CN104988466B - One kind is using double glow plasma surface alloying technology low temperature preparation α Al2O3The method of coating - Google Patents
One kind is using double glow plasma surface alloying technology low temperature preparation α Al2O3The method of coating Download PDFInfo
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Abstract
The present invention relates to one kind using double glow plasma surface alloying technology low temperature preparation α Al2O3The new method of coating.First, by with the addition of rare earth element y and α Al in Al targets2O3Crystal seed, Y and α Al are prepared for using double glow plasma surface alloying technology in 316L stainless steel surfaces2O3The Al coatings of crystal seed codope；Then, 580oHigh content of alpha Al in surface is obtained by the plasma oxidation coating under C low temperature2O3Coating.The invention provides one kind in 316L stainless steel surfaces low temperature preparation high content of alpha Al2O3The new method of coating, the coating can be widely applied to that metal stainless steel is corrosion-resistant, anti-oxidant and resistance tritium etc. field.
Description
Technical field
The present invention relates to one kind using double glow plasma surface alloying technology low temperature preparation α-Al2O3The new method of coating, belongs to
Technical field of surface coating.
Background technology
α-Al2O3With thermodynamic stability, even if also having good insulating properties, excellent chemically stable at high temperature
Property, and hardness is high, anti-tritium-permeation is strong and has the advantages that good selfreparing, therefore, led in electronic component, optics
The field such as domain and machinery has a wide range of applications.α-Al are prepared at present2O3The method of coating can be divided into a step and deposit by preparation section
With Combined Processing method（First prepare the treatment of aluminium lamination rear oxidation）.One step sedimentation mainly has physical vapour deposition (PVD), chemical vapor deposition
With plasma spraying etc..Matrix, is typically heated to 1000 by traditional chemical vapour deposition techniqueoMore than C can just make metastable phase
Al2O3Transformation forms the α-Al of stabilization2O3.But thermal expansion mismatch can produce residual stress, and the crackle pair that residual stress is produced
Adhesive force between film and matrix can have a negative impact.Chemical vapour deposition technique is not suitable in high-speed steel（HSS）Upper deposition,
Which limits the selection of matrix, too high preparation temperature can cause to damage and influence its structure and performance on matrix.Physics gas
Phase sedimentation provides the low temperature deposition methods of feasible replacement high temperature, and these methods are normally used for depositing at low temperature amorphous
Al2O3Coating.But, in order to obtain α phases, noncrystal membrane will undergo annealing in post synthesis, and its temperature is generally 750oC
Or it is higher.Therefore, how the high-quality α-Al of low temperature preparation2O3Coating tool is of great significance.
α phase transformations are a nucleation and the process grown up, and wherein being mostly used in for energy needed for phase transformation overcomes into nuclear potential
Build.Unformed Al2O3→ γ phases belong to the transformation of non-lattice rebuilding type, it is only necessary to which a small amount of energy can be completed, and the transformation of θ phases → α phases belongs to
In the transformation of lattice rebuilding type, it then follows forming core → growth mechanism, i.e., α nucleus is first generated in θ phases, elapsed more than critical by crystal boundary
Particle diameter come complete phase transformation, it is necessary to phase transformation higher activate can, most of energy ezpenditure is in nucleation process.Accordingly, it would be desirable to higher
Temperature providing the nucleating potential barrier of α.In the research hair such as corrosion science and the interim Li Mei bolts of guard technology periodical 2000,12 (1)
It is existing, aluminising coating in common thermal oxidation process, the starting stage surface form metastable phase.Thereafter, α-Al2O3In metastable phase
Al2O3/ alloy interface forming core, prevents metastable phase growth, and the metastable phase being initially formed starts to α phase in version.Therefore, promote steady
State α-Al2O3Preferentially being formed and reduce crystal transfer temperature can be by increasing Enhancing Nucleation Density and high-energy ion bombardment to overcome
α-Al2O3Nucleating potential barrier realize.
Surface mass can be promoted to accelerate movement by high-energy ion bombardment, while Ions Bombardment can also make Crystallization
Defect.The crystal defect that Ions Bombardment is produced also can be to promoting stable state α-Al2O3Preferentially formed and produce material impact.Because ion
Bombardment is a kind of activation process, and many crystal defects can be produced in this process, and these defects have laid in certain energy, one
Determine energy release at temperature, partial reaction energy barrier can be offset, promote stable state α-Al2O3Formation.Addition has " catalytic effect "
Alloying element or nanocrystalline influence whether stable state α-Al2O3Preferentially formed, because in crystal transfer this forming core, length again
In big process, nanocrystalline or alloying element presence increased the formation of crystal boundary, and for aluminium and oxygen are provided, quick diffusion is logical for this
Road, while being also Al2O3The transformation of crystal formation provides more equiax crystals, when nucleus depends on these particles in its surface
During forming core, nucleating surface can be reduced, so that forming core is easier to make for, macroscopically then show as α-Al2O3Phase transition temperature
Reduce.In addition, the alloying element (yttrium, cerium etc.) with catalytic effect is mixed in the preparation process of material can promote α-Al2O3
Growth.Rovere et al. researchs find on Surface and Coatings Technology periodical 202 phases in 2008
The doping of a small amount of Y can enter into metastable phase Al2O3Defect in, tied because the addition of Y promotes negative ions room compound
Structure restructuring releases energy such that it is able to promote metastable phase Al2O3To α-Al2O3Transformation.Meanwhile, the addition of Y is also greatly improved
The antioxygenic property of Cr-Al-N coatings.
Under plasma bombardment, by adding rare earth element y and α-Al2O3Crystal seed promotes stable state α-Al2O3Low temperature shape
Into the technology has important theory significance and application value in resistance tritium coating, low-temperature oxidation and metal protection coatings art.
The content of the invention
It is an object of the invention to open a kind of using double glow plasma surface alloying technology low temperature preparation α-Al2O3Coating
New method.Temperature needed for preparing is low, does not influence substrate performance, enhances coating.316L stainless steel surfaces prepare containing α-
Al2O3The coat of aluminide of crystal seed and rare earth element y, the Fe-Al transition zones formed in deposition process can improve coating and matrix
Bond strength.Meanwhile, by introducing α-Al2O3Crystal seed and rare earth element y reduce α-Al2O3The formation temperature of coating.
Technical solution of the invention is：In double glow discharge alloying process technology, in the initial depositional phase,
Sputtering and again sputtering and deposition process exist simultaneously, and this causes FeAl and Fe3Al phases are easier the interface in coating and matrix
Place is formed, with the carrying out of sputtering, because the voltage of the voltage ratio matrix of target is more negative, the Al particles sputtered out from target
The Fe particles sputtered out from matrix are far longer than, deposition occupies leading position so that Fe and Al points in depositing coating
Cloth forms concentration gradient, and then has promoted Al to be spread to matrix direction.And Fe spreads to coating surface, because bombardment is formd greatly
The defect of amount is more beneficial for carrying out in causing mutually to be diffused in subsequent deposition process, Fe-Al phase diffusion layers is formd, so as to obtain
Surface richness Al and it is internal be the aluminising coating of FeAl metallurgical bindings.By plasma bombardment, addition α-Al in oxidizing process2O3
Low temperature preparation high content of alpha-Al is realized under the coupling of crystal seed and rare earth element y2O3Coating.
General principle of the invention is：α-Al2O3The granularity very little of crystal seed, and its crystal structure and α-Al2O3Nucleus
It is the same.In α-Al2O3Also in compliance with the process of forming core-growth in growth course.In subsequent oxidation stage, in the coating α-
Al2O3Crystal seed is to α-Al2O3Formation have inducing action, the Al near crystal seed can be attached on crystal seed so as to reduce forming core energy；
Meanwhile, Y depends on the heterogeneous forming core of microstructure and hinders its crystal grain to grow up to the facilitation of metastable phase；Research discovery, only
The transformation of metastable opposite α phases can be promoted when there are Y contents relatively low, and content Y high then hinders the formation of α phases.Meanwhile, rare earth unit
Plain radius ratio is larger, can eliminate lattice vacancy, in alloy/interfacial oxide film room can be prevented to be formed, and improves adhesion and cause
Close property.
The method includes step in detail below：
（1）By 10 wt% Y, 10 wt% α-Al2O3Crystal seed and 80 wt% Al powder carry out uniform ball on planetary ball mill
Mill mixing, using being pressed into disk on small-sized cold press, then is sintered prepared Al/Y/ α-Al in vacuum hotpressing stove2O3Target；
（2）Doped alpha-Al is prepared in 316L stainless steel surfaces by double glow plasma surface alloying technology2O3Crystal seed and rare earth unit
The Al coatings of plain Y.Experiment parameter is：Vacuum, 2 × 10-4 Pa；Source voltage, -700 V, matrix voltage, -300 V, interpolar
Away from 15 mm；Air pressure, 30 Pa；Sputtering time, 3h；Sputter temperature, 580oC；
（3）To obtained containing Y and α-Al by the way of plasma oxidation2O3The Al coatings of crystal seed codope carry out hot place
Reason.Oxidizing temperature is 580oC, the sccm of argon flow amount 40, air pressure 40 Pa, oxidization time 1h, by changing single factor test oxygen flow
Size, prepare satisfactory coating, oxygen flow is 0.5~4sccm.
The present invention obtain technological progress be：1）α-the Al2O3Coating uses codope α-Al2O3Crystal seed and rare earth element y
Al targets, carry out permeation in stainless steel surfaces using double glow plasma surface alloying technology, realize three factor couplings
Under (Ions Bombardment, addition α-Al2O3Crystal seed and rare earth element y) low temperature 580oHigh content of alpha-Al is prepared under C2O3Coating.2）Utilize
Double glow plasma surface alloying technology makes preparation α-Al2O3The temperature reduction of coating, prevent the performance of matrix is influenceed by high temperature.3）
The aluminized coating surfacing prepared is fine and close, and the defect such as non-microcracked and Microfocus X-ray tube, and matrix is well combined, continuous, interface without
Hole and crackle, aluminium element percentage composition in interface distribution gradient, the α-Al2O3Coating is corrosion-resistant to 316L stainless steels
And the performance such as anti-oxidant is improved.
Brief description of the drawings
Fig. 1 is source electrode and workpiece pole arrangement schematic diagram；
Fig. 2 is the GAXRD collection of illustrative plates of sample 1-4；
Fig. 3（a）（b）（c）（d）It is the surface topography of sample 1-4；
Fig. 4 is（a）（b）（c）（d）It is the cut curve of sample 1-4；
Fig. 5 is polarization curves of the sample 1-4 in 3.5%NaCl solution.
Specific embodiment
With reference to specific embodiments and the drawings, the invention will be further described.
During double glow plasma surface alloying,, using hollow cathode effect come heated substrate, its electrode structure is such as we
Shown in Fig. 1.Argon gas is filled with after body of heater is evacuated into vacuum, switching on power will produce aura to put between source electrode 1 and workpiece pole 2
Electricity, using the argon ion bombardment target 3 produced by glow discharge, on the one hand can be such that alloying element is sputtered from source electrode target
Out, it is transported to up to the surface of workpiece 5 by space and is adsorbed by workpiece surface.At the same time, argon ion bombardment workpiece makes it
High temperature is heated to, the temperature in stove is determined by thermocouple 4.Because the fusing point of Al is only 660.4 oC, in dual-layer glow ion
In implantation technique, when temperature is too high can make aluminum portions region melt and ooze out aluminium liquid so that localised glow enhancing produce beat
Arc phenomenon, in order to avoid this phenomenon, while disclosure satisfy that (580 the need for substrate temperature againoC), using two pieces of stainless steel plates 6
Form hollow cathode effect and carry out heated partses 5.
Embodiment 1
（1）By 10 wt% Y, 10 wt% α-Al2O3Crystal seed and 80 wt% Al powder carry out uniform ball on planetary ball mill
Mill mixing, using being pressed into disk on small-sized cold press, then is sintered prepared Al/Y/ α-Al in vacuum hotpressing stove2O3Target；
（2）Doped alpha-Al is prepared in 316L stainless steel surfaces by double glow plasma surface alloying technology2O3Crystal seed and rare earth unit
The Al coatings of plain Y.Experiment parameter is：Vacuum, 2 × 10-4 Pa；Source voltage, -700 V, matrix voltage, -300 V, interpolar
Away from 15 mm；Air pressure, 30 Pa；Sputtering time, 3h；Sputter temperature, 580oC；
（3）To obtained containing Y and α-Al by the way of plasma oxidation2O3The Al coatings of crystal seed codope carry out hot place
Reason.Oxidizing temperature is 580oC, the sccm of argon flow amount 40, air pressure 40 Pa, oxidization time 1h, by changing single factor test oxygen flow
Size, prepare satisfactory coating, oxygen flow is 0.5sccm.
Embodiment 2
（1）By 10 wt% Y, 10 wt% α-Al2O3Crystal seed and 80 wt% Al powder carry out uniform ball on planetary ball mill
Mill mixing, using being pressed into disk on small-sized cold press, then is sintered prepared Al/Y/ α-Al in vacuum hotpressing stove2O3Target；
（2）Doped alpha-Al is prepared in 316L stainless steel surfaces by double glow plasma surface alloying technology2O3Crystal seed and rare earth unit
The Al coatings of plain Y.Experiment parameter is：Vacuum, 2 × 10-4 Pa；Source voltage, -700 V, matrix voltage, -300 V, interpolar
Away from 15 mm；Air pressure, 30 Pa；Sputtering time, 3h；Sputter temperature, 580oC；
（3）To obtained containing Y and α-Al by the way of plasma oxidation2O3The Al coatings of crystal seed codope carry out hot place
Reason.Oxidizing temperature is 580oC, the sccm of argon flow amount 40, air pressure 40 Pa, oxidization time 1h, by changing single factor test oxygen flow
Size, prepare satisfactory coating, oxygen flow is 1sccm.
Embodiment 3
（1）By 10 wt% Y, 10 wt% α-Al2O3Crystal seed and 80 wt% Al powder carry out uniform ball on planetary ball mill
Mill mixing, using being pressed into disk on small-sized cold press, then is sintered prepared Al/Y/ α-Al in vacuum hotpressing stove2O3Target；
（2）Doped alpha-Al is prepared in 316L stainless steel surfaces by double glow plasma surface alloying technology2O3Crystal seed and rare earth unit
The Al coatings of plain Y.Experiment parameter is：Vacuum, 2 × 10-4 Pa；Source voltage, -700 V, matrix voltage, -300 V, interpolar
Away from 15 mm；Air pressure, 30 Pa；Sputtering time, 3h；Sputter temperature, 580oC；
（3）To obtained containing Y and α-Al by the way of plasma oxidation2O3The Al coatings of crystal seed codope carry out hot place
Reason.Oxidizing temperature is 580oC, the sccm of argon flow amount 40, air pressure 40 Pa, oxidization time 1h, by changing single factor test oxygen flow
Size, prepare satisfactory coating, oxygen flow is 2sccm.
Embodiment 4
（1）By 10 wt% Y, 10 wt% α-Al2O3Crystal seed and 80 wt% Al powder carry out uniform ball on planetary ball mill
Mill mixing, using being pressed into disk on small-sized cold press, then is sintered prepared Al/Y/ α-Al in vacuum hotpressing stove2O3Target；
（2）Doped alpha-Al is prepared in 316L stainless steel surfaces by double glow plasma surface alloying technology2O3Crystal seed and rare earth unit
The Al coatings of plain Y.Experiment parameter is：Vacuum, 2 × 10-4 Pa；Source voltage, -700 V, matrix voltage, -300 V, interpolar
Away from 15 mm；Air pressure, 30 Pa；Sputtering time, 3h；Sputter temperature, 580oC；
（3）To obtained containing Y and α-Al by the way of plasma oxidation2O3The Al coatings of crystal seed codope carry out hot place
Reason.Oxidizing temperature is 580oC, the sccm of argon flow amount 40, air pressure 40 Pa, oxidization time 1h, by changing single factor test oxygen flow
Size, prepare satisfactory coating, oxygen flow is 4sccm.
Performance evaluation to sample is as follows：
1st, the phase composition of coating surface：
Fig. 2 is the GAXRD collection of illustrative plates of sample 1-4.From Figure 2 it can be seen that have in the oxide layer prepared under different oxygen flows α-
Al2O3And Fe2O3Diffraction maximum.With the change of oxygen flow, the thing in coating is mutually different, when oxygen flow is 0.5sccm
When, still there is FeAl and Fe in coating2Al5The presence of phase, in the case that this explanation oxygen is insufficient, the Fe-Al phases in coating are not
It is substantially oxidized；When flow is 1sccm, Fe2Al5Mutually disappear, meanwhile, oxygen flow increase, α-Al in coating2O3Diffraction maximum
Become strong, this explanation O2-The concentration of ion plays vital effect for the diffusion of oxonium ion, oxygen concentration increase to α-
Al2O3Formation have facilitation；When oxygen flow continues to increase to 2-4sccm, mutually there is no substantially change in the thing in coating
Change, simply Fe2O3With α-Al2O3Becoming for diffraction maximum is more sharp, illustrates that oxygen flow increases so that more Fe-Al phases are by oxygen
Change.Meanwhile, the Al of metastable phase crystal formation is not found in the coating2O3In the presence of, it may be possible to rare earth element y and α-Al2O3Crystal seed plus
Enter to promote metastable opposite α-Al2O3Transformation.
2nd, the surface topography of coating
The surface topography of sample 1-4 such as Fig. 3（a）（b）（c）（d）It is shown.As seen from Figure 3, coating is in oxygen flow
When 0.5sccm is aoxidized, the surface topography of sample 1 has no obvious change；When oxygen flow is when increasing to 1sccm, the painting of sample 2
Layer surface becomes finer and close, occurs in that the raised structure of island；When oxygen flow is 2sccm, oxide covering surface is without obvious
Defect, surface roughness increase, coating surface island projection increases.The addition of Y can suppress nanocrystal to a certain extent
Growth, although the coating surface for preparing is relatively rough, the release of Y element can improve the mechanical property of coating, increase and apply
The adhesion of layer.During with the further increase of oxygen flow for 4sccm, the floating coat outer layer of sample 4 occurs in that a large amount of holes and splits
Line, or even the local phenomenon for occurring peeling off, this is probably due to the Al that oxygen flow increase is resulted in2O3The heat of coating and matrix
The coefficient of expansion mismatches the peeling phenomenon so as to produce.
3rd, the adhesion of coating
Fig. 4（a）（b）（c）（d）It is the cut curve of sample 1-4.From fig. 4, it can be seen that the adhesion of coating is with oxygen flow
Increase first increases and then decreases.As shown in Fig. 4 (a), when oxygen flow is 0.5sccm, the adhesion of the coating of sample 1 has reached 68N；
When oxygen flow is 1 and 2sccm, the adhesion of the coating of sample 2 and 3 has reached more than 70N, and research finds that Y can promote Al2O3
The selective oxidation of coating, reduces alloy and forms Al2O3The critical Al content of coating；Meanwhile, rare earth element y or its oxide
It is present at alloy interface, makes oxide covering and alloy surface strong bonded；On the other hand, rare earth element radius is big, can disappear
Except lattice vacancy, room can be prevented to be formed at alloy/oxide covering interface, improve adhesion；With the further increasing of oxygen flow
Greatly, the adhesion of the coating of sample 4 declines more apparent, only 50N, but remains to be attached on matrix, and this is probably due to oxygen flow
Increase, coating surface forms the aluminum oxide coating layer of fragility, therefore is easier to peel off.
In double glow plasma surface alloying technology, due to foring the metallurgical binding of Fe-Al between coating and matrix, therefore can
To find out, the adhesion of coating is preferable, and research shows that the critical adhesion of coating meets actual skimming wear by reaching 30N
Operating mode application, this shows that prepared coating is combined row preferably with matrix, it is sufficient to meet the demand of practical application.
4th, the corrosion resisting property of coating
Fig. 5 is polarization curves of the sample 1-4 in 3.5%NaCl solution.As shown in Figure 5, the coating after oxidation show compared with
Good decay resistance, when oxygen flow is 2sccm, the corrosion potential of the coating of sample 3 is up to -0.130V, and corrosion current is most
Low level is 0.009 μ A cm-2, than 316L stainless steel base, reduce nearly 3 orders of magnitude.With the increase of oxygen flow, coating
Corrosion potential first rises and then decreases.On the whole, doping Y and α-Al2O3The corrosive nature of the oxide covering of seed crystal is improved
, this is probably because of these Y2O3With α-Al2O3" physical barrier " or Rare Earth Y can be served as in the environment of corrosion2O3
Grain can form many " corrosion micro cells ", and wherein oxide particle serves as negative electrode and stainless steel base serves as anode；Meanwhile, this
The entrance of a little particles has also promoted crystal grain refinement so that the corrosive nature of composite is improved.
Concrete application approach of the present invention is a lot, and the above is only the preferred embodiment of the present invention, it is noted that for
For those skilled in the art, under the premise without departing from the principles of the invention, some improvement can also be made, this
A little improvement also should be regarded as protection scope of the present invention.
Claims (2)
1. a kind of using double glow plasma surface alloying technology low temperature preparation α-Al2O3The method of coating, it is characterised in that including with
Lower step：
（1）By 10wt%Y, 10wt% α-Al2O3Crystal seed and 80wt%Al powder carry out uniform ball milling mixing on planetary ball mill, utilize
Disk is pressed on small-sized cold press, then is sintered in vacuum hotpressing stove, Al/Y/ α-Al are obtained2O3Target；
（2）Doped alpha-Al is prepared in 316L stainless steel surfaces by double glow plasma surface alloying technology2O3Crystal seed and rare earth element y
Al coatings；
Parameter is：Vacuum, 2 × 10-4Pa；Source voltage, -700V, matrix voltage, -300V, die opening, 15mm；Air pressure,
30Pa；Sputtering time, 3h；Sputter temperature, 580oC；
（3）To obtained containing Y and α-Al by the way of plasma oxidation2O3The Al coatings of crystal seed codope are heat-treated, oxygen
It is 580 DEG C to change temperature, argon flow amount 40sccm, air pressure 40Pa, oxidization time 1h, by changing the size of single factor test oxygen flow,
Satisfactory coating is prepared, oxygen flow is 0.5~4sccm；
Al/Y/ α-the Al2O3Contain 10wt%Y, 10wt% α-Al in composite target material2O3Crystal seed and 80wt%Al powder.
2. as claimed in claim 1 a kind of using double glow plasma surface alloying technology low temperature preparation α-Al2O3The method of coating,
It is characterized in that：The coating is applied to that metal stainless steel is corrosion-resistant, anti-oxidant and resistance tritium field.
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| CN105714244B (en) * | 2016-03-30 | 2018-02-23 | 青岛滨海学院 | A kind of titanium alloy surface ceramic/metal step high temperature composite coating and preparation method thereof |
| SG11201903343VA (en) * | 2017-03-15 | 2019-05-30 | Jx Nippon Mining & Metals Corp | Al2o3 sputtering target and production method thereof |
| CN107641794A (en) * | 2017-09-30 | 2018-01-30 | 铜山县利国钢铁有限公司 | A kind of stable corrosion-resistant stainless steel part |
| CN108411262B (en) * | 2018-03-05 | 2020-09-25 | 华南理工大学 | Low-temperature reactive sputtering deposition nanometer α -Al2O3Method for coating |
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| CN109989044B (en) * | 2019-04-03 | 2021-09-21 | 华南理工大学 | AlCr + alpha-Al2O3Sputtering target material and preparation and application thereof |
| CN109987947A (en) * | 2019-04-19 | 2019-07-09 | 中国科学院上海硅酸盐研究所 | Utilize the thermally conductive method with mechanical property of in-situ stress induced transformation Synchronous fluorimetry aluminum oxide coating layer |
| CN113802094B (en) * | 2020-06-16 | 2024-04-05 | 中微半导体设备(上海)股份有限公司 | Coating method of corrosion-resistant coating, plasma etched part and reaction device |
| CN114196917A (en) * | 2021-11-05 | 2022-03-18 | 南华大学 | Al2O3Tritium-resistant coating and preparation method thereof |
| CN114807854A (en) * | 2022-04-14 | 2022-07-29 | 华南理工大学 | Method for depositing alpha-alumina dielectric film on surface of silicon substrate |
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