CN104928742A - MAX phase ceramic and composite material surface modification processing method thereof - Google Patents
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Abstract
The invention relates to the field of material surface modification processing, in particular to MAX phase ceramic and a composite material surface modification processing method thereof. A micro-arc oxidation method is adopted for generating oxide film layers on the MAX phase ceramic and a composite material surface of the MAX phase ceramic in situ, and mainly, the MAX phase ceramic with M being valve metal elements (Ti, Mg, Al, Zr, Nb, Ta and the like) and solid solutions or second-phase modified composite materials with the MAX phase ceramic being bases are processed. A micro-arc oxidation processing technology is adopted so that the composite oxide film layers which are well combined with base bodies compactly can be prepared on the surfaces of ceramic materials. The method is low in cost, simple in technology, environmentally friendly, and capable of being applied on a large scale and remarkably improving the surface hardness, the corrosion resistance, the abrasion resistance, high-temperature thermal stability and other performance of the MAX phase ceramic materials with good performance of ceramic and metal and the composite materials of the MAX phase ceramic materials.
Description
Technical field
The present invention relates to field of material surface modification treatment, be specially the treatment process of a kind of MAX phase ceramics and composite material surface modification thereof, it adopts differential arc oxidation method in the method for MAX phase ceramics and composite material surface in-situ preparation oxide membranous layer thereof.
Background technology
MAX phase, be the common name that a class has the ternary compound of microcosmic laminate structure, its chemical formula can be expressed as M
n+1aX
n, M is transiting group metal elements, and A is main group element (mainly referring to III A and IV A race element), and X is C or N element, and n is the integer of 1 ~ 6.Typical MAX phase comprises: Ti
3siC
2, Ti
3alC
2, Ti
2alC, Cr
2alC etc.MAX phase compound has the premium properties of metal and pottery concurrently because of the crystalline structure of its uniqueness and bonding pattern, as low density, high elastic coefficient, good heat conduction and electroconductibility, workability, high damage tolerance etc.Particularly this kind of material has high damage tolerance and workability, overcome the shortcoming of the large and difficult processing of typical ceramic material intrinsic fragility, be with a wide range of applications as high-temperature structural material, wear resistant friction reducing material, corrosion resistant material and bio-medical material etc.On the other hand, this kind of material is little compared with typical ceramic material surface hardness, and element evaporation or selective oxidation easily occur under hot environment and then causes material to decompose/phase in version, therefore MAX phase ceramics surface modification treatment is also very necessary.
Differential arc oxidation is that the metals such as a kind of Al, Ti, Mg, Nb, Zr, Ta or its alloy are placed in special electrolytic solution, differential of the arc effect is utilized to make material surface produce small spark discharge spot, under thermochemistry, plasma chemistry and electrochemical acting in conjunction, in the new technology of surface in situ growth oxide ceramic membrane.Utilize this technology can at valve metal and the different ceramic film of alloy surface growth performance thereof, as: wear-resisting, corrosion-resistant, heat shock resistance protective membrane and there is katalysis, or function ceramics rete to gas sensitization compatible with biophase.And micro-arc oxidation process process is simple, easy to operate, can form uniform rete, clean environment firendly, make this technology have broad application prospects on complex-shaped workpiece.
Although differential arc oxidization technique has been widely used in the alloy surface process such as Al, Mg, Ti, seldom study for the carbide of routine or nitride ceramics.This is because: first, compared with oxide ceramics, conventional carbide or nitride ceramics inherently have that hardness is high, the feature of Heat stability is good, carry out differential arc oxidation process and lack necessity; Secondly, most conventional carbide or nitride ceramics are isolator at low temperatures, are difficult to realize plasma discharge, cannot carry out differential arc oxidation process.
Summary of the invention
The object of the present invention is to provide the treatment process of a kind of MAX phase ceramics and composite material surface modification thereof; at MAX phase ceramics or its composite material surface growth in situ composite oxides rete; significantly improve its surface hardness, anticorrosive and wear-resistingly undermine the performances such as high-temperature stability; and preparation method's technique is simple; environmental protection, can mass-producing application.
Technical scheme of the present invention is as follows:
A treatment process for MAX phase ceramics and composite material surface modification thereof, adopt water-proof abrasive paper the surface of test piece of MAX phase ceramics or its matrix material to be polished flat, then the peace and quiet surface of de-oiling degreasing, finally dries; Immersed in electrolytic solution by test specimen after cleaning and carry out differential arc oxidation, electrolytic solution used is one or more composite electrolytic solutions of silicate systems, phosphate system, aluminates system; Power supply is the pulse power, and electrolyte temperature controls between 25 ~ 50 DEG C, and the time is 10 ~ 60 minutes, and final voltage is 200 ~ 700V; Use distilled water flushing workpiece surface afterwards, then use hot blast drying.
Described MAX phase ceramics and the treatment process of composite material surface modification thereof, MAX phase ceramics refers to that M is the ternary layered carbon/nitride of valve metal element, and molecular formula is expressed as M
n+1aX
n, M is transiting group metal elements, and A is main group element, and mainly refer to III A and IV A race element, X is C or N element, and n is the integer of 1 ~ 6; MAX phase ceramics matrix material refers to, is base with above-mentioned MAX phase ceramics, adds the matrix material of solid solution element or second-phase.
Described MAX phase ceramics and the treatment process of composite material surface modification thereof, valve metal element is Ti, Mg, Al, Zr, Nb or Ta etc.
Described MAX phase ceramics and the treatment process of composite material surface modification thereof, MAX phase ceramics comprises: Ti
3siC
2, Ti
3alC
2, Ti
2alC, Ti
2geC, Ti
2snC, Ti
2alN, Nb
2alC, Nb
2gaC, Nb
4alC
3, Ta
2alC or Zr
2snC etc.; MAX phase ceramics matrix material comprises: Ti
3(Si, Al) C
2, (Ti, Nb)
3siC
2, (Ti, Nb)
3(Si, Al) C
2, Ti
3siC
2-SiC, Ti
3siC
2-Al
2o
3, Ti
3siC
2-Ti
5si
3or Ti
3alC
2-TiB
2deng.
Described MAX phase ceramics and the treatment process of composite material surface modification thereof, relative density >=85% of MAX phase ceramics or its matrix material, room temperature resistivity is lower than 1 Ω m.
Described MAX phase ceramics and the treatment process of composite material surface modification thereof, electrolytic solution comprises: the Na of 1 ~ 40g/L
2siO
3, (NaPO
3)
6, NaAlO
2one or more, the KF of the NaOH of 3 ~ 25g/L, 5 ~ 30g/L, the deionized water of surplus.
Described MAX phase ceramics and the treatment process of composite material surface modification thereof, add additive in the electrolytic solution as required, additive accounts for 2 ~ 40% of electrolytic solution gross weight, and additive is mainly soluble salt or organism.
Described MAX phase ceramics and the treatment process of composite material surface modification thereof, additive is suppress specimen surface point discharge, the KF improving electrolytic solution stability, glycerine or C
3h
8o
3; Or additive is NaOH, KOH, NaF or NaAlO of contributing to electric discharge, improving electrical conductivity of solution
2; Or additive is the Na improving ceramic dense, corrosion resisting property
2wO
4or montmorillonite; Or additive is the Cu that can adjust ceramic layer color
2+, Ni
2+or Cr
3+deng composition; Or additive is the H improving film forming speed
2o
2deng.
Described MAX phase ceramics and the treatment process of composite material surface modification thereof, the power supply used during differential arc oxidation is the pulse power, adopts the method for boosted voltage gradually, and final voltage controls at 300 ~ 600V, range of frequency 500 ~ 2000Hz, current density 5 ~ 50mA/cm
2, dutycycle 10 ~ 40%; Electrolytic solution carries out induction stirring always, and temperature maintains 30 ~ 40 DEG C, 20 ~ 60 minutes treatment times.
Described MAX phase ceramics and the treatment process of composite material surface modification thereof, generate the mixed oxide rete of one deck M and A through differential arc oxidation process rear surface, be combined closely with matrix, and maximum ga(u)ge 200 ~ 300 μm, hardness reaches 5 ~ 35GPa.
Design philosophy of the present invention is as follows:
Consider that MAX phase ceramics is with metal and ceramic special performance, particularly electroconductibility and can oxidized property, the present invention proposes MAX ceramic composite materials and carries out the processing method that differential arc oxidation treat surface forms composite oxides rete, not only can widen the use field of differential arc oxidization technique, the performance of MAX phase can be promoted further simultaneously, expand its Application Areas, therefore there is obvious practical value.Adopt present method can MAX phase ceramics and composite material surface thereof prepare even compact with matrix in conjunction with good oxide membranous layer.
Advantage of the present invention and beneficial effect are:
1, the method for MAX phase ceramics of the present invention and composite material surface modification thereof can be the oxide membranous layer that the MAX phase ceramics of valve metal and composite material surface preparation thereof have property at M.
2, the present invention has widened the use field of differential arc oxidization technique.
3, the oxide film layer thickness utilizing the present invention to obtain is even, compact structure, and smooth surface is good with basal body binding force.
4, utilize the present invention to prepare one deck mixed oxide rete at MAX phase ceramics and composite material surface thereof, its surface hardness, anticorrosive and wear-resistingly undermine the performances such as high-temperature stability can be significantly improved.
Accompanying drawing explanation
Fig. 1 is the Ti after differential arc oxidation process
3alC
2surface SEM shape appearance figure.
Fig. 2 is the Ti after differential arc oxidation process
3alC
2cross Section Morphology figure.
Fig. 3 is the Ti after differential arc oxidation process
3(Si
0.95al
0.05) C
2surface SEM shape appearance figure.
Fig. 4 is the Ti after differential arc oxidation process
3(Si
0.95al
0.05) C
2cross Section Morphology figure.
Embodiment
In a specific embodiment, the treatment process of MAX phase ceramics of the present invention and composite material surface modification thereof, MAX phase ceramics refers to that M is ternary layered carbon/nitride (the molecular formula M of valve metal element (Ti, Mg, Al, Zr, Nb, Ta etc.)
n+1aX
n, M is transiting group metal elements, A is main group element (mainly refer to III A and IV A race element), and X is C or N element, and n is the integer of 1 ~ 6), particularly as Ti
3siC
2, Ti
3alC
2, Ti
2alC, Ti
2geC, Ti
2snC, Ti
2alN, Nb
2alC, Nb
2gaC, Nb
4alC
3, Ta
2alC, Zr
2snC etc.; MAX phase ceramics matrix material refers to, add the matrix material being base with above-mentioned MAX of solid solution element or second-phase, particularly as Ti
3(Si, Al) C
2, (Ti, Nb)
3siC
2, (Ti, Nb)
3(Si, Al) C
2, Ti
3siC
2-SiC, Ti
3siC
2-Al
2o
3, Ti
3siC
2-Ti
5si
3, Ti
3alC
2-TiB
2deng.MAX phase clean for surfacing and composite material test piece thereof are immersed in micro-arc oxidation electrolyte, smooth surface can be prepared, with matrix in conjunction with good composite oxides rete, concrete steps are as follows:
Adopt water-proof abrasive paper surface of test piece to be polished flat, then use the peace and quiet surfaces of de-oiling degreasing such as acetone, alcohol, deionized water respectively, finally dry.Immersed in electrolytic solution by test specimen after cleaning and carry out differential arc oxidation, electrolytic solution used can be silicate systems, phosphate system, aluminates system or composite electrolytic solution.Electrolytic solution comprises: the Na of 1 ~ 40g/L
2siO
3(silicate systems)/(NaPO
3)
6(phosphate system)/NaAlO
2(aluminates system), the KF of the NaOH of 3 ~ 25g/L, 5 ~ 30g/L, the deionized water of surplus, and add appropriate additive as required.Power supply is the pulse power, and electrolyte temperature controls between 25 ~ 50 DEG C, and the time is 10 ~ 60 minutes, adopts the method for boosted voltage gradually, and final voltage is 200 ~ 700V.Use distilled water flushing workpiece surface afterwards, then use hot blast drying.
Differential arc oxidation method is adopted to carry out surface modification to MAX phase ceramics and matrix material thereof in the present invention, at the growing mixed oxide membranous layer of its surface in situ, its surface hardness, anticorrosive and wear-resistingly undermine the performances such as high-temperature stability can be significantly improved, and then promote the potential using value of MAX phase.The method cost is low, and technological process is simple, clean environment firendly.
Below, the present invention is described in further detail by embodiment and accompanying drawing.But these embodiments must not be used for being interpreted as limiting the scope of the invention, all within the scope of technical solution of the present invention basic ideas or the change being equal to technical solution of the present invention be in essence protection scope of the present invention.
Embodiment 1
Test specimen is Ti
3alC
2, the peace and quiet surfaces of de-oiling degreasing such as acetone, alcohol, deionized water, through the polishing of 600 ~ 2000# water-proof abrasive paper, are then used respectively in surface, dry.Immersed in anolyte by test specimen after cleaning, solution is by the Na of 15g/L again
2siO
3, the KF of NaOH, 8g/L of 6g/L, the deionized water composition of surplus.Adopt the pulse power, current density 20mA/cm
2, frequency 600Hz, dutycycle 30%, electrolytic solution carries out induction stirring always, and temperature maintains 40 DEG C, handling duration 15min, final voltage 400V.Sample distilled water rinsing afterwards also dries up, and oxidation film layer is primarily of Al
2o
3and TiO
2group and part Al
2tiO
5composition.
Prepared oxide membranous layer surface topography is shown in accompanying drawing 1.As seen from Figure 1, Ti after differential arc oxidation
3alC
2surface topography occurs obviously to change, and define the ceramic layer of one deck porous, surface ceramii layer is smooth, aperture fine uniform.
As shown in Figure 2, from the Ti after differential arc oxidation process
3alC
2cross Section Morphology figure can find out, oxidation film layer is combined with matrix well, and layer inner tissue is fine and close in perforation, and thicknesses of layers is 2.8 μm.Microhardness tester are utilized to measure, film hardness 10.0GPa.
Embodiment 2
Test specimen is Ti
3(Si
0.95al
0.05) C
2, the peace and quiet surfaces of de-oiling degreasing such as acetone, alcohol, deionized water, through the polishing of 600 ~ 2000# water-proof abrasive paper, are used respectively afterwards in surface, dry.Immerse in anolyte by workpiece again, solution is by the Na of 30g/L
2siO
3, the KF of NaOH, 20g/L of 10g/L, the deionized water composition of surplus.Adopt the pulse power, current density 35mA/cm
2, frequency 800Hz, dutycycle 35%, electrolytic solution carries out induction stirring always, and temperature maintains 30 DEG C, handling duration 20min, final voltage 500V.Sample is with drying up from distilled water rinsing afterwards, and oxidation film layer is primarily of TiO
2with part Al
2tiO
5composition, a small amount of Si is with amorphous SiO
2form exists.Thicknesses of layers is 4 μm, hardness 9.5GPa.
Preparation-obtained oxide film surface topography is shown in accompanying drawing 3.As seen from Figure 3, Ti after differential arc oxidation
3(Si
0.95al
0.05) C
2surface topography changes, and define the ceramic layer of one deck porous, ceramic layer is smooth, aperture fine uniform.
As shown in Figure 4, as can be seen from the Cross Section Morphology after differential arc oxidation process, oxidation film layer is combined with matrix well, and layer inner tissue is fine and close in perforation.
Embodiment 3
Test specimen is Ti
3siC
2-2vol.%Al
2o
3, surface, through 600 ~ 2000# sand papering, by acetone alcohol deionized water clean surface respectively, is dried.Immerse in anolyte by sample again, solution is by the NaAlO of 20g/L
2, 4g/L the 30wt%H of KF, 3mL/L of NaOH, 15g/L
2o
2(its effect reacts in the solution to provide film forming necessary O
2, improve film forming speed and thicknesses of layers), the deionized water composition of surplus adopts the pulse power, current density 40mA/cm
2, frequency 1000Hz, dutycycle 30%, electrolytic solution carries out induction stirring always, and temperature maintains 45 DEG C, handling duration 60min, final voltage 600V.Sample distilled water rinsing afterwards also dries up.Oxidation film layer thickness is 50 μm, and surface uniform, is combined well with matrix.
To sum up three embodiments, its design parameter is as follows:
Table 1
Test specimen composition | Ti 3AlC 2 | Ti 3(Si,Al)C 2 | Ti 3SiC 2-2vol.%Al 2O 3 |
Electrolytic solution | Silicate systems | Silicate systems | Aluminates system |
Thicknesses of layers | 2.8μm | 4μm | 50μm |
Rete main component | TiO 2、Al 2O 3、Al 2TiO 5 | TiO 2、SiO 2、Al 2TiO 5 | TiO 2、SiO 2、Al 2TiO 5 |
Film hardness | 10.0GPa | 9.5GPa | 12.3GPa |
Embodiment result shows, the present invention adopts microarc oxidation treatment process, can to prepare with matrix in conjunction with good, fine and close combined oxidation rete in ceramic material surfaces, the surface hardness, anticorrosive and wear-resistingly undermine the performances such as high high-temp stability improving the MAX phase material having pottery and metal premium properties concurrently can be shown.
Claims (10)
1. a treatment process for MAX phase ceramics and composite material surface modification thereof, is characterized in that, adopt water-proof abrasive paper the surface of test piece of MAX phase ceramics or its matrix material to be polished flat, then the peace and quiet surface of de-oiling degreasing, finally dries; Immersed in electrolytic solution by test specimen after cleaning and carry out differential arc oxidation, electrolytic solution used is one or more composite electrolytic solutions of silicate systems, phosphate system, aluminates system; Power supply is the pulse power, and electrolyte temperature controls between 25 ~ 50 DEG C, and the time is 10 ~ 60 minutes, and final voltage is 200 ~ 700V; Use distilled water flushing workpiece surface afterwards, then use hot blast drying.
2., according to the treatment process of the MAX phase ceramics described in claims 1 and composite material surface modification thereof, it is characterized in that, MAX phase ceramics refers to that M is the ternary layered carbon/nitride of valve metal element, and molecular formula is expressed as M
n+1aX
n, M is transiting group metal elements, and A is main group element, and mainly refer to III A and IV A race element, X is C or N element, and n is the integer of 1 ~ 6; MAX phase ceramics matrix material refers to, is base with above-mentioned MAX phase ceramics, adds the matrix material of solid solution element or second-phase.
3., according to the treatment process of the MAX phase ceramics described in claims 2 and composite material surface modification thereof, it is characterized in that, valve metal element is Ti, Mg, Al, Zr, Nb or Ta etc.
4., according to the treatment process of the MAX phase ceramics described in claims 2 and composite material surface modification thereof, it is characterized in that, MAX phase ceramics comprises: Ti
3siC
2, Ti
3alC
2, Ti
2alC, Ti
2geC, Ti
2snC, Ti
2alN, Nb
2alC, Nb
2gaC, Nb
4alC
3, Ta
2alC or Zr
2snC etc.; MAX phase ceramics matrix material comprises: Ti
3(Si, Al) C
2, (Ti, Nb)
3siC
2, (Ti, Nb)
3(Si, Al) C
2, Ti
3siC
2-SiC, Ti
3siC
2-Al
2o
3, Ti
3siC
2-Ti
5si
3or Ti
3alC
2-TiB
2deng.
5., according to the treatment process of the MAX phase ceramics described in claims 1 and composite material surface modification thereof, it is characterized in that, relative density >=85% of MAX phase ceramics or its matrix material, room temperature resistivity is lower than 1 Ω m.
6., according to the treatment process of the MAX phase ceramics described in claims 1 and composite material surface modification thereof, it is characterized in that, electrolytic solution comprises: the Na of 1 ~ 40g/L
2siO
3, (NaPO
3)
6, NaAlO
2one or more, the KF of the NaOH of 3 ~ 25g/L, 5 ~ 30g/L, the deionized water of surplus.
7. according to the treatment process of the MAX phase ceramics described in claims 6 and composite material surface modification thereof, it is characterized in that, add additive in the electrolytic solution as required, additive accounts for 2 ~ 40% of electrolytic solution gross weight, and additive is mainly soluble salt or organism.
8. according to the treatment process of the MAX phase ceramics described in claims 7 and composite material surface modification thereof, it is characterized in that, additive is suppress specimen surface point discharge, the KF improving electrolytic solution stability, glycerine or C
3h
8o
3; Or additive is NaOH, KOH, NaF or NaAlO of contributing to electric discharge, improving electrical conductivity of solution
2; Or additive is the Na improving ceramic dense, corrosion resisting property
2wO
4or montmorillonite; Or additive is the Cu that can adjust ceramic layer color
2+, Ni
2+or Cr
3+deng composition; Or additive is the H improving film forming speed
2o
2deng.
9. according to the treatment process of the MAX phase ceramics described in claims 1 and composite material surface modification thereof, it is characterized in that, the power supply used during differential arc oxidation is the pulse power, adopt the method for boosted voltage gradually, final voltage controls at 300 ~ 600V, range of frequency 500 ~ 2000Hz, current density 5 ~ 50mA/cm
2, dutycycle 10 ~ 40%; Electrolytic solution carries out induction stirring always, and temperature maintains 30 ~ 40 DEG C, 20 ~ 60 minutes treatment times.
10. according to the treatment process of the MAX phase ceramics described in claims 1 and composite material surface modification thereof, it is characterized in that, generate the mixed oxide rete of one deck M and A through differential arc oxidation process rear surface, be combined with matrix closely, maximum ga(u)ge 200 ~ 300 μm, hardness reaches 5 ~ 35GPa.
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