CN102634755B - Compact nitride ceramic layer and preparation method thereof - Google Patents
Compact nitride ceramic layer and preparation method thereof Download PDFInfo
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- CN102634755B CN102634755B CN201210110473.8A CN201210110473A CN102634755B CN 102634755 B CN102634755 B CN 102634755B CN 201210110473 A CN201210110473 A CN 201210110473A CN 102634755 B CN102634755 B CN 102634755B
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Abstract
The invention discloses a compact nitride ceramic layer and a preparation method thereof. The preparation method comprises the following steps of: firstly cleaning the surface to be processed of a mechanical part; then preparing a nitride coating layer by a reaction deposition method, wherein the bias voltage changes alternatively between the high bias voltage and the lower bias voltage during the process for preparing the nitride coating layer by the reaction deposition method, the nitride coating layer has high hardness of 1700Hv-2600Hv and low stress of 0.1GPa-1GPa, the crystal grain proportion is 0-0.5, and the crystal grain size is about 10nm-200nm. The coating layer deposition technology provided by the invention is simple, the deposition speed rate is high, and the stress is low.
Description
technical field
The present invention relates to process for treating surface, particularly a kind of preparation method of fine and close nitride coatings, relates in particular to nitride coatings corrosion-resistant and diffusion barrier application.
background technology
Owing to having good hardness, unreactiveness, bio-compatibility and obstruction atomic diffusion performance, transition metal nitride coating is in tribology, biologic medical, corrosion-resistant and electron trade acquisition extensive application.But easily there is (111) preferred orientation in transition metal nitride in process of growth, (111) face of crystal grain is along coating normal direction Fast Growth, cause loose column crystal to produce, this will be unfavorable for the raising of coating hardness, erosion resistance and diffusion barrier performance.Conventionally adopt at present different methods to suppress the growth of column crystal: adding other element is a kind of effective ways, but the interpolation of the third composition may change original character of coating, and multi-source codeposition or adopt alloy deposition source must use special alloy target material or many targets codeposition, thereby this all can obviously improve process complexity increase cost; Improving deposited particles energy is also conventional way, by increasing coating structure defect, promotes forming core, crystal grain thinning, thus coating compactness extent improved, but the method is often brought larger stress, be unfavorable for coating bonding properties, and the method can reduce coating sedimentation rate, reduction production efficiency.Therefore obtain the fine and close nitride ceramics coating of high deposition rate low-stress very important in industrial production and practical application.
summary of the invention
The invention provides a kind of fine and close nitride ceramics coating and preparation method thereof, can take into account high deposition rate and low-stress.
Technical scheme of the present invention is: a kind of preparation method of fine and close nitride ceramics coating, cleans by the first pending surface to mechanical component; Pass through again reactive deposition legal system for nitride coatings, in the process of reactive deposition legal system for nitride coatings, be biased between high bias voltage and low bias voltage and alternately change.
Described high bias voltage is arbitrary in 0 ~-80V, and low bias voltage is arbitrary in-80 V ~-150V; The reaction times of each bias voltage is 1 minute-10 minutes.
Preferred scheme is: preparing the Ti that first adopts vapour deposition process to deposit 50 nm-200 nm thickness before nitride coatings or Cr middle layer in surface;
The fine and close nitride ceramics coating that the preparation method of the fine and close nitride ceramics coating based on described obtains, the higher hardness with 1700Hv-2600Hv of described nitride ceramics coating and the lower stress of 0.1 GPa-1GPa, crystal grain ratio is 0-0.5, and grain-size is about 10 nm-200nm.
beneficial effect:
(1) depositing operation is simple: as improved coating compactness by adding other elements, must use special alloy target material or many targets codeposition, this will make technical process complicated, and cost rises; And this technique is only carried out periodic adjustment to bias voltage in deposition process, do not need other complicated technologies, be easy to improve original technique, improve coating quality.
(2) high deposition rate: constant high bias voltage deposition, due to reverse sputtering effect, high-energy particle bombardment coatingsurface causes part deposited particles to depart from coating, and coating sedimentation rate reduces; And the present invention has reduced high bias voltage depositing time, be conducive to the raising of coating speed, thereby increase work efficiency, reduce job costs.
(3) low-stress: constant high bias voltage deposition process, high-energy particle bombardment coating, causes the generation of a large amount of defects, and stress obviously increases.When stress increase to a certain degree, coating will be peeled off inefficacy, even unstripped, the bonding properties of coating obviously declines, its application carrying scope reduces.For fear of peeling off, coat-thickness just must reduce, and this is also just unfavorable for its wear-resisting, anticorrosion and diffusion barrier performance.And adopt method of the present invention owing to having reduced high bias voltage deposition process, so can take into account thickness and stress.
(4) can be suitable for diffusion impervious layer in precise part, mould/cutter and medical apparatus surface strengthening and microelectronic chip.
embodiment
First adopt ordinary method to treat treat surface and carry out cleaning processing; Pending surface is placed in to vacuum vapor deposition system and utilizes reverse sputtering method clean surface, process rear surface clean enough through this two step, so just can better ensure coating quality; Again by reactive deposition deposition techniques nitride coatings.In deposition process, vacuum moulding machine parameter-bias voltage-periodical change between two numerical value, promotes deposited particles to sprawl at nitride coatings surface uniform, improves coating density.Bias voltage alternation parameter value in 0 ~-80V and-80 V ~ two of-150V interval each get a value; Alternating cycles is 1 minute-10 minutes.Be deposited into desired thickness, cooling under vacuum condition, then pass into drying nitrogen, open vacuum chamber, obtain fine and close nitride coatings.The hardness of described nitride ceramics coating is 1700Hv-2600Hv, and stress is 0.1GPa-1GPa.Preferred orientation has [111] and [100] two kinds of directions to form, and ratio can be from main regulation, and crystal grain ratio is 0-0.5, and grain-size is about 10 nm-200nm.
Before nitride coatings, can also adopt vapour deposition process to deposit 50 nm-200 nmTi or Cr middle layer in treat surface preparing, can omit this step according to practical situation.Because middle layer is mainly used to increase coating associativity, thus in some industry such as microelectronic industry does not just need.
embodiment 1
A kind of preparation method for fine and close unicircuit diffusion impervious layer TiN: after unicircuit front film depositing operation completes, Direct precipitation TiN diffusion impervious layer.Operating air pressure 0.1-2 Pa, nitrogen partial pressure is 0.016 Pa-0.25 Pa, and other gases are argon gas, and Ti target Sputtering power density is 2-7 W/cm
2, bias voltage alternation parameter value-50 V and-125V; Alternating cycles is 1 minute, and TiN coating deposit thickness is about 100 nm.
embodiment 2
A kind of preparation method for fine and close joint prosthesis surface strengthen layer TiN: first cleaning is carried out in the pending surface of joint prosthesis and process, this cleaning processing comprises to be carried out degreasing, oil removing, ash disposal, remove insulation layer and adopt reverse sputtering method clean surface in vacuum vapor deposition.Be placed in vacuum chamber; Pass into Ar gas at 0.1-10Pa, make the negative bias state of pending mechanical component in 0-1000V, negative bias causes plasma generation, and it is clean that the pending surface of ion bombardment further clean surface 5-20 minute completes reverse sputtering method; By controlled sputtering source depositing Ti or Cr middle layer, in treat surface, target as sputter power density is 2-7 W/cm
2, intermediate layer thickness is 50 nm-200 nm; By sputtering method depositing TiN coating, nitrogen partial pressure is 0.1 Pa again, and Sputtering power density can be 2,5,7 W/cm
2, bias voltage alternation parameter value being-75V and-150V; Alternating cycles is 2 minutes or 5 minutes, and thickness is 3,5,7,9 microns.
embodiment 3
A kind of preparation method for fine and close injection mold strengthening layer CrN: first elementary clean processing carried out in the pending surface of mould, this cleaning processing comprises to be carried out degreasing, oil removing, ash disposal and removes insulation layer etc.Remake further clean: be placed in vacuum chamber; Pass into Ar gas at 0.1-10Pa, make pending mechanical component in 0-1000V negative bias state, negative bias causes plasma generation, the further clean surface 5-20 minute in the pending surface of ion bombardment.By controlled sputtering source depositing Ti or Cr middle layer, in treat surface, target as sputter power density is 2-7 W/cm
2, intermediate layer thickness is 50 nm-200 nm; Deposit CrN coating by sputtering method again, nitrogen partial pressure is 0.2 Pa, and Sputtering power density can be 2,5,7 W/cm
2, bias voltage alternation parameter value-80V and-150V; Alternating cycles is 1 minute or 3 minutes, and thickness is 3,5,7,9 microns.
This CrN coating hardness is (1700Hv-2600Hv), lower stress (0.1 GPa-1GPa), and preferred orientation has [111] and [100] two kinds of directions to form, and corresponding crystal grain ratio is 0-0.5, and grain-size is about 10 nm-200nm.
Claims (3)
1. a preparation method for fine and close nitride ceramics coating, first cleans the pending surface of mechanical component; Pass through again reactive deposition legal system for nitride coatings, it is characterized in that, in the process of reactive deposition legal system for nitride coatings, be biased between high bias voltage and low bias voltage and alternately change; Described high bias voltage is arbitrary in 0--80V, and low bias voltage is arbitrary in-80 V--150V; The reaction times of each bias voltage is 1 minute-10 minutes.
2. the preparation method of fine and close nitride ceramics coating as claimed in claim 1, is characterized in that, preparing the Ti that first adopts vapour deposition process to deposit 50 nm-200 nm thickness before nitride coatings or Cr middle layer in surface.
3. the fine and close nitride ceramics coating that the preparation method of the fine and close nitride ceramics coating based on described in claim 1 or 2 obtains, it is characterized in that, the hardness of described nitride ceramics coating is 1700Hv-2600Hv, stress is 0.1GPa-1GPa, preferred orientation is made up of [111] and [100] two kinds of directions, crystal grain ratio is 0-0.5, and grain-size is at 10 nm-200nm.
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| CN201210110473.8A CN102634755B (en) | 2012-04-16 | 2012-04-16 | Compact nitride ceramic layer and preparation method thereof |
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| CN105779936B (en) * | 2016-01-20 | 2018-12-04 | 北京师范大学 | It is a kind of to keep superhard characteristic for super thick TiN film layer while improving the preparation method of toughness |
| CN108004517B (en) * | 2017-11-23 | 2019-11-22 | 中国航发北京航空材料研究院 | A kind of fiber-reinforced metal matrix composite Y2O3The physical gas-phase deposite method of coating |
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| CN1962927A (en) * | 2005-11-08 | 2007-05-16 | 中国科学院金属研究所 | Metal materials protection method (3) |
| WO2008053792A1 (en) * | 2006-11-01 | 2008-05-08 | Panasonic Corporation | Information recording medium, its manufacturing method, and sputtering target for forming information recording medium |
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| US7527713B2 (en) * | 2004-05-26 | 2009-05-05 | Applied Materials, Inc. | Variable quadruple electromagnet array in plasma processing |
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| CN1962927A (en) * | 2005-11-08 | 2007-05-16 | 中国科学院金属研究所 | Metal materials protection method (3) |
| WO2008053792A1 (en) * | 2006-11-01 | 2008-05-08 | Panasonic Corporation | Information recording medium, its manufacturing method, and sputtering target for forming information recording medium |
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Address after: Jiangning District of Tangshan street in Nanjing city of Jiangsu Province, 211131 soup Road No. 18 Applicant after: Southeast University Address before: 211189 Jiangsu Road, Jiangning Development Zone, Southeast University, No. 2, No. Applicant before: Southeast University |
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