can play a good protection role on personal ornaments, and simultaneously, the wear resistance and the corrosion resistance of the personal ornaments are improved, and the service life of the titanium nitride is prolonged.
Description
Technical Field
The invention relates to the technical field of personal ornaments, in particular to a preparation method of a personal ornament with a titanium nitride hard coating.
Background
The origin of the ornaments, originally because of the shielding body, with the continuous development of the living level and the creativity of people, begins to be converted to the decoration part, and derives various decorations mainly based on the decoration. The ornaments are used for decoration and wearing, some ornaments can play roles of fragrance, cleanness, beautification and the like, good ornaments can enable a wearer to feel new and relaxed, a plurality of ornament boutiques on the street increasingly pay attention to the market of the ornaments, and the ornaments can not be separated from the ornaments in home decoration, birthday gifts, friends parties, men and women, and the like. The consumption trend of the ornament industry is as follows: the ornament industry is a new industry which is formed by separating and integrating the industries of jewelry and artworks gifts. Ornaments are used as growth points of new economy, and developed countries gradually mature. All grades of exclusive shops and point-of-sale chess cloth; various styles and various levels of products fully meet the increasing market demand. In China, the industry is still in the early development stage. With the leap development of social economy and culture, people step into a well-off type from a full-warm type, advocate humanity and fashion, continuously shape personality and charm, and become the pursuit of people.
The existing personal ornaments such as a gold watch and the like have the defects of low strength and no wear resistance, and the titanium nitride hard coating plated on the surface of the existing personal ornaments can effectively improve the strength and the wear resistance of the existing personal ornaments.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of a personal ornament with a titanium nitride hard coating, which aims to improve the strength and the wear resistance of the personal ornament and prolong the service life of the personal ornament.
A method for preparing a personal ornament with a titanium nitride hard coating comprises the following steps:
step 1: carrying out ultrasonic cleaning on a substrate sample, blowing dry moisture on the surface of the substrate sample by using high-pressure nitrogen, putting the substrate sample into a dryer, and putting the substrate sample into a vacuum coating chamber after the sample is completely dried;
step 2: the vacuum coating chamber is preheated by a diffusion pump, then is vacuumized, and is further heated by a heater;
and step 3: cleaning and etching the surface of the matrix sample by using argon ions;
and 4, step 4: the titanium is evaporated and ionized and is plated on the substrate sample.
Preferably, in the step 1, the substrate sample is subjected to ultrasonic cleaning for 10 min.
Preferably, in the step 2, the preheating time of the diffusion pump is 60min, and the heating time of the heater is 90 min.
Preferably, in the step 2, the vacuum-pumping treatment specifically comprises: firstly opening a pre-pumping valve to perform rough pumping on the vacuum chamber to 4-5 Pa, and then opening a front stage and a high valve to perform vacuum pumping to 5.5E-3 Pa.
Preferably, in the step 3, the bias voltage for cleaning and etching the surface of the substrate sample by the argon ions is-500V, and the etching time is 5 min.
Preferably, in the step 4, the arc source current is 70-150A, the pulse bias is 0-1000V, the direct current bias is 0-500V, the argon partial pressure is 1.3E-1Pa, the nitrogen partial pressure is 0.5E-1Pa, and the coating time is 50 min.
The invention has the beneficial effects that: the titanium nitride prepared by the invention has the advantages of uniform coating thickness, compact tissue and no defect, the coating is tightly combined with a matrix, the crystal grains are uniform, and compact columnar crystals are formed, the titanium nitride is a structural material with attractive golden yellow color, high melting point, high hardness, good chemical stability and small metal wetting, and has higher conductivity and superconductivity, the surface coating used for the personal ornament can play a good protection role, simultaneously the wear resistance and the corrosion resistance of the personal ornament are improved, the weight can be increased, and the service life of the personal ornament can be prolonged.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. Throughout the drawings, like elements or portions are generally identified by like reference numerals. In the drawings, elements or portions are not necessarily drawn to scale.
FIG. 1 is an electron microscope image of the fracture structure of the personal ornaments with the titanium nitride hard coating prepared in example 1 of the invention;
FIG. 2 is an electron microscope image of the fracture structure of the personal ornaments with the titanium nitride hard coating prepared in example 2 of the invention;
FIG. 3 is an electron microscope image of the fracture structure of the personal ornaments with the titanium nitride hard coating prepared in example 3 of the invention;
FIG. 4 is an XRD analysis of a personal ornament having a titanium nitride hard coating made in accordance with example 1 of the present invention;
FIG. 5 is an XRD analysis of a personal ornament having a titanium nitride hard coating made in accordance with example 2 of the present invention;
FIG. 6 is an XRD analysis of a personal ornament having a titanium nitride hard coating made in accordance with example 3 of the present invention;
FIG. 7 is a scanning spectrum of a personal ornament having a titanium nitride hard coating layer prepared in example 1 of the present invention;
FIG. 8 is a scanned spectrum of a personal ornament having a titanium nitride hard coating made in accordance with example 2 of the present invention;
FIG. 9 is a scanned spectrum of a personal ornament having a titanium nitride hard coating made in accordance with example 3 of the present invention;
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
Example 1
A method for preparing a personal ornament with a titanium nitride hard coating comprises the following steps:
step 1: firstly, fixing a substrate sample on a clamp, adding a special detergent solution into ultrasonic equipment, heating to about 60 ℃, then cleaning the substrate sample in ultrasonic for 10min, removing dust, grease, sweat stains, surface oxidation films, adsorbed gas, burrs and the like on the surface of the substrate to ensure the bonding strength and purity of a coating, blowing off water on the surface of the substrate sample by using high-pressure nitrogen, then placing the substrate sample into a dryer, and after the sample is completely dried, placing the substrate sample into a vacuum coating chamber;
step 2: the method comprises the following steps of utilizing a diffusion pump to conduct primary preheating on a vacuum coating chamber for 60min, and then conducting vacuumizing treatment on the vacuum coating chamber, wherein the vacuumizing treatment specifically comprises the following steps: firstly opening a pre-pumping valve to perform rough pumping on a vacuum chamber to 4-5 Pa, then opening a front stage and a high valve to perform vacuum pumping to 5.5E-3Pa, and further heating for 90min by using a heater;
and step 3: cleaning and etching the surface of the matrix sample by argon ions, wherein the bias voltage is-500V, and the etching time is 5 min;
and 4, step 4: titanium is evaporated and ionized and is plated on a substrate sample, wherein: the arc source current is 110A, the pulse bias is 300V, the direct current bias is 200V, the argon partial pressure is 1.3E-1Pa, the nitrogen partial pressure is 0.5E-1Pa, and the coating time is 50 min.
Example 2
A method for preparing a personal ornament with a titanium nitride hard coating comprises the following steps:
step 1: firstly, fixing a substrate sample on a clamp, adding a special detergent solution into ultrasonic equipment, heating to about 60 ℃, then cleaning the substrate sample in ultrasonic for 10min, removing dust, grease, sweat stains, surface oxidation films, adsorbed gas, burrs and the like on the surface of the substrate to ensure the bonding strength and purity of a coating, blowing off water on the surface of the substrate sample by using high-pressure nitrogen, then placing the substrate sample into a dryer, and after the sample is completely dried, placing the substrate sample into a vacuum coating chamber;
step 2: the method comprises the following steps of utilizing a diffusion pump to conduct primary preheating on a vacuum coating chamber for 60min, and then conducting vacuumizing treatment on the vacuum coating chamber, wherein the vacuumizing treatment specifically comprises the following steps: firstly opening a pre-pumping valve to perform rough pumping on a vacuum chamber to 4-5 Pa, then opening a front stage and a high valve to perform vacuum pumping to 5.5E-3Pa, and further heating for 90min by using a heater;
and step 3: cleaning and etching the surface of the matrix sample by argon ions, wherein the bias voltage is-500V, and the etching time is 5 min;
and 4, step 4: titanium is evaporated and ionized and is plated on a substrate sample, wherein: the arc source current is 110A, the pulse bias is 300V, the direct current bias is 150V, the argon partial pressure is 1.3E-1Pa, the nitrogen partial pressure is 0.5E-1Pa, and the coating time is 50 min.
Example 3
A method for preparing a personal ornament with a titanium nitride hard coating comprises the following steps:
step 1: firstly, fixing a substrate sample on a clamp, adding a special detergent solution into ultrasonic equipment, heating to about 60 ℃, then cleaning the substrate sample in ultrasonic for 10min, removing dust, grease, sweat stains, surface oxidation films, adsorbed gas, burrs and the like on the surface of the substrate to ensure the bonding strength and purity of a coating, blowing off water on the surface of the substrate sample by using high-pressure nitrogen, then placing the substrate sample into a dryer, and after the sample is completely dried, placing the substrate sample into a vacuum coating chamber;
step 2: the method comprises the following steps of utilizing a diffusion pump to conduct primary preheating on a vacuum coating chamber for 60min, and then conducting vacuumizing treatment on the vacuum coating chamber, wherein the vacuumizing treatment specifically comprises the following steps: firstly opening a pre-pumping valve to perform rough pumping on a vacuum chamber to 4-5 Pa, then opening a front stage and a high valve to perform vacuum pumping to 5.5E-3Pa, and further heating for 90min by using a heater;
and step 3: cleaning and etching the surface of the matrix sample by argon ions, wherein the bias voltage is-500V, and the etching time is 5 min;
and 4, step 4: titanium is evaporated and ionized and is plated on a substrate sample, wherein: the arc source current is 110A, the pulse bias is 300V, the direct current bias is 100V, the argon partial pressure is 1.3E-1Pa, the nitrogen partial pressure is 0.5E-1Pa, and the coating time is 50 min.
Fracture scanning analysis is carried out on the personal ornaments with the titanium nitride hard coatings prepared in the examples 1 to 3 through a Scanning Electron Microscope (SEM), and the TiN coatings prepared through the fracture scanning analysis are uniform in thickness, compact in structure and free of defects as shown in figures 1 to 3. The coating is tightly combined with the matrix, the crystal grains are uniform, and compact columnar crystals are formed. The coating thickness increased with increasing bias and arc current, with the coating being the thickest, 5.8 μm, at an arc of 110A, a pulse bias of 300V, and a DC bias of 200V.
And analyzing the phase structure of the coating by using an X-ray diffraction analyzer. As shown in fig. 4 to 6, XRD analysis results showed that the coating was mainly composed of TiN, and that the major three diffraction peaks of TiN corresponded to (111), (220), and (311), and that XRD results showed that the major preferred orientation plane of TiN was (111). TiN is a face-centered cubic structure, and (111) is a close-packed surface, so that the higher the bias voltage is, the more obvious the orientation of the (111) crystal plane is. The increase of the bias voltage increases the energy of incident particles, the particles migrate more sufficiently on the surface and are easier to stack in a close-packed plane manner, and thus the diffraction peak of the (111) crystal plane, which mainly appears under the bias voltage, is increased. It was found by comparing the metallographic results that the higher the bias, the smoother the coating surface, which is related to the migration ability of the surface particles. Under different biases, TiN diffraction peaks have different displacements, which can be presumed as stress-induced displacements, the incident particle capacity is increased along with the increase of the bias, and under the action of particle bombardment, more crystal defects are formed, so that the internal stress is increased.
By energy spectrum analysis of a scanning electron microscope, as shown in fig. 7-9, according to the energy spectrum analysis, the main elements of the coating are composed of Ti and N, and a small amount of W and Co. The atomic number ratio of Ti to N was close to 1:1, and the results of the phase analysis by XRD were obtained.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (6)
1. A method for preparing a personal ornament with a titanium nitride hard coating is characterized by comprising the following steps: the method comprises the following steps:
step 1: carrying out ultrasonic cleaning on a substrate sample, blowing dry moisture on the surface of the substrate sample by using high-pressure nitrogen, putting the substrate sample into a dryer, and putting the substrate sample into a vacuum coating chamber after the sample is completely dried;
step 2: the vacuum coating chamber is preheated by a diffusion pump, then is vacuumized, and is further heated by a heater;
and step 3: cleaning and etching the surface of the matrix sample by using argon ions;
and 4, step 4: the titanium is evaporated and ionized and is plated on the substrate sample.
2. The method of making a personal ornament having a titanium nitride hard coating according to claim 1, wherein: in the step 1, the substrate sample is subjected to ultrasonic cleaning for 10 min.
3. The method of making a personal ornament having a titanium nitride hard coating according to claim 1, wherein: in the step 2, the preheating time of the diffusion pump is 60min, and the heating time of the heater is 90 min.
4. The method of making a personal ornament having a titanium nitride hard coating according to claim 1, wherein: in the step 2, the vacuum-pumping treatment specifically comprises the following steps: firstly opening a pre-pumping valve to perform rough pumping on the vacuum chamber to 4-5 Pa, and then opening a front stage and a high valve to perform vacuum pumping to 5.5E-3 Pa.
5. The method of making a personal ornament having a titanium nitride hard coating according to claim 1, wherein: in the step 3, the bias voltage for cleaning and etching the surface of the matrix sample by the argon ions is-500V, and the etching time is 5 min.
6. The method of making a personal ornament having a titanium nitride hard coating according to claim 1, wherein: in the step 4, the arc source current is 70-150A, the pulse bias is 0-1000V, the direct current bias is 0-500V, the argon partial pressure is 1.3E-1Pa, the nitrogen partial pressure is 0.5E-1Pa, and the coating time is 50 min.
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| CN202010803647.3A CN111893439A (en) | 2020-08-11 | 2020-08-11 | Method for preparing personal ornaments with titanium nitride hard coating |
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| CN202010803647.3A CN111893439A (en) | 2020-08-11 | 2020-08-11 | Method for preparing personal ornaments with titanium nitride hard coating |
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Citations (6)
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|---|---|---|---|---|
| JPS62199763A (en) * | 1986-02-25 | 1987-09-03 | Matsushita Electric Works Ltd | Formation of tin film |
| CN1281057A (en) * | 1999-10-11 | 2001-01-24 | 中国科学院力学研究所 | Equipment and process for preparing film by pulse aided filter and arc deposition |
| CN104278235A (en) * | 2013-07-12 | 2015-01-14 | 重庆文理学院 | Cutter with titanium nitride ceramic membrane and preparation method of cutter |
| CN105779936A (en) * | 2016-01-20 | 2016-07-20 | 北京师范大学 | Super-thick TiN film layer preparation method capable of maintaining super-hard characteristic and improving toughness at the same time |
| CN105887159A (en) * | 2016-05-12 | 2016-08-24 | 广东省材料与加工研究所 | Method for preparing magnesium alloy composite coating with decorativeness and functionality |
| CN111041429A (en) * | 2019-12-25 | 2020-04-21 | 上海子创镀膜技术有限公司 | Champagne toning technology combining multi-arc technology and magnetic control technology |
-
2020
- 2020-08-11 CN CN202010803647.3A patent/CN111893439A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62199763A (en) * | 1986-02-25 | 1987-09-03 | Matsushita Electric Works Ltd | Formation of tin film |
| CN1281057A (en) * | 1999-10-11 | 2001-01-24 | 中国科学院力学研究所 | Equipment and process for preparing film by pulse aided filter and arc deposition |
| CN104278235A (en) * | 2013-07-12 | 2015-01-14 | 重庆文理学院 | Cutter with titanium nitride ceramic membrane and preparation method of cutter |
| CN105779936A (en) * | 2016-01-20 | 2016-07-20 | 北京师范大学 | Super-thick TiN film layer preparation method capable of maintaining super-hard characteristic and improving toughness at the same time |
| CN105887159A (en) * | 2016-05-12 | 2016-08-24 | 广东省材料与加工研究所 | Method for preparing magnesium alloy composite coating with decorativeness and functionality |
| CN111041429A (en) * | 2019-12-25 | 2020-04-21 | 上海子创镀膜技术有限公司 | Champagne toning technology combining multi-arc technology and magnetic control technology |
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| Title |
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| 陈甥怡: "氮化钛硬质薄膜抗氧化性能研究", 《中国优秀硕士论文全文数据库（电子期刊）》 * |
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