CN103866243A - Preparation method for nitrogen oxygen titanium aluminum/titanium aluminum nitrogen and titanium aluminum composite film - Google Patents
Preparation method for nitrogen oxygen titanium aluminum/titanium aluminum nitrogen and titanium aluminum composite film Download PDFInfo
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- CN103866243A CN103866243A CN201410124720.9A CN201410124720A CN103866243A CN 103866243 A CN103866243 A CN 103866243A CN 201410124720 A CN201410124720 A CN 201410124720A CN 103866243 A CN103866243 A CN 103866243A
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Abstract
The invention discloses a preparation method for a nitrogen oxygen titanium aluminum/titanium aluminum nitrogen and titanium aluminum composite film. The preparation method sequentially comprises the following steps: 1, Determining a precipitation technology and target components; 2, selecting and pretreating a substrate workpiece; 3, determining the suspension position of the substrate workpiece; 4, performing vacuum heating treatment; 5, determining a pre-bombardment process; 6, determining a precipitation process. According to the preparation method, the adhesive force between the film and a substrate can be improved, the hardness of the film can be improved, and excellent stability and repeatability can be achieved.
Description
Technical field
The present invention relates to a kind of preparation method of oxynitride composite membrane, particularly adopt multiple reactant gases to prepare the method for multi-arc ion coating oxynitride composite membrane, such as the preparation method of nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane.
Background technology
Multi-arc ion coating is a kind of physical vacuum deposition technique that is provided with the multiple cathodic arc evaporation sources that can simultaneously evaporate, has the distinguishing features such as sedimentation velocity is fast, morphology is fine and close, strong adhesion, good uniformity.TiAlN be a kind ofly there is higher hardness, compared with the film material of high-wearing feature, its hardness and wear resistance are all apparently higher than traditional titanium nitride (TiN) rete.And existing nitrogen oxygen titanium aluminium (TiAlON) rete is as solar selectively absorbing coating, there is higher specific absorption and lower infrared reflectance in visible-near infrared district.But this film hardness is generally lower, generally poor with the sticking power of matrix.The present invention adopts multi sphere ion plating technology to prepare nitrogen oxygen titanium aluminium/TiAlN/titanium aluminium (TiAlON/TiAlN/TiAl) composite membrane, can effectively improve film hardness, increases the sticking power between rete and matrix, thereby rete mechanical property is improved.
Summary of the invention
The object of this invention is to provide the preparation method of a kind of nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane (TiAlON/TiAlN/TiAl), the method has improved the sticking power between rete and matrix, improve film hardness simultaneously, and there is satisfactory stability and repeatability.
Technical scheme of the present invention is: a kind of preparation method of nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane comprises successively:
1, determining of deposition technique and target composition: determine the technology of preparing of multi-arc ion coating as nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, select the commercial titanium-aluminum alloy target that a purity is 99.9% to deposit, the atomic ratio of titanium-aluminum alloy target is Ti:Al=50:50.
2, the selection of matrix workpiece and pre-treatment: select the sheet material of commercial rapid steel 2 ~ 3 mm thick as matrix workpiece material, carry out before plated film putting into coating chamber, use metal detergent matrix workpiece to be carried out to routine is deoiled, decontamination is processed and carry out surface finish processing, finally carry out ultrasonic cleaning with acetone and ethanol respectively, hair dryer dries up with for subsequent use.
3, determining of matrix workpiece suspension orientation: the sheet material matrix workpiece of 2 ~ 3 cleaned mm thick is hanging and placing apart from right on, titanium-aluminum alloy target surface approximately 23 ~ 25 centimeters, matrix workpiece suspension 23 ~ 25 centimeters on titanium-aluminum alloy target central axis are that the center of circle, radius are in the border circular areas that is parallel to titanium-aluminum alloy target surface of 15 centimetres, matrix workpiece surface is approximate is parallel to titanium-aluminum alloy target surface, and two surperficial angles are less than 15 degree.
4, vacuum heating treatment: matrix workpiece type of heating adopts electric heating element Baking out, reaches 3.5 × 10 in coating chamber back end vacuum
-2when handkerchief, start workpiece heating, heat-up rate remains on 3 ~ 5 ° of C/ minute, can reach 180 ° of C after 50 minutes.
5, bombard in advance determining of technique: refer to the ion bombardment technique of carrying out for obtaining multi-arc ion coating nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane before deposition, when coating chamber back end vacuum tightness reaches 8.0 × 10
-3handkerchief, temperature are filled with argon gas while reaching 180 ° of C, make coating chamber vacuum tightness reach 2.0 × 10
-1handkerchief, opens arc source, keeps arc current at 52 ~ 53 amperes, carries out ion bombardment, and bombardment bias voltage keeps 300 volts to bombard 5 minutes, and bombardment bias voltage keeps 350 volts to bombard 5 minutes.
6, determining of depositing operation: refer to the depositing operation that adopts for obtaining multi-arc ion coating nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, coating process is divided into three phases.The first step, remains on 2.0 × 10 by the ar pressure in coating chamber
-1handkerchief, the arc current of titanium-aluminum alloy target is placed in 52 amperes, and workpiece bias is 150 ~ 160 volts, depositing time 5 minutes; Second step, closes argon gas entrance, and making argon flow amount is 0, and partial pressure of ar gas is 0, in coating chamber, passes into nitrogen, makes its partial pressure reach 2.0 × 10
-1handkerchief.The arc current of titanium-aluminum alloy target is placed in 55 amperes, and workpiece bias is 150 ~ 160 volts, depositing time 5 minutes.The 3rd step passes into oxygen in coating chamber, makes its partial pressure reach (0.4 ~ 0.5) × 10
-1handkerchief; Adjust nitrogen flow simultaneously, make mixed gas total pressure remain on 2.0 × 10
-1handkerchief, the arc current of titanium-aluminum alloy target is placed in 55 amperes, and workpiece bias is 150 ~ 160 volts, depositing time 20 minutes.According to employing proposed by the invention take nitrogen, oxygen as reactant gases, take titanium-aluminum alloy target as arc evaporation source, prepare the method for multi-arc ion coating nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, can obtain above-mentioned nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane.
Compared with the existing technology, the present invention has determined the technology of preparing of conventional general multi-arc ion coating as nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, determine that commercial titanium-aluminum alloy target is as arc source, avoided special smelting, prepared the limitation of titanium-aluminum alloy target, reduced coating cost; The present invention has determined target composition, quantity and configuration orientation, determine that commercial rapid steel is as workpiece material, workpiece pre-treating technology and depositing operation are determined, when having guaranteed rete high adhesive force (3200N), high rigidity (HV3800 ~ HV4200), realize, and there is satisfactory stability and repeatability, thereby in the work-ing life that is more conducive to improve nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, make this rete be more suitable for the application in solar absorption field.
Embodiment
embodiment 1
At upper nitrogen oxygen titanium aluminium/TiAlN/titanium aluminium processed (TiAlON/TiAlN/TiAl) composite membrane of commercial rapid steel (W18Cr4V), its method is:
1, determining of deposition technique and target composition: determine the technology of preparing of multi-arc ion coating as nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, select the commercial titanium-aluminum alloy target that a purity is 99.9% to deposit, the atomic ratio of titanium-aluminum alloy target is Ti:Al=50:50.
2, the selection of matrix workpiece and pre-treatment: select the sheet material of commercial rapid steel (W18Cr4V) 2 mm thick as matrix workpiece material, carry out before plated film putting into coating chamber, use metal detergent matrix workpiece to be carried out to routine is deoiled, decontamination is processed and carry out surface finish processing, finally carry out ultrasonic cleaning with acetone and ethanol respectively, hair dryer dries up with for subsequent use.
3, determining of matrix workpiece suspension orientation: the sheet material matrix workpiece of 2 cleaned mm thick is hanging and placing apart from right on, titanium-aluminum alloy target surface approximately 23 centimeters, matrix workpiece suspension take 23 centimeters on titanium-aluminum alloy target central axis as the center of circle, radius is in the border circular areas that is parallel to titanium-aluminum alloy target surface of 15 centimetres, matrix workpiece surface is approximate is parallel to titanium-aluminum alloy target surface, and two surperficial angles are less than 15 degree.
4, vacuum heating treatment: matrix workpiece type of heating adopts electric heating element Baking out, reaches 3.5 × 10 in coating chamber back end vacuum
-2when handkerchief, start workpiece heating, heat-up rate remains on 3 ~ 5 ° of C/ minute, can reach 180 ° of C after 50 minutes.
5, bombard in advance determining of technique: refer to the ion bombardment technique of carrying out for obtaining multi-arc ion coating nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane before deposition, when coating chamber back end vacuum tightness reaches 8.0 × 10
-3handkerchief, temperature are filled with argon gas while reaching 180 ° of C, make coating chamber vacuum tightness reach 2.0 × 10
-1handkerchief, opens arc source, keeps arc current at 52 ~ 53 amperes, carries out ion bombardment, and bombardment bias voltage keeps 300 volts to bombard 5 minutes, and bombardment bias voltage keeps 350 volts to bombard 5 minutes.
6, determining of depositing operation: refer to the depositing operation that adopts for obtaining multi-arc ion coating nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, coating process is divided into three phases.The first step, remains on 2.0 × 10 by the ar pressure in coating chamber
-1handkerchief, the arc current of titanium-aluminum alloy target is placed in 52 amperes, and workpiece bias is 150 volts, depositing time 5 minutes; Second step, closes argon gas entrance, and making argon flow amount is 0, and partial pressure of ar gas is 0, in coating chamber, passes into nitrogen, makes its partial pressure reach 2.0 × 10
-1handkerchief.The arc current of titanium-aluminum alloy target is placed in 55 amperes, and workpiece bias is 150 volts, depositing time 5 minutes.The 3rd step passes into oxygen in coating chamber, makes its partial pressure reach 0.4 × 10
-1handkerchief; Adjust nitrogen flow simultaneously, make mixed gas total pressure remain on 2.0 × 10
-1handkerchief, the arc current of titanium-aluminum alloy target is placed in 55 amperes, and workpiece bias is 150 volts, depositing time 20 minutes.
According to employing proposed by the invention take nitrogen, oxygen as reactant gases, take titanium-aluminum alloy target as arc evaporation source, prepare the method for multi-arc ion coating nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, can obtain above-mentioned nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, this nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane has following features: strong adhesion (3200N), hardness high (HV4200).
embodiment 2
At upper nitrogen oxygen titanium aluminium/TiAlN/titanium aluminium processed (TiAlON/TiAlN/TiAl) composite membrane of commercial rapid steel (W18Cr4V), its method is:
1, determining of deposition technique and target composition: determine the technology of preparing of multi-arc ion coating as nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, select the commercial titanium-aluminum alloy target that a purity is 99.9% to deposit, the atomic ratio of titanium-aluminum alloy target is Ti:Al=50:50.
2, the selection of matrix workpiece and pre-treatment: select the sheet material of commercial rapid steel (W18Cr4V) 3 mm thick as matrix workpiece material, carry out before plated film putting into coating chamber, use metal detergent matrix workpiece to be carried out to routine is deoiled, decontamination is processed and carry out surface finish processing, finally carry out ultrasonic cleaning with acetone and ethanol respectively, hair dryer dries up with for subsequent use.
3, determining of matrix workpiece suspension orientation: the sheet material matrix workpiece of 3 cleaned mm thick is hanging and placing apart from right on, titanium-aluminum alloy target surface approximately 25 centimeters, matrix workpiece suspension take 25 centimeters on titanium-aluminum alloy target central axis as the center of circle, radius is in the border circular areas that is parallel to titanium-aluminum alloy target surface of 15 centimetres, workpiece surface is approximate is parallel to titanium-aluminum alloy target surface, and two surperficial angles are less than 15 degree.
4, vacuum heating treatment: matrix workpiece type of heating adopts electric heating element Baking out, reaches 3.5 × 10 in coating chamber back end vacuum
-2when handkerchief, start workpiece heating, heat-up rate remains on 3 ~ 5 ° of C/ minute, can reach 180 ° of C after 50 minutes.
5, bombard in advance determining of technique: refer to the ion bombardment technique of carrying out for obtaining multi-arc ion coating nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane before deposition, when coating chamber back end vacuum tightness reaches 8.0 × 10
-3handkerchief, temperature are filled with argon gas while reaching 180 ° of C, make coating chamber vacuum tightness reach 2.0 × 10
-1handkerchief, opens arc source, keeps arc current at 52 ~ 53 amperes, carries out ion bombardment, and bombardment bias voltage keeps 300 volts to bombard 5 minutes, and bombardment bias voltage keeps 350 volts to bombard 5 minutes.
6, determining of depositing operation: refer to the depositing operation that adopts for obtaining multi-arc ion coating nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, coating process is divided into three phases.The first step, remains on 2.0 × 10 by the ar pressure in coating chamber
-1handkerchief, the arc current of titanium-aluminum alloy target is placed in 52 amperes, and workpiece bias is 160 volts, depositing time 5 minutes; Second step, closes argon gas entrance, and making argon flow amount is 0, and partial pressure of ar gas is 0, in coating chamber, passes into nitrogen, makes its partial pressure reach 2.0 × 10
-1handkerchief.The arc current of titanium-aluminum alloy target is placed in 55 amperes, and workpiece bias is 160 volts, depositing time 5 minutes.The 3rd step passes into oxygen in coating chamber, makes its partial pressure reach 0.5 × 10
-1handkerchief; Adjust nitrogen flow simultaneously, make mixed gas total pressure remain on 2.0 × 10
-1handkerchief, the arc current of titanium-aluminum alloy target is placed in 55 amperes, and workpiece bias is 160 volts, depositing time 20 minutes.
According to employing proposed by the invention take nitrogen, oxygen as reactant gases, take titanium-aluminum alloy target as arc evaporation source, prepare the method for multi-arc ion coating nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, can obtain above-mentioned nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, this nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane has following features: strong adhesion (3200N), hardness high (HV3950).
Claims (1)
1. the preparation method of nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, it is characterized in that: its preparation method comprises successively: (1), deposition technique and target composition determine: determine the technology of preparing of multi-arc ion coating as nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, select the commercial titanium-aluminum alloy target that a purity is 99.9% to deposit, the atomic ratio of titanium-aluminum alloy target is Ti:Al=50:50; (2), the selection of matrix workpiece and pre-treatment: select the sheet material of commercial rapid steel 2 ~ 3 mm thick as matrix workpiece material, carry out before plated film putting into coating chamber, use metal detergent matrix workpiece to be carried out to routine is deoiled, decontamination is processed and carry out surface finish processing, finally carry out ultrasonic cleaning with acetone and ethanol respectively, hair dryer dries up with for subsequent use; (3), determining of matrix workpiece suspension orientation: the sheet material matrix workpiece of 2 ~ 3 cleaned mm thick is hanging and placing apart from right on, titanium-aluminum alloy target surface approximately 23 ~ 25 centimeters, matrix workpiece suspension 23 ~ 25 centimeters on titanium-aluminum alloy target central axis are that the center of circle, radius are in the border circular areas that is parallel to titanium-aluminum alloy target surface of 15 centimetres, matrix workpiece surface is approximate is parallel to titanium-aluminum alloy target surface, and two surperficial angles are less than 15 degree; (4), vacuum heating treatment: matrix workpiece type of heating adopts electric heating element Baking out, reaches 3.5 × 10 in coating chamber back end vacuum
-2when handkerchief, start workpiece heating, heat-up rate remains on 3 ~ 5 ° of C/ minute, can reach 180 ° of C after 50 minutes; (5) bombard, in advance determining of technique: refer to the ion bombardment technique of carrying out for obtaining multi-arc ion coating nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane before deposition, when coating chamber back end vacuum tightness reaches 8.0 × 10
-3handkerchief, temperature are filled with argon gas while reaching 180 ° of C, make coating chamber vacuum tightness reach 2.0 × 10
-1handkerchief, opens arc source, keeps arc current at 52 ~ 53 amperes, carries out ion bombardment, and bombardment bias voltage keeps 300 volts to bombard 5 minutes, and bombardment bias voltage keeps 350 volts to bombard 5 minutes; (6), the determining of depositing operation: refer to the depositing operation that adopts for obtaining multi-arc ion coating nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, coating process is divided into three phases; The first step, remains on 2.0 × 10 by the ar pressure in coating chamber
-1handkerchief, the arc current of titanium-aluminum alloy target is placed in 52 amperes, and workpiece bias is 150 ~ 160 volts, depositing time 5 minutes; Second step, closes argon gas entrance, and making argon flow amount is 0, and partial pressure of ar gas is 0, in coating chamber, passes into nitrogen, makes its partial pressure reach 2.0 × 10
-1handkerchief; The arc current of titanium-aluminum alloy target is placed in 55 amperes, and workpiece bias is 150 ~ 160 volts, depositing time 5 minutes; The 3rd step passes into oxygen in coating chamber, makes its partial pressure reach (0.4 ~ 0.5) × 10
-1handkerchief; Adjust nitrogen flow simultaneously, make mixed gas total pressure remain on 2.0 × 10
-1handkerchief, the arc current of titanium-aluminum alloy target is placed in 55 amperes, and workpiece bias is 150 ~ 160 volts, depositing time 20 minutes; According to employing proposed by the invention take nitrogen, oxygen as reactant gases, take titanium-aluminum alloy target as arc evaporation source, prepare the method for multi-arc ion coating nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane, can obtain above-mentioned nitrogen oxygen titanium aluminium/TiAlN/titanium aluminum composite membrane.
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Cited By (6)
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| CN104831233A (en) * | 2015-03-27 | 2015-08-12 | 华南理工大学 | Decorative blue ceramic coating and preparation method thereof |
| CN105887013A (en) * | 2016-06-12 | 2016-08-24 | 沈阳大学 | Preparation method of titanium-zirconium nitride metal film for surface modification of nickel-titanium root canal file |
| CN105908136A (en) * | 2016-06-12 | 2016-08-31 | 沈阳大学 | Preparation method for modified metallic nitrogen-oxygen titanium-zirconium composite film on surface of nickel-titanium root canal file |
| CN105908131A (en) * | 2016-06-15 | 2016-08-31 | 中国科学院金属研究所 | TiAl coating capable of achieving heat growth of aluminum oxide film and preparing method of TiAl coating |
| CN106048525A (en) * | 2016-07-15 | 2016-10-26 | 沈阳大学 | Preparation method of titanium-chromium metal nitride composite hard film with continuous change |
| CN113151781A (en) * | 2021-03-23 | 2021-07-23 | 法德(浙江)机械科技有限公司 | Titanium aluminum nitride type superhard coating and preparation method thereof |
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| CN101709450A (en) * | 2009-11-30 | 2010-05-19 | 沈阳大学 | Method for preparing zirconium-titanium-aluminum-nitrogen nitride gradient hard reaction film |
| CN102062485A (en) * | 2010-11-19 | 2011-05-18 | 山东帅克新能源有限公司 | Heat collection plate of solar energy flat plate collector and film plating method for heat collection plate |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20060284237A1 (en) * | 2005-06-20 | 2006-12-21 | Jae-Hyun Park | Phase change memory cells having a cell diode and a bottom electrode self-aligned with each other and methods of fabricating the same |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104831233A (en) * | 2015-03-27 | 2015-08-12 | 华南理工大学 | Decorative blue ceramic coating and preparation method thereof |
| CN104831233B (en) * | 2015-03-27 | 2017-10-20 | 华南理工大学 | One kind decoration blue ceramic coating and preparation method thereof |
| CN105887013A (en) * | 2016-06-12 | 2016-08-24 | 沈阳大学 | Preparation method of titanium-zirconium nitride metal film for surface modification of nickel-titanium root canal file |
| CN105908136A (en) * | 2016-06-12 | 2016-08-31 | 沈阳大学 | Preparation method for modified metallic nitrogen-oxygen titanium-zirconium composite film on surface of nickel-titanium root canal file |
| CN105908131A (en) * | 2016-06-15 | 2016-08-31 | 中国科学院金属研究所 | TiAl coating capable of achieving heat growth of aluminum oxide film and preparing method of TiAl coating |
| CN105908131B (en) * | 2016-06-15 | 2018-09-04 | 中国科学院金属研究所 | It is a kind of can thermally grown oxide aluminium film TiAl coatings and preparation method thereof |
| CN106048525A (en) * | 2016-07-15 | 2016-10-26 | 沈阳大学 | Preparation method of titanium-chromium metal nitride composite hard film with continuous change |
| CN106048525B (en) * | 2016-07-15 | 2018-10-30 | 沈阳大学 | A kind of preparation method of the titanium chromium metal nitride composite ganoine film of consecutive variations |
| CN113151781A (en) * | 2021-03-23 | 2021-07-23 | 法德(浙江)机械科技有限公司 | Titanium aluminum nitride type superhard coating and preparation method thereof |
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