CN104697918A - Test method for high-temperature oxidation resistance of CrTiAlN coating - Google Patents
Test method for high-temperature oxidation resistance of CrTiAlN coating Download PDFInfo
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- CN104697918A CN104697918A CN201510060521.0A CN201510060521A CN104697918A CN 104697918 A CN104697918 A CN 104697918A CN 201510060521 A CN201510060521 A CN 201510060521A CN 104697918 A CN104697918 A CN 104697918A
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Abstract
The invention relates to a test method for high-temperature oxidation resistance of a CrTiAlN coating. The test method comprises the following steps: depositing a CrTiAlN coating on the surface by using a British Teer-UDP650/4 type closed field unbalanced magnetron sputtering ion plating device; and then carrying out high-temperature oxidation experiment on a test sample by using an SX2-4-10 high-temperature box type resistance furnace at the temperature of 500-700 DEG C, performing heat preservation for 1 hour and cooling naturally in the furnace to room temperature. The test method provided by the invention is simple and fast, and can effectively detect the high-temperature oxidation resistance of the CrTiAlN coating.
Description
Technical field
The present invention relates to a kind of method of testing, particularly relate to a kind of method of testing of CrTiAlN coating high-temp antioxygenic property.
Background technology
M2 high-speed steel is used for manufacturing cutting tool, in recent years, along with high-speed cutting industrial expansion, the temperature that working angles cutter bears and cutting force significantly rise, cutter oxidation is serious, causes deformation failure, reduced lifetime, for this high-temperature oxidation resistance to cutter is had higher requirement.
Utilize physical vapor deposition (PVD) technology at high-speed steel tool surface deposition hard coat, to improving cutter high-temperature oxidation resistance and increasing the service life very effective.TiN is first generation PVD hard coat, is widely used in cutter coat, but going deep into along with application, its high-temperature oxidation resistance can not satisfy the demands, and when temperature is more than 500 DEG C, TiN coating surface can the larger TiO of oxidized generation fragility
2, due to TiN and TiO
2between the greatest differences of molar volume, can compressive stress be produced in oxide layer, make coating breaks down, thus destroy the protective effect of coating, limit the application of TiN coating under high-speed cutting condition in machining.On TiN coating basis, introduce Al element and form ternary system coating TiAlN, the high-temperature oxidation resistance of coating can be improved further.Although and know that ternary system coating TiAlN can improve high-temperature oxidation resistance, how its oxidation susceptibility specifically but cannot be learnt.
Summary of the invention
The object of the invention is to the method for testing in order to provide a kind of simple and quick, effective CrTiAlN coating high-temp antioxygenic property.
In order to realize above-mentioned order ground, the present invention by the following technical solutions:
A kind of CrTiAlN coating high-temp antioxygenic property method of testing, described method of testing for prepare CrTiAlN coating on M2 high speed steel substrate, obtain sample, then high-temperature oxydation experiment is carried out to sample, adopt the EDS energy spectrum analysis that grazing incidence X-ray diffraction and SEM carry.In the technical program, adopt SX2-4-10 high temperature box type resistance furnace to carry out high-temperature oxydation experiment to sample, temperature is set to 500 DEG C, 700 DEG C, 900 DEG C respectively, cools to room temperature with the furnace after insulation 1h.Adopt scanning electron microscope (SEM, Zeiss Sigma, Germany) CrTiAlN coating oxidation front and rear surfaces and cross-section morphology is observed, thing phase composition analysis adopts grazing incidence X-ray diffraction (GIXRD, Panalytica X ' pert PRO, Netherlands) and the EDS energy spectrum analysis that carries of SEM.GIXRD test analysis: the institutional framework of CrTiAlN coating adopts glancing incidence XRD analysis, Fig. 1 is the XRD collection of illustrative plates of coating after different temperatures oxidation, can see that the diffraction peak of fcc-CrN phase only appears in CrTiAlN coating under normal temperature, diffraction crystal face is respectively CrN(111), (200), (220), there is not the diffraction peak of Al, Ti and compound thereof
As preferably, each constituent content of CrTiAlN coating is respectively: Cr:44.80at.%, Ti:6.45at.%, Al:5.26at.%, N:43.48at.%.
As preferably, in high-temperature oxydation experiment, temperature is 500-900 DEG C, cools after insulation 1-3h with stove.
As preferably, CrTiAlN coating thickness is 5-20 μm.
As preferably, M2 high speed steel substrate adopt the mode of ion plating prepare CrTiAlN coating.
The invention has the beneficial effects as follows that method of testing of the present invention is simple and quick, effectively can detect the high-temperature oxidation resistance of CrTiAlN coating.
Accompanying drawing explanation
Fig. 1 is XRD collection of illustrative plates under different temperatures of the present invention.
Fig. 2 is CrTiAlN coating different temperatures lower surface pattern.
Fig. 3 is cross-section morphology under CrTiAlN coating different temperatures.
Fig. 4 is section EDS surface sweeping figure under CrTiAlN coating different temperatures.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.
In the present invention, if not refer in particular to, the raw material adopted and equipment etc. all can be buied from market or this area is conventional.
Method in following embodiment, if no special instructions, is the conventional method of this area.
Embodiment 1
One deck CrTiAlN coating that utilized Britain Teer-UDP650/4 type closed field unbalanced magnetron sputtering ion plating equipment at its surface deposition, this coating thickness is 5 μm, then SX2-4-10 high temperature box type resistance furnace is adopted to carry out high-temperature oxydation experiment to sample, temperature is set to 500 DEG C, cools to room temperature with the furnace after insulation 1h.Wherein, each constituent content of CrTiAlN coating is respectively: Cr:44.80at.%, Ti:6.45at.%, Al:5.26at.%, N:43.48at.%.
Embodiment 2
One deck CrTiAlN coating that utilized Britain Teer-UDP650/4 type closed field unbalanced magnetron sputtering ion plating equipment at its surface deposition, this coating thickness is 15 μm, then SX2-4-10 high temperature box type resistance furnace is adopted to carry out high-temperature oxydation experiment to sample, temperature is set to 700 DEG C, cools to room temperature with the furnace after insulation 2h.Wherein, each constituent content of CrTiAlN coating is respectively: Cr:44.80at.%, Ti:6.45at.%, Al:5.26at.%, N:43.48at.%.
Embodiment 3
One deck CrTiAlN coating that utilized Britain Teer-UDP650/4 type closed field unbalanced magnetron sputtering ion plating equipment at its surface deposition, this coating thickness is 20 μm, then SX2-4-10 high temperature box type resistance furnace is adopted to carry out high-temperature oxydation experiment to sample, temperature is set to 900 DEG C, cools to room temperature with the furnace after insulation 3h.Wherein, each constituent content of CrTiAlN coating is respectively: Cr:44.80at.%, Ti:6.45at.%, Al:5.26at.%, N:43.48at.%.
GIXRD test analysis: the institutional framework of CrTiAlN coating adopts glancing incidence XRD analysis, Fig. 1 is the XRD collection of illustrative plates of coating after different temperatures oxidation, can see that the diffraction peak of fcc-CrN phase only appears in CrTiAlN coating under normal temperature, diffraction crystal face is respectively CrN(111), (200), (220), do not occur the diffraction peak of Al, Ti and compound thereof, reason is that in coating, Al, Ti atom content is lower.Along with temperature raises, CrN diffraction peak width reduces, and this represents that annealing makes defect concentrations in crystals reduce, grain growth, and grating constant becomes large.500 DEG C and 700 DEG C time, all there is not the diffraction peak of oxide in XRD collection of illustrative plates, when 900 DEG C, in collection of illustrative plates, occurred Cr
2o
3the diffraction peak of phase, diffraction crystal face is respectively Cr
2o
3(012), (104), (110), (116), (119), when this shows 900 DEG C, CrTiAlN coating starts oxidation.
EDS Surface scan is analyzed: CrTiAlN coating EDS Surface scan result after different temperatures oxidation is as shown in table 1, when can see 500 DEG C and 700 DEG C, atom N number mark is respectively 40.92at.%, 39.58at.%, minimizing is few compared with atom N number mark (43.48at.%) in coating under normal temperature, and O atomicity mark is respectively 4.42at.%, 7.06at.%, known in conjunction with XRD analysis result above, when 500 DEG C, 700 DEG C, CrTiAlN coating does not also start oxidation, and these oxygen are that oxygen desorption in air is at specimen surface.When 900 DEG C, atom N number mark and O atomicity mark are respectively 13.75at.%, 32.44at.%, compare with 700 DEG C with 500 DEG C, and atom N number mark obviously reduces, O atomicity mark showed increased.In conjunction with before XRD analysis result, illustrates CrTiAlN coating 900 DEG C start be oxidized.
Table 1
| N(at.％) | O(at.％) | Cr(at.％) | Ti(at.％) | Al(at.％) | |
| RT | 43.48 | 0.00 | 44.80 | 6.45 | 5.26 |
| 500℃ | 40.92 | 4.42 | 43.31 | 6.34 | 5.00 |
| 700℃ | 39.58 | 7.06 | 41.31 | 6.60 | 5.46 |
| 900℃ | 13.75 | 32.44 | 42.32 | 6.55 | 4.94 |
Coating surface Morphology analysis before and after oxidation: Fig. 2 is the surface topography of CrTiAlN coating, can see, under normal temperature, CrTiAlN coating surface is smooth, dense structure, particle fine uniform and regular shape, combine closely between particle, do not have the defect such as gap, pin hole.When 500 DEG C, CrTiAlN coating granule becomes large, and particle size becomes uneven, cause coating surface roughness descent, but the defect such as gap, pin hole does not appear in coating, organizes still fine and close.When 700 DEG C, coating is not too large change compared with 500 DEG C, and melting phenomenon appears in coating surface.When 900 DEG C, coating microscopic appearance there occurs significant change, can see that coating surface dense structure property obviously declines, particle size becomes large and size is uneven, and coating surface defines obvious oxide grain, EDS analysis result in associative list 1, when this illustrates 900 DEG C, coating has started oxidation, but does not have Fe element in EDS Surface scan result, this illustrates that CrTiAlN coating is not destroyed, and still plays high temperature protection effect to matrix.
Coating section Morphology analysis before and after oxidation: the cross-section morphology of CrTiAlN coating as shown in Figure 3, can see, CrTiAlN coating section is obvious columnar crystal structure, combine closely between crystal column, section is without defects such as obvious micro-crack, pin holes, the interface of coating and matrix is smooth, high-visible simultaneously, and the coating section close to matrix can observe the very fine and close fine grain of one deck, and this can ensure to obtain good film substrate bond strength between coatings and substrate.When 500 DEG C, coating section does not change substantially, and the fine grain bottom coating becomes finer and close, combines good between coating and matrix.When 700 DEG C, there is non-columnar characteristic in coating section gradually, and combine closely between crystal column, the coating section close to matrix presents without grain shape, becomes finer and close, coating and matrix is combined together, combines tightr between coated substrate.When 900 DEG C, can see the oxide layer having thin layer above coating, coating section is dispersed with some oxides along column crystal, this illustrates that the oxygen in air is diffused into coat inside, makes coat inside start oxidation.The oxidation mechanism of CrTiAlN coating is: the oxygen in air spreads towards coat inside, temperature more high diffusivity faster, when 900 DEG C, oxygen is diffused into coat inside, make coating start oxidation, but combine good between coating and matrix, coating still plays protective action to matrix.
Before and after oxidation, coating section EDS line scanning: Fig. 4 is the section EDS line sweep result of CrTiAlN coating after 500 DEG C, 700 DEG C and 900 DEG C of oxidations, and can see, in CrTiAlN coating, essential element is Cr, is secondly N, also has a small amount of Al and Ti in addition.When 500 DEG C, Cr, Ti in coating, Al, N element content are substantially constant, and when O content is zero, 700 DEG C substantially, O content is still zero.When 900 DEG C; coating is oxidized, and oxide layer has appearred in coating surface, but still containing each elemental composition of coating in oxide layer region; this illustrates that coating still plays protective effect to matrix 900 DEG C time, and coating has good antioxygenic property 900 DEG C time.
Claims (5)
1. a CrTiAlN coating high-temp antioxygenic property method of testing, it is characterized in that, described method of testing, for prepare CrTiAlN coating on M2 high speed steel substrate, obtains sample, then high-temperature oxydation experiment is carried out to sample, adopt the EDS energy spectrum analysis that grazing incidence X-ray diffraction and SEM carry.
2. a kind of CrTiAlN coating high-temp antioxygenic property method of testing according to claim 1, it is characterized in that, each constituent content of CrTiAlN coating is respectively: Cr:44.80at.%, Ti:6.45at.%, Al:5.26at.%, N:43.48at.%.
3. a kind of CrTiAlN coating high-temp antioxygenic property method of testing according to claim 1, is characterized in that, in high-temperature oxydation experiment, temperature is 500-900 DEG C, cools after insulation 1-3h with stove.
4. a kind of CrTiAlN coating high-temp antioxygenic property method of testing according to claim 1 or 2 or 3, it is characterized in that, CrTiAlN coating thickness is 5-20 μm.
5. a kind of CrTiAlN coating high-temp antioxygenic property method of testing according to claim 1 or 2 or 3, is characterized in that, M2 high speed steel substrate adopts the mode of ion plating prepare CrTiAlN coating.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105675637A (en) * | 2016-01-22 | 2016-06-15 | 河北钢铁股份有限公司 | Method for enhancing X-ray diffraction intensity of surface oxide layer of steel |
| CN109518139A (en) * | 2018-12-13 | 2019-03-26 | 北京金轮坤天特种机械有限公司 | A kind of titanium fire flame retardant coating and preparation method thereof |
| CN112159955A (en) * | 2020-09-21 | 2021-01-01 | 宁波云涂科技有限公司 | Hard hydrophobic coating with micro-nano structure and preparation method thereof |
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| CN102776474A (en) * | 2012-07-12 | 2012-11-14 | 济南大学 | Nano composite coating layer for surface treatment of substrate, and preparation method and device of nano composite coating layer |
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| CN102166849A (en) * | 2010-12-20 | 2011-08-31 | 武汉新铬涂层设备有限公司 | Chromium nitride aluminum-titanium composite coating, cutter deposited with same, and preparation method |
| CN102776474A (en) * | 2012-07-12 | 2012-11-14 | 济南大学 | Nano composite coating layer for surface treatment of substrate, and preparation method and device of nano composite coating layer |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105675637A (en) * | 2016-01-22 | 2016-06-15 | 河北钢铁股份有限公司 | Method for enhancing X-ray diffraction intensity of surface oxide layer of steel |
| CN109518139A (en) * | 2018-12-13 | 2019-03-26 | 北京金轮坤天特种机械有限公司 | A kind of titanium fire flame retardant coating and preparation method thereof |
| CN109518139B (en) * | 2018-12-13 | 2021-02-26 | 北京金轮坤天特种机械有限公司 | Titanium fire flame-retardant coating and preparation method thereof |
| CN112159955A (en) * | 2020-09-21 | 2021-01-01 | 宁波云涂科技有限公司 | Hard hydrophobic coating with micro-nano structure and preparation method thereof |
| CN112159955B (en) * | 2020-09-21 | 2022-05-13 | 宁波云涂科技有限公司 | Hard hydrophobic coating with micro-nano structure and preparation method thereof |
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