CN102703954A - Preparation method for micro-arc oxidized ceramic layer on surface of TiC particle enhanced titanium-base compound material - Google Patents
Preparation method for micro-arc oxidized ceramic layer on surface of TiC particle enhanced titanium-base compound material Download PDFInfo
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- CN102703954A CN102703954A CN2012102066593A CN201210206659A CN102703954A CN 102703954 A CN102703954 A CN 102703954A CN 2012102066593 A CN2012102066593 A CN 2012102066593A CN 201210206659 A CN201210206659 A CN 201210206659A CN 102703954 A CN102703954 A CN 102703954A
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Abstract
The invention provides a preparation method for a micro-arc oxidized ceramic layer on a surface of a TiC particle enhanced titanium-base compound material and relates to a method for micro-arc oxidizing a ceramic layer on the surface of a titanium-base compound material. The preparation method provided by the invention is used for solving the technical problem of the poor abrasion resistance of the present TiC particle enhanced titanium-base compound material. The preparation method comprises the following steps: placing the TiC particle enhanced titanium-base compound material into an electrolyte; adopting a bidirectional pulse power supply for treating for 3-30min; washing for 3-5 times; and drying, thereby obtaining the micro-arc oxidized ceramic layer on the surface of the TiC particle enhanced titanium-base compound material. According to the method for micro-arc oxidizing provided by the invention, the problems that the TiC ceramic enhancing particles have poor discharging uniformity during a micro-arc oxidizing discharging process for the surface of the compound material and the coating completeness is inferior are simply and effectively solved, and the abrasion resistance of the surface of the compound material is obviously enhanced.
Description
Technical field
The present invention relates to a kind of method at the titanium matrix composite micro-arc oxidation ceramic layer on surface.
Background technology
The TiC granule intensified titanium-base compound material pays close attention to because of its excellent obdurability and high thermal resistance have received widely, but its relatively poor wear resistance has directly restricted its application as abrasion-proof structure in fields such as automobile making, aerospace.Through differential arc oxidation method, generate ceramic coating at composite material surface, can effectively improve its wear resistance.Further promote it as the application in high-strength, the high-temperature wearable structural part.
Differential arc oxidation is that valve metals such as Ti, Mg, Al or its alloy are placed aqueous electrolyte liquid; Utilize electrochemical method; In the surface micropore of this material, produce the spark discharge spot, under thermochemistry, plasma chemistry and electrochemical acting in conjunction, original position generates the method for ceramic membrane.Because TiC ceramic enhancement phase and titanium, titanium alloy substrate physical chemistry of metal character differ greatly; Can directly have influence on the homogeneity of discharging in the differential arc oxidation process and the integrity of coating, so also directly do not carry out the report that differential arc oxidation is handled both at home and abroad up to now about the TiC granule intensified titanium-base compound material.
Summary of the invention
The objective of the invention is provides a kind of preparation method of TiC granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface in order to solve the technical problem that existing TiC granule intensified titanium-base compound material wears no resistance.
The preparation method of iC granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface of the present invention carries out according to the following steps:
One, the TiC granule intensified titanium-base compound material is put into electrolytic solution; With the TiC granule intensified titanium-base compound material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 10～60 ℃; Adopting the bidirectional pulse power supply, is that 200～800V, negative pulse voltage are that 0～400V, positive pulse operating frequency are that 200～2000Hz, negative pulse operating frequency are that 200～2000Hz, dutycycle are under 4～20% the condition at positive pulse voltage, handles 3～30min;
The TiC granule intensified titanium-base compound material that two, will pass through the step 1 processing washes 3～5 times, and drying promptly gets micro-arc oxidation ceramic layer on surface TiC granule intensified titanium-base compound material;
Electrolytic solution described in the step 1 is made up of water glass, sodium aluminate, sodium phosphate, ethanol and deionized water, and electrolytic solution mesosilicic acid na concn is 3～35g/L, and concentration of sodium aluminate is 3～60g/L, and sodium phosphate concentration is 3～40g/L, and alcohol concn is 5～20ml/L.
TiC particle as wild phase in the granule intensified titanium-base compound material of TiC described in the step 1 is with micron order or nano level; Matrix in the TiC granule intensified titanium-base compound material is titanium, TC3 titanium alloy or TC4 titanium alloy, and the volume content of TiC is 3%～20% in the TiC granule intensified titanium-base compound material.
The present invention can directly carry out differential arc oxidation on TiC granule intensified titanium-base compound material surface and generate ceramic layer, and through the scratch method test, the bonding force of arc differential oxide ceramic layer and titanium alloy is difficult for peeling off, coming off greater than 75N; Ceramic layer thickness can be controlled between 10～40 μ m, has comparatively excellent abrasive; And more still keep the high value of former matrix material through the mechanical property of the TiC of differential arc oxidation granule intensified titanium-base compound material.When not passing through differential arc oxidation, the TiC granule intensified titanium-base compound material is 0.7～0.8 with GCr 15 steel balls to the frictional coefficient that grinds directly, and the volume wear rate is 20 * 10
-6～100 * 10
-6Mm
3(mN)
-1, and after surface by micro-arc oxidation was handled, its frictional coefficient reduced to 0.5～0.7, the volume wear rate reduces to 0.02 * 10
-6～0.3 * 10
-6Mm
3(mN)
-1, be merely the per mille of former matrix material, can accomplish zero wearing and tearing basically.
Differential arc oxidation method of the present invention is simple; Do not receive the influence of TiC granule intensified titanium-base compound material workpiece size, shape; Environmentally safe; Solve TiC pottery enhanced granule effectively to discharge lack of homogeneity and the bad problem of coating integrity in the composite material surface differential arc oxidation discharge process, significantly strengthened the wear resistance of composite material surface.
Description of drawings
Fig. 1 is the cross section shape appearance figure of arc differential oxide ceramic layer in the experiment 11 gained arc differential oxide ceramic layer TiC/TC4 matrix materials.
Embodiment
Technical scheme of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of this embodiment TiC granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface carries out according to the following steps:
One, the TiC granule intensified titanium-base compound material is put into electrolytic solution; With the TiC granule intensified titanium-base compound material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 10～60 ℃; Adopting the bidirectional pulse power supply, is that 200～800V, negative pulse voltage are that 0～400V, positive pulse operating frequency are that 200～2000Hz, negative pulse operating frequency are that 200～2000Hz, dutycycle are under 4～20% the condition at positive pulse voltage, handles 3～30min;
The TiC granule intensified titanium-base compound material that two, will pass through the step 1 processing washes 3～5 times, and drying promptly gets arc differential oxide ceramic layer TiC granule intensified titanium-base compound material;
Electrolytic solution described in the step 1 is made up of water glass, sodium aluminate, sodium phosphate, ethanol and deionized water, and electrolytic solution mesosilicic acid na concn is 3～35g/L, and concentration of sodium aluminate is 3～60g/L, and sodium phosphate concentration is 3～40g/L, and alcohol concn is 5～20ml/L.
High base strength in arc differential oxide ceramic layer in the employing scratch method test arc differential oxide ceramic layer TiC granule intensified titanium-base compound material and the titanium matrix composite, its bonding force is difficult for peeling off, coming off greater than 90N; Arc differential oxide ceramic layer thickness is even, is 10～40 μ m, has the advantages of good abrasion performance, and arc differential oxide ceramic layer and GCr 15 steel balls are 0.6～0.7 to the frictional coefficient of mill, and the volume wear rate is 0.10 * 10
-6～0.20 * 10
-6Mm
3(mN)
-1, being merely one of three percentages of former matrix material (TiC granule intensified titanium-base compound material), wear resisting property is significantly improved.
Embodiment two: this embodiment and embodiment one are different be in the granule intensified titanium-base compound material of TiC described in the step 1 as the TiC particle of wild phase for micron order or nano level; Matrix in the TiC granule intensified titanium-base compound material is titanium, TC3 titanium alloy or TC4 titanium alloy, and the volume content of TiC is 3%～20% in the TiC granule intensified titanium-base compound material.Other is identical with embodiment one.
Embodiment three: what this embodiment was different with embodiment one or two is that the voltage of positive pulse described in the step 1 is 300～700V.Other is identical with embodiment one or two.
Embodiment four: what this embodiment was different with one of embodiment one to three is that the voltage of positive pulse described in the step 1 is 500～600V.Other is identical with one of embodiment one to three.
Embodiment five: what this embodiment was different with one of embodiment one to four is that negative pulse voltage described in the step 1 is 0～300V.Other is identical with one of embodiment one to four.
Embodiment six: what this embodiment was different with one of embodiment one to five is that negative pulse voltage described in the step 1 is 200V.Other is identical with one of embodiment one to five.
Embodiment seven: what this embodiment was different with one of embodiment one to six is that the operating frequency of positive pulse described in the step 1 is 400～1200Hz.Other is identical with one of embodiment one to six.
Embodiment eight: what this embodiment was different with one of embodiment one to seven is that the operating frequency of negative pulse described in the step 1 is 1000Hz.Other is identical with one of embodiment one to seven.
Embodiment nine: what this embodiment was different with one of embodiment one to eight is that dutycycle described in the step 1 is 4～16%.Other is identical with one of embodiment one to eight.
Embodiment ten: what this embodiment was different with one of embodiment one to nine is that the temperature of exsiccant described in the step 2 is 40～80 ℃.Other is identical with one of embodiment one to nine.
Adopt following experimental verification effect of the present invention:
Experiment one:
One, be that 6% ratio takes by weighing the TC4 powder and TiC powder (micron order) is a raw material according to TiC volumetric solid concentration in the TiC/TC4 matrix material; In glove box under the Ar atmosphere protection condition; Guarantee that ball-to-powder weight ratio is 10: 1; TC4 powder, TiC powder and GCr15 mill ball are packed in the batch mixing bottle, and the sealing back is to mix with ball mill under the condition of 120r/min at rotating speed, and mixing time is 24h.The mixed powder graphite jig of packing into is colded pressing, and is that insulation 1h obtains the TiC/TC4 matrix material under the condition of 20MPa, argon atmospher protection at 1200 ℃, pressure.
Two, the TiC/TC4 matrix material is put into electrolytic solution; With the TiC/TC4 matrix material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 60 ℃; Adopting the bidirectional pulse power supply, is that 200～600V, negative pulse voltage are that 0～50V, positive pulse operating frequency are that 600～1600Hz, negative pulse operating frequency are that 600～1600Hz, dutycycle are under 4～12% the condition at positive pulse voltage, handles 10～30min;
The TiC/TC4 matrix material that three, will pass through the step 2 processing washes 3～5 times, and drying promptly gets arc differential oxide ceramic layer TiC/TC4 matrix material;
With the bonding strength of arc differential oxide ceramic layer TiC/TC4 composite material by adopting scratch method test arc differential oxide ceramic layer and TC4 alloy, its bonding force is difficult for peeling off, coming off greater than 90N; Arc differential oxide ceramic layer thickness is even, is 10～40 μ m, has the advantages of good abrasion performance, and arc differential oxide ceramic layer and GCr 15 steel balls are 0.6～0.7 to the frictional coefficient of mill, and the volume wear rate is 0.10 * 10
-6～0.20 * 10
-6Mm
3(mN)
-1, being merely one of three percentages of former matrix material, wear resisting property is significantly improved.
Experiment two:
One, be that 9% ratio takes by weighing the TC4 powder and TiC powder (micron order) is a raw material according to TiC volumetric solid concentration in the TiC/TC4 matrix material; In glove box under the Ar atmosphere protection condition; Guarantee that ball-to-powder weight ratio is 10: 1; TC4 powder, TiC powder and GCr15 mill ball are packed in the batch mixing bottle, and the sealing back is to mix with ball mill under the condition of 120r/min at rotating speed, and mixing time is 24h.The mixed powder graphite jig of packing into is colded pressing, and is that insulation 1h obtains the TiC/TC4 matrix material under the condition of 20MPa, argon atmospher protection at 1200 ℃, pressure.
Two, the TiC/TC4 matrix material is put into electrolytic solution; With the TiC/TC4 matrix material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 60 ℃; Adopting the bidirectional pulse power supply, is that 200～600V, negative pulse voltage are that 0～50V, positive pulse operating frequency are that 600～1600Hz, negative pulse operating frequency are that 600～1600Hz, dutycycle are under 4～12% the condition at positive pulse voltage, handles 10～30min;
The TiC/TC4 matrix material that three, will pass through the step 2 processing washes 5 times, and drying promptly gets arc differential oxide ceramic layer TiC/TC4 matrix material;
With the bonding strength of arc differential oxide ceramic layer TiC/TC4 composite material by adopting scratch method test arc differential oxide ceramic layer and TC4 alloy, its bonding force is difficult for peeling off, coming off greater than 85N; Arc differential oxide ceramic layer thickness is even, is 10～40 μ m, has the advantages of good abrasion performance, and arc differential oxide ceramic layer and GCr 15 steel balls are 0.6～0.7 to the frictional coefficient of mill, and the volume wear rate is 0.05 * 10
-6～0.15 * 10
-6Mm
3(mN)
-1
Experiment three:
One, be that 12% ratio takes by weighing the TC4 powder and TiC powder (micron order) is a raw material according to TiC volumetric solid concentration in the TiC/TC4 matrix material; In glove box under the Ar atmosphere protection condition; Guarantee that ball-to-powder weight ratio is 10: 1; TC4 powder, TiC powder and GCr15 mill ball are packed in the batch mixing bottle, and the sealing back is to mix with ball mill under the condition of 120r/min at rotating speed, and mixing time is 24h.The mixed powder graphite jig of packing into is colded pressing, and is that insulation 1h obtains the TiC/TC4 matrix material under the condition of 20MPa, argon atmospher protection at 1200 ℃, pressure.
Two, the TiC/TC4 matrix material is put into electrolytic solution; With the TiC/TC4 matrix material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 60 ℃; Adopting the bidirectional pulse power supply, is that 200～600V, negative pulse voltage are that 0～50V, positive pulse operating frequency are that 600～1600Hz, negative pulse operating frequency are that 600～1600Hz, dutycycle are under 4～12% the condition at positive pulse voltage, handles 10～30min;
The TiC/TC4 matrix material that three, will pass through the step 2 processing washes 3～5 times, and drying promptly gets arc differential oxide ceramic layer TiC/TC4 matrix material;
With the bonding strength of arc differential oxide ceramic layer TiC/TC4 composite material by adopting scratch method test arc differential oxide ceramic layer and TC4 alloy, its bonding force is difficult for peeling off, coming off greater than 80N; Arc differential oxide ceramic layer thickness is even, is 10～40 μ m, has the advantages of good abrasion performance, and arc differential oxide ceramic layer and GCr 15 steel balls are 0.65～0.75 to the frictional coefficient of mill, and the volume wear rate is 0.02 * 10
-6～0.10 * 10
-6Mm
3(mN)
-1
Experiment four:
One, be that 15% ratio takes by weighing the TC4 powder and TiC powder (micron order) is a raw material according to TiC volumetric solid concentration in the TiC/TC4 matrix material; In glove box under the Ar atmosphere protection condition; Guarantee that ball-to-powder weight ratio is 10: 1; TC4 powder, TiC powder and GCr15 mill ball are packed in the batch mixing bottle, and the sealing back is to mix with ball mill under the condition of 120r/min at rotating speed, and mixing time is 24h.The mixed powder graphite jig of packing into is colded pressing, and is that insulation 1h obtains the TiC/TC4 matrix material under the condition of 20MPa, argon atmospher protection at 1200 ℃, pressure.
Two, the TiC/TC4 matrix material is put into electrolytic solution; With the TiC/TC4 matrix material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 60 ℃; Adopting the bidirectional pulse power supply, is that 200～600V, negative pulse voltage are that 0～50V, positive pulse operating frequency are that 600～1600Hz, negative pulse operating frequency are that 600～1600Hz, dutycycle are under 4～12% the condition at positive pulse voltage, handles 10～30min;
The TiC/TC4 matrix material that three, will pass through the step 2 processing washes 3 times, and drying promptly gets arc differential oxide ceramic layer TiC/TC4 matrix material;
With the bonding strength of arc differential oxide ceramic layer TiC/TC4 composite material by adopting scratch method test arc differential oxide ceramic layer and TC4 alloy, its bonding force is difficult for peeling off, coming off greater than 75N; Arc differential oxide ceramic layer thickness is even, is 10～40 μ m, has the advantages of good abrasion performance, and arc differential oxide ceramic layer and GCr 15 steel balls are 0.65～0.75 to the frictional coefficient of mill, and the volume wear rate is 0.02 * 10
-6～0.05 * 10
-6Mm
3(mN)
-1
Experiment five:
One, be that 6% ratio takes by weighing the TC4 powder and TiC powder (micron order) is a raw material according to TiC volumetric solid concentration in the TiC/TC4 matrix material; In glove box under the Ar atmosphere protection condition; Guarantee that ball-to-powder weight ratio is 10: 1; TC4 powder, TiC powder and GCr15 mill ball are packed in the batch mixing bottle, and the sealing back is to mix with ball mill under the condition of 120r/min at rotating speed, and mixing time is 24h.The mixed powder graphite jig of packing into is colded pressing, and is that insulation 1h obtains the TiC/TC4 matrix material under the condition of 20MPa, argon atmospher protection at 1200 ℃, pressure.
Two, the TiC/TC4 matrix material is put into electrolytic solution; With the TiC/TC4 matrix material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 30 ℃; Adopting the bidirectional pulse power supply, is that 300～500V, negative pulse voltage are that 20～100V, positive pulse operating frequency are that 1000Hz, negative pulse operating frequency are that 1000Hz, dutycycle are under 20% the condition at positive pulse voltage, handles 30min;
The TiC/TC4 matrix material that three, will pass through the step 2 processing washes 3～5 times, and drying promptly gets arc differential oxide ceramic layer TiC/TC4 matrix material;
With the bonding strength of arc differential oxide ceramic layer TiC/TC4 composite material by adopting scratch method test arc differential oxide ceramic layer and TC4 alloy, its bonding force is difficult for peeling off, coming off greater than 95N; Arc differential oxide ceramic layer thickness is even, is 15～40 μ m, has the advantages of good abrasion performance, and arc differential oxide ceramic layer and GCr 15 steel balls are 0.55～0.65 to the frictional coefficient of mill, and the volume wear rate is 0.10 * 10
-6～0.20 * 10
-6Mm
3(mN)
-1
Experiment six:
One, be that 9% ratio takes by weighing the TC4 powder and TiC powder (micron order) is a raw material according to TiC volumetric solid concentration in the TiC/TC4 matrix material; In glove box under the Ar atmosphere protection condition; Guarantee that ball-to-powder weight ratio is 10: 1; TC4 powder, TiC powder and GCr15 mill ball are packed in the batch mixing bottle, and the sealing back is to mix with ball mill under the condition of 120r/min at rotating speed, and mixing time is 24h.The mixed powder graphite jig of packing into is colded pressing, and is that insulation 1h obtains the TiC/TC4 matrix material under the condition of 20MPa, argon atmospher protection at 1200 ℃, pressure.
Two, the TiC/TC4 matrix material is put into electrolytic solution; With the TiC/TC4 matrix material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 30 ℃; Adopting the bidirectional pulse power supply, is that 300～500V, negative pulse voltage are that 20～100V, positive pulse operating frequency are that 1000Hz, negative pulse operating frequency are that 1000Hz, dutycycle are under 20% the condition at positive pulse voltage, handles 30min;
The TiC/TC4 matrix material that three, will pass through the step 2 processing washes 3～5 times, and drying promptly gets arc differential oxide ceramic layer TiC/TC4 matrix material;
With the bonding strength of arc differential oxide ceramic layer TiC/TC4 composite material by adopting scratch method test arc differential oxide ceramic layer and TC4 alloy, its bonding force is difficult for peeling off, coming off greater than 90N; Arc differential oxide ceramic layer thickness is even, is 15～40 μ m, has the advantages of good abrasion performance, and arc differential oxide ceramic layer and GCr 15 steel balls are 0.55～0.65 to the frictional coefficient of mill, and the volume wear rate is 0.05 * 10
-6～0.15 * 10
-6Mm
3(mN)
-1
Experiment seven:
One, be that 12% ratio takes by weighing the TC4 powder and TiC powder (micron order) is a raw material according to TiC volumetric solid concentration in the TiC/TC4 matrix material; In glove box under the Ar atmosphere protection condition; Guarantee that ball-to-powder weight ratio is 10: 1; TC4 powder, TiC powder and GCr15 mill ball are packed in the batch mixing bottle, and the sealing back is to mix with ball mill under the condition of 120r/min at rotating speed, and mixing time is 24h.The mixed powder graphite jig of packing into is colded pressing, and is that insulation 1h obtains the TiC/TC4 matrix material under the condition of 20MPa, argon atmospher protection at 1200 ℃, pressure.
Two, the TiC/TC4 matrix material is put into electrolytic solution; With the TiC/TC4 matrix material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 30 ℃; Adopting the bidirectional pulse power supply, is that 300～500V, negative pulse voltage are that 20～100V, positive pulse operating frequency are that 1000Hz, negative pulse operating frequency are that 1000Hz, dutycycle are under 20% the condition at positive pulse voltage, handles 30min;
The TiC/TC4 matrix material that three, will pass through the step 2 processing washes 3～5 times, and drying promptly gets arc differential oxide ceramic layer TiC/TC4 matrix material;
With the bonding strength of arc differential oxide ceramic layer TiC/TC4 composite material by adopting scratch method test arc differential oxide ceramic layer and TC4 alloy, its bonding force is difficult for peeling off, coming off greater than 85N; Arc differential oxide ceramic layer thickness is even, is 15～40 μ m, has the advantages of good abrasion performance, and arc differential oxide ceramic layer and GCr 15 steel balls are 0.6～0.7 to the frictional coefficient of mill, and the volume wear rate is 0.02 * 10
-6～0.15 * 10
-6Mm
3(mN)
-1
Experiment eight:
One, be that 15% ratio takes by weighing the TC4 powder and TiC powder (micron order) is a raw material according to TiC volumetric solid concentration in the TiC/TC4 matrix material; In glove box under the Ar atmosphere protection condition; Guarantee that ball-to-powder weight ratio is 10: 1; TC4 powder, TiC powder and GCr15 mill ball are packed in the batch mixing bottle, and the sealing back is to mix with ball mill under the condition of 120r/min at rotating speed, and mixing time is 24h.The mixed powder graphite jig of packing into is colded pressing, and is that insulation 1h obtains the TiC/TC4 matrix material under the condition of 20MPa, argon atmospher protection at 1200 ℃, pressure.
Two, the TiC/TC4 matrix material is put into electrolytic solution; With the TiC/TC4 matrix material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 30 ℃; Adopting the bidirectional pulse power supply, is that 300～500V, negative pulse voltage are that 20～100V, positive pulse operating frequency are that 1000Hz, negative pulse operating frequency are that 1000Hz, dutycycle are under 20% the condition at positive pulse voltage, handles 30min;
The TiC/TC4 matrix material that three, will pass through the step 2 processing washes 3～5 times, and drying promptly gets arc differential oxide ceramic layer TiC/TC4 matrix material;
With the bonding strength of arc differential oxide ceramic layer TiC/TC4 composite material by adopting scratch method test arc differential oxide ceramic layer and TC4 alloy, its bonding force is difficult for peeling off, coming off greater than 80N; Arc differential oxide ceramic layer thickness is even, is 10～40 μ m, has the advantages of good abrasion performance, and arc differential oxide ceramic layer and GCr 15 steel balls are 0.6～0.7 to the frictional coefficient of mill, and the volume wear rate is 0.02 * 10
-6～0.10 * 10
-6Mm
3(mN)
-1
Experiment nine:
One, be that 6% ratio takes by weighing the TC4 powder and TiC powder (micron order) is a raw material according to TiC volumetric solid concentration in the TiC/TC4 matrix material; In glove box under the Ar atmosphere protection condition; Guarantee that ball-to-powder weight ratio is 10: 1; TC4 powder, TiC powder and GCr15 mill ball are packed in the batch mixing bottle, and the sealing back is to mix with ball mill under the condition of 120r/min at rotating speed, and mixing time is 24h.The mixed powder graphite jig of packing into is colded pressing, and is that insulation 1h obtains the TiC/TC4 matrix material under the condition of 20MPa, argon atmospher protection at 1200 ℃, pressure.
Two, the TiC/TC4 matrix material is put into electrolytic solution; With the TiC/TC4 matrix material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 30 ℃; Adopting the bidirectional pulse power supply, is that 300～500V, negative pulse voltage are that 20～100V, positive pulse operating frequency are that 1000Hz, negative pulse operating frequency are that 1000Hz, dutycycle are under 20% the condition at positive pulse voltage, handles 30min;
The TiC/TC4 matrix material that three, will pass through the step 2 processing washes 3～5 times, and drying promptly gets arc differential oxide ceramic layer TiC/TC4 matrix material;
With the bonding strength of arc differential oxide ceramic layer TiC/TC4 composite material by adopting scratch method test arc differential oxide ceramic layer and TC4 alloy, its bonding force is difficult for peeling off, coming off greater than 75N; Arc differential oxide ceramic layer thickness is even, is 15～40 μ m, has the advantages of good abrasion performance, and arc differential oxide ceramic layer and GCr 15 steel balls are 0.55～0.65 to the frictional coefficient of mill, and the volume wear rate is 0.04 * 10
-6～0.20 * 10
-6Mm
3(mN)
-1
Experiment ten:
One, be that 6% ratio takes by weighing the TC4 powder and TiC powder (micron order) is a raw material according to TiC volumetric solid concentration in the TiC/TC4 matrix material; In glove box under the Ar atmosphere protection condition; Guarantee that ball-to-powder weight ratio is 10: 1; TC4 powder, TiC powder and GCr15 mill ball are packed in the batch mixing bottle, and the sealing back is to mix with ball mill under the condition of 120r/min at rotating speed, and mixing time is 24h.The mixed powder graphite jig of packing into is colded pressing, and is that insulation 1h obtains the TiC/TC4 matrix material under the condition of 20MPa, argon atmospher protection at 1200 ℃, pressure.
Two, the TiC/TC4 matrix material is put into electrolytic solution; With the TiC/TC4 matrix material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 20 ℃; Adopting the bidirectional pulse power supply, is that 400V, negative pulse voltage are that 5～100V, positive pulse operating frequency are that 1500Hz, negative pulse operating frequency are that 1500Hz, dutycycle are under 6～10% the condition at positive pulse voltage, handles 10min;
The TiC/TC4 matrix material that three, will pass through the step 2 processing washes 3～5 times, and drying promptly gets arc differential oxide ceramic layer TiC/TC4 matrix material;
With the bonding strength of arc differential oxide ceramic layer TiC/TC4 composite material by adopting scratch method test arc differential oxide ceramic layer and TC4 alloy, its bonding force is difficult for peeling off, coming off greater than 90N; Arc differential oxide ceramic layer thickness is even, is 15～40 μ m, has the advantages of good abrasion performance, and arc differential oxide ceramic layer and GCr 15 steel balls are 0.5～0.6 to the frictional coefficient of mill, and the volume wear rate is 0.05 * 10
-6～0.30 * 10
-6Mm
3(mN)
-1
Test 11:
One, be that 6% ratio takes by weighing the TC4 powder and TiC powder (micron order) is a raw material according to TiC volumetric solid concentration in the TiC/TC4 matrix material; In glove box under the Ar atmosphere protection condition; Guarantee that ball-to-powder weight ratio is 10: 1; TC4 powder, TiC powder and GCr15 mill ball are packed in the batch mixing bottle, and the sealing back is to mix with ball mill under the condition of 120r/min at rotating speed, and mixing time is 24h.The mixed powder graphite jig of packing into is colded pressing, and is that insulation 1h obtains the TiC/TC4 matrix material under the condition of 20MPa, argon atmospher protection at 1200 ℃, pressure.
Two, the TiC/TC4 matrix material is put into electrolytic solution; With the TiC/TC4 matrix material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 20 ℃; Adopting the bidirectional pulse power supply, is that 400V, negative pulse voltage are that 90V, positive pulse operating frequency are that 1500Hz, negative pulse operating frequency are that 1500Hz, dutycycle are under 8% the condition at positive pulse voltage, handles 10min;
The TiC/TC4 matrix material that three, will pass through the step 2 processing washes 4 times, 40～80 ℃ of dryings, promptly gets arc differential oxide ceramic layer TiC/TC4 matrix material;
With the bonding strength of arc differential oxide ceramic layer TiC/TC4 composite material by adopting scratch method test arc differential oxide ceramic layer and TC4 alloy, its bonding force is difficult for peeling off, coming off greater than 90N; Arc differential oxide ceramic layer thickness is even, is 20 μ m, has the advantages of good abrasion performance, and arc differential oxide ceramic layer and GCr 15 steel balls are 0.5 to the frictional coefficient of mill, and the volume wear rate is 0.05 * 10
-6Mm
3(mN)
-1
Find out the TiC particle that has a large amount of net distribution in the matrix by Fig. 1.
Claims (10)
1.TiC the preparation method of granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface is characterized in that the preparation method of TiC granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface carries out according to the following steps:
One, the TiC granule intensified titanium-base compound material is put into electrolytic solution; With the TiC granule intensified titanium-base compound material is that positive pole, iron plate are negative pole; The control electrolyte temperature is 10～60 ℃; Adopting the bidirectional pulse power supply, is that 200～800V, negative pulse voltage are that 0～400V, positive pulse operating frequency are that 200～2000Hz, negative pulse operating frequency are that 200～2000Hz, dutycycle are under 4～20% the condition at positive pulse voltage, handles 3～30min;
The TiC granule intensified titanium-base compound material that two, will pass through the step 1 processing washes 3～5 times, and drying promptly gets arc differential oxide ceramic layer TiC granule intensified titanium-base compound material;
Electrolytic solution described in the step 1 is made up of water glass, sodium aluminate, sodium phosphate, ethanol and deionized water, and electrolytic solution mesosilicic acid na concn is 3～35g/L, and concentration of sodium aluminate is 3～60g/L, and sodium phosphate concentration is 3～40g/L, and alcohol concn is 5～20ml/L.
2. according to the preparation method of the said TiC granule intensified titanium-base compound material of claim 1 micro-arc oxidation ceramic layer on surface; It is characterized in that the TiC particle as wild phase is with micron order or nano level in the granule intensified titanium-base compound material of TiC described in the step 1; Matrix in the TiC granule intensified titanium-base compound material is titanium, TC3 titanium alloy or TC4 titanium alloy, and the volume content of TiC is 3%～20% in the TiC granule intensified titanium-base compound material.
3. according to the preparation method of claim 1 or 2 said TiC granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface, it is characterized in that the voltage of positive pulse described in the step 1 is 300～700V.
4. according to the preparation method of claim 1 or 2 said TiC granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface, it is characterized in that the voltage of positive pulse described in the step 1 is 500～600V.
5. according to the preparation method of claim 1 or 2 said TiC granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface, it is characterized in that negative pulse voltage described in the step 1 is 0～300V.
6. according to the preparation method of claim 1 or 2 said TiC granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface, it is characterized in that negative pulse voltage described in the step 1 is 200V.
7. according to the preparation method of claim 1 or 2 said TiC granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface, it is characterized in that the operating frequency of positive pulse described in the step 1 is 400～1200Hz.
8. according to the preparation method of claim 1 or 2 said TiC granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface, it is characterized in that the operating frequency of negative pulse described in the step 1 is 1000Hz.
9. according to the preparation method of claim 1 or 2 said TiC granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface, it is characterized in that dutycycle described in the step 1 is 4～16%.
10. according to the preparation method of claim 1 or 2 said TiC granule intensified titanium-base compound material micro-arc oxidation ceramic layer on surface, it is characterized in that the temperature of exsiccant described in the step 2 is 40～80 ℃.
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