CN101781755B - Method for preparing aluminum-based alloy with Al-Si-O-N wearproof anticorrosive layer - Google Patents
Method for preparing aluminum-based alloy with Al-Si-O-N wearproof anticorrosive layer Download PDFInfo
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- CN101781755B CN101781755B CN2010101207167A CN201010120716A CN101781755B CN 101781755 B CN101781755 B CN 101781755B CN 2010101207167 A CN2010101207167 A CN 2010101207167A CN 201010120716 A CN201010120716 A CN 201010120716A CN 101781755 B CN101781755 B CN 101781755B
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 56
- 239000000956 alloy Substances 0.000 title claims abstract description 40
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 37
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910006360 Si—O—N Inorganic materials 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 10
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 15
- 239000000919 ceramic Substances 0.000 claims abstract description 11
- 238000009792 diffusion process Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 7
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract 2
- 238000000151 deposition Methods 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 23
- 239000011159 matrix material Substances 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 238000005238 degreasing Methods 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 14
- 230000000694 effects Effects 0.000 claims description 13
- 230000008021 deposition Effects 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 238000000746 purification Methods 0.000 claims description 8
- 239000012159 carrier gas Substances 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 239000000356 contaminant Substances 0.000 claims description 7
- 238000011109 contamination Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 238000005268 plasma chemical vapour deposition Methods 0.000 claims description 7
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 7
- 239000013049 sediment Substances 0.000 claims description 7
- 235000017550 sodium carbonate Nutrition 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- PXLIDIMHPNPGMH-UHFFFAOYSA-N sodium chromate Chemical compound [Na+].[Na+].[O-][Cr]([O-])(=O)=O PXLIDIMHPNPGMH-UHFFFAOYSA-N 0.000 claims description 7
- 238000013517 stratification Methods 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims 1
- 229910000838 Al alloy Inorganic materials 0.000 abstract description 17
- 230000035939 shock Effects 0.000 abstract description 6
- 229910018516 Al—O Inorganic materials 0.000 abstract description 3
- 238000005452 bending Methods 0.000 abstract description 3
- 239000010410 layer Substances 0.000 abstract 3
- 239000002344 surface layer Substances 0.000 abstract 2
- 230000008595 infiltration Effects 0.000 abstract 1
- 238000001764 infiltration Methods 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 239000002585 base Substances 0.000 description 26
- 239000000463 material Substances 0.000 description 9
- 230000003213 activating effect Effects 0.000 description 6
- 238000000280 densification Methods 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 238000010791 quenching Methods 0.000 description 5
- 230000000171 quenching effect Effects 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 230000003245 working effect Effects 0.000 description 2
- UPLPHRJJTCUQAY-WIRWPRASSA-N 2,3-thioepoxy madol Chemical compound C([C@@H]1CC2)[C@@H]3S[C@@H]3C[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@](C)(O)[C@@]2(C)CC1 UPLPHRJJTCUQAY-WIRWPRASSA-N 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- 229910018104 Ni-P Inorganic materials 0.000 description 1
- 229910002650 Ni-SiC Inorganic materials 0.000 description 1
- 229910018536 Ni—P Inorganic materials 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910007991 Si-N Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910006294 Si—N Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 238000004372 laser cladding Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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Abstract
The invention discloses a method for preparing an aluminum-based alloy with an Al-Si-O-N wearproof anticorrosive layer, which comprises the following steps of: performing routine chemical preoxidation treatment to form a micropore surface layer with an Al-O structure on the surface of the aluminum-based alloy; on the basis, performing radio-frequency plasma chemical vapor deposition on Si and N to penetrate Si and N atoms into a micropore film with the Al-O structure; and forming the aluminum-based alloy of which the surface contains an Al-Si-O-N ceramic layer through diffusion and infiltration of Si, Al, O and N elements. The Al-Si-O-N layer of the invention has the characteristics of certain toughness, high intensity, high temperature resistance, high hardness, high bending strength, high abrasive resistance, high corrosive resistance, high thermal shock resistance and the like and endows the aluminum alloy with new surface property; and the Al-Si-O-N surface layer and an aluminum alloy substrate have high binding force.
Description
Technical field
The present invention relates to wear-resistant pantal alloy material preparation method, especially relate to the aluminum base alloy preparation method of the wear-resistant anticorrosion layer of a kind of Al-Si-O-N of having.
Background technology
Aluminum base alloy is the lightweight structural material of industrial circle widespread use, aluminum base alloy rigidity is low then, frictional coefficient is big, be difficult to lubricate, the deficiency of performances such as wear resistance and seizure resistance difference, influence the range of application and the work-ing life of aluminum base alloy, greatly limited the application of aluminum base alloy on the automobile with relatively sliding requirement, motorcycle, aerospace component.
The chemical property of aluminium is active, and the aluminum base alloy surface often has fine and close natural oxide film, but the natural oxide film physical strength of tens dust thickness is low, easily goes to pot, and is very limited to the provide protection of matrix, can't satisfy the various strict demands of modern industry development.Surface Hardening Treatment is the key that promotes the aluminum base alloy over-all properties, handle as aluminum alloy surface strengthenings such as anodic oxidation, plasma electrolytic oxidation, differential arc oxidations, though these technologies can suitably improve the strong bonded top coat of surface hardness, acquisition and the matrix of aluminium, but the porous structure alumina layer that the aluminum base alloy surface forms, can not resist the corrosion that contains the chlorion media environment, the raising of wear resistance and seizure resistance is not obvious simultaneously.Development along with the modern Application technology, plasma spraying process and Laser Cladding Treatment method obtain to use in the aluminum base alloy surface Hardening Treatment in succession, aluminium and aluminum alloy surface nitriding method are disclosed as patent CN86105732A, to improve aluminium and intensity of aluminum alloy and wear resistance, the characteristics of higher processing temperature requirement are extremely improper for the lower aluminium alloy of fusing point, easily cause the havoc of body material performance.And sol-gel method, brush plates local high speed electro-deposition method, Ni-P anodised aluminium pore packing lubrication material, in the hope of strengthening the anti-wear and wear-resistant performance of aluminum base alloy, patent CN1227282A discloses aluminium alloy cylinder inner wall nickel pottery (Ni-SiC) composite plating process, make engine cylinder durable in use, power stability, but there is the composition sudden change between this surface composite layer and the matrix, top layer and matrix are discontinuous, there is bigger thermal stresses, cause that peeling in use appears in coating, be full of cracks, phenomenon such as tiny crack and foaming causes performance can't reach service requirements and fails really to be adopted by actual production.
Summary of the invention
The object of the present invention is to provide the aluminum base alloy preparation method of the wear-resistant anticorrosion layer of a kind of Al-Si-O-N of having, the applied chemistry vapor phase process is at aluminum base alloy material, the wear-resistant anticorrosion layer of piece surface uniform deposition Al-Si-O-N, form new surface tissue, improve wear resistant friction reducing, the corrosion resistance of aluminum base alloy.
Al-Si-O-N is a kind of settled layer with ceramic characteristics, and it is high temperature resistant, high strength, and certain toughness is arranged, and has unusual high rigidity, bending strength, anti-friction wear-resistant, corrosion-resistant, resistance to sudden heating and radiation resistance, excellent electric insulating and thermal conductivity.The Al-O group that aluminum alloy material surface often has, similar to Si-O, Si-N unit structure, can ooze mutually under proper condition, dissolve each other forms the Al-Si-O-N ceramic layer.The present invention adopts the aluminum base alloy surface preoxidizing, ammonia and silane gas low-temperature decomposition, chemical gas phase reaction deposition obtain the novel surface of Al-Si-O-N structure, by meticulous component proportions of regulating Si, Al, O, N element, control Si, Al, O, N elemental diffusion and process of osmosis, change aluminum base alloy upper layer composition, structure and with the bonding force of matrix, obtain densification, adhesion, the meticulous controlled Al-Si-O-N ceramic layer of structure, improve the comprehensive mechanical performance of aluminum base alloy.
The step of the technical solution used in the present invention is as follows:
Step 1: the aluminum base alloy matrix carries out pre-oxidation treatment
Surface contaminants and oxide compound are removed in (1-1) mechanical polishing;
(1-2) the ultrasonic wave acetone soln cleans 10～15min, and deionized water rinsing is removed surface contamination and degreasing degreasing;
(1-3) with NaOH or KOH electrochemical deoiling, concentration is 2～5g/L, and the oil removing time is 2～10min, and with nitric acid neutralization, concentration of nitric acid is 100～200g/L, in and the time be 2～10min;
(1-4) preoxidation, at soda ash: the Sodium chromate weight percent is 1: 3～5, and concentration is 50～100g/L, 90～100 ℃ of treatment temps, preoxidation time 3～8min, deionized water rinsing dries up, and obtains having the surface tissue of preoxidation film;
Step 2: the aluminum base alloy matrix with preoxidation film carries out the plasma CVD depositing treatment, and preparation contains the upper layer of Al, O, Si and N component
(2-1) pretreated sample is packed in the PECVD CVD (Chemical Vapor Deposition) chamber, system is evacuated down to 3Pa, logical high-purity H
2Open radio frequency, produce glow discharge and bombard purification activating aluminum alloy surface 10～20min in advance, make its surface active, purification, heat to 300～500 ℃;
(2-2) with N
2Be carrier gas, logical SiH
4And NH
3The work source of the gas, gas flow rate is 120ml/min～200ml/min, source gas flow ratio: N
2: SiH
4: NH
3=9: 1: 2～9, deposition pressure 10～200Pa, radio frequency power 60～150w, depositing time 10～30min obtains containing the upper layer of Al, O, Si and N component;
Step 3: the upper layer aluminum base alloy matrix that contains Al, O, Si and N component carries out heat diffusion treatment
Control sediment chamber temperature is 450-500 ℃, continues the logical H with 50-100ml/min
2, it is constant that pressure keeps, insulation 60min, impel and be adsorbed on surperficial activity [Si], [N] atom to internal divergence, and generate the Al-Si-O-N ceramic film with the effect of preoxidation stratification, below the furnace cooling to 100 ℃, take out the alumina-base material that obtains having the Al-Si-O-N rete.
Described source of the gas is through N
2Dilute Si H
4Concentration be 10%, high-purity N H
3Purity be 99.999%, high-purity H
2Purity be 99.999%.
Described PECVD chemical vapor depsotition equipment is that HQ-2 type radio-frequency plasma strengthens chemical vapor depsotition equipment.
The beneficial effect that the present invention has is:
Al-Si-O-N layer of the present invention has characteristics such as certain toughness, high strength, high temperature resistant, high rigidity, bending strength, anti-friction wear-resistant, corrosion-resistant, resistance to sudden heating and gives aluminium alloy new surface property, Al-Si-O-N upper layer and alloy matrix aluminum bonding force are strong, dense structure, internal stress is little, greatly improves the work-ing life with relatively sliding aluminum alloy part.
Embodiment
Embodiment 1:
Step 1: ZL101 commonly used is a matrix with industry, carries out pre-oxidation treatment:
(1) surface contaminants and oxide compound are removed in mechanical polishing;
(2) the ultrasonic wave acetone soln cleans 10min, and deionized water rinsing is removed surface contamination and degreasing degreasing;
(3) alkali electroless oil removing, 2g/L sodium hydroxide solution normal temperature washing 2min, in the 100g/L salpeter solution and 2min, rinsed with deionized water, being continuously uniformly until surperficial moisture film, moisture film is that oil removing is clean;
(4) preoxidation, at soda ash: Sodium chromate is 1: 3, and concentration is in the 50g/L solution, 90 ℃ of preoxidation 3min clean 10min at the deionized water for ultrasonic ripple then, obtain having the surface tissue of preoxidation film.
Step 2: the ZL101 with preoxidation film carries out the plasma CVD depositing treatment, and preparation contains the upper layer of Al, O, Si, N component:
(1) pretreated sample is packed in the PECVD CVD (Chemical Vapor Deposition) chamber, system is evacuated down to 3Pa, logical high-purity H
2Open radio frequency generation glow discharge and bombard purification in advance, activating aluminum alloy surface 10min.And be heated to 300 ℃;
(2) with N
2Be carrier gas, logical SiH
4, NH
3Work gas, gas flow rate is 120ml/min, source gas flow ratio: N
2: SiH
4: NH
3=9: 1: 2, deposition pressure 10Pa, radio frequency power 60w, depositing time 10min obtains containing the upper layer of Al, O, Si, N component.
Step 3: heat diffusion treatment, control sediment chamber temperature is at 450 ℃, and it is constant that pressure keeps, and continues the logical H with 50ml/min
2, insulation 60min impels the activity [Si], [N] atom that are adsorbed on the surface to internal divergence, and generates the Al-Si-O-N ceramic film with the effect of preoxidation stratification, below the furnace cooling to 100 ℃, takes out the alumina-base material that obtains having the Al-Si-O-N rete.Sem analysis shows the about 20 μ m of thickness, and rete and matrix bond are good, film smooth surface, densification, and film hardness reaches 108HV, handles through 10 thermal shock quenchings, bubble, peeling, peeling phenomenon do not occur.
Embodiment 2:
Step 1: the ZL101 commonly used with industry is matrix, carries out pre-oxidation treatment:
(1) surface contaminants and oxide compound are removed in mechanical polishing;
(2) the ultrasonic wave acetone soln cleans 15min, and deionized water rinsing is removed surface contamination and degreasing degreasing;
(3) alkali electroless oil removing, the 5g/L potassium hydroxide solution, normal temperature washing 10min, in the 200g/L salpeter solution and 10min, rinsed with deionized water, being continuously uniformly until surperficial moisture film, moisture film is that oil removing is clean;
(4) preoxidation, at soda ash: Sodium chromate is 1: 5, and concentration is in the 100g/L solution, preoxidation 8min under 100 ℃ of temperature cleans 15min at the deionized water for ultrasonic ripple then, obtains having the surface tissue of preoxidation film.
Step 2: the ZL101 with preoxidation film carries out the plasma CVD depositing treatment, and preparation contains the upper layer of Al, O, Si, N component:
(1) pretreated sample is packed in the PECVD CVD (Chemical Vapor Deposition) chamber, system vacuumizes 3Pa, logical high-purity H
2Open radio frequency generation glow discharge and bombard purification in advance, activating aluminum alloy surface 20min, and be heated to 500 ℃;
(2) with N
2Be carrier gas, logical SiH
4, NH
3Work gas, gas flow rate is 200ml/min, source gas flow ratio: N
2: SiH
4: NH
3=9: 1: 9, control deposition pressure 200Pa, radio frequency power 150w, depositing time 30min obtains containing the upper layer of Al, O, Si, N component.
Step 3: heat diffusion treatment, control sediment chamber temperature is at 500 ℃, and it is constant that pressure keeps, and continues the logical H with 100ml/min
2, insulation 60min impels the activity [Si], [N] atom that are adsorbed on the surface to internal divergence, and generates the Al-Si-O-N ceramic film with the effect of preoxidation stratification, below the furnace cooling to 100 ℃, takes out the alumina-base material that obtains having the Al-Si-O-N rete.Sem analysis shows that thickness is 35 μ m, and rete and matrix bond are good, film smooth surface, densification, and film hardness reaches 180HV, handles through 10 thermal shock quenchings, bubble, peeling, peeling phenomenon do not occur.
Embodiment 3
Step 1: the ZL101 commonly used with industry is matrix, carries out pre-oxidation treatment:
(1) surface contaminants and oxide compound are removed in mechanical polishing;
(2) the ultrasonic wave acetone soln cleans 12min, and deionized water rinsing is removed surface contamination and degreasing degreasing;
(3) alkali electroless oil removing, the 3g/L sodium hydroxide solution, normal temperature washing 5min, in the 150g/L salpeter solution and 6min, rinsed with deionized water, being continuously uniformly until surperficial moisture film, moisture film is that oil removing is clean;
(4) preoxidation, at soda ash: Sodium chromate is 1: 4, and concentration is in the 75g/L solution, preoxidation 4min under 95 ℃ of temperature cleans 12min at the deionized water for ultrasonic ripple then, obtains having the surface tissue of preoxidation film.
Step 2: the ZL101 with preoxidation film carries out the plasma CVD depositing treatment, and preparation contains the upper layer of Al, O, Si, N component:
(1) pretreated sample is packed in the PECVD CVD (Chemical Vapor Deposition) chamber, system vacuumizes 3Pa, logical high-purity H
2Open radio frequency and produce glow discharge and bombard in advance and purify 15min, activating aluminum alloy surface, and heating sample to 400 ℃;
(2) with N
2Be carrier gas, SiH
4, NH
3Be reactant gas source, gas flow rate is 150ml/min, source gas flow ratio: N
2: SiH
4: NH
3=9: 1: 4, deposition pressure 100Pa, radio frequency power 120w, 400 ℃ of depositing temperatures, depositing time 20min obtains containing the upper layer of Al, O, Si, N component.
Step 3: heat diffusion treatment, control sediment chamber temperature is at 500 ℃, and it is constant that pressure keeps, and continues the logical H with 75ml/min
2, insulation 60min impels the activity [Si], [N] atom that are adsorbed on the surface to internal divergence, and generates the Al-Si-O-N ceramic film with the effect of preoxidation stratification, below the furnace cooling to 100 ℃, takes out the alumina-base material that obtains having the Al-Si-O-N rete.Sem analysis shows that thickness is 30 μ m, and rete and matrix bond are good, film smooth surface, densification, and film hardness reaches 170HV, handles through 10 thermal shock quenchings, bubble, peeling, peeling phenomenon do not occur.
Embodiment 4
Step 1: with industry ADC12 alloy commonly used is matrix, carries out pre-oxidation treatment:
(1) surface contaminants and oxide compound are removed in mechanical polishing;
(2) the ultrasonic wave acetone soln cleans 10min, and deionized water rinsing is removed surface contamination and degreasing degreasing;
(3) alkali electroless oil removing, the 2g/L sodium hydroxide solution, normal temperature washing 2min, in the 100g/L salpeter solution and 3min, rinsed with deionized water, being continuously uniformly until surperficial moisture film, moisture film is that oil removing is clean;
(4) preoxidation, at soda ash: Sodium chromate is 1: 3, and concentration is in the 50g/L solution, and preoxidation 3min under 90 ℃ of temperature then through deionized water ultrasonic cleaning 10min, obtains having the surface tissue of preoxidation film.
Step 2: the ADC12 alloy with preoxidation film carries out the plasma CVD depositing treatment, and preparation contains the upper layer of Al, O, Si, N component:
(1) pretreated ADC12 alloy is packed in the CVD (Chemical Vapor Deposition) chamber, system is evacuated down to 3Pa, and logical high-purity H2 opens radio frequency and produces glow discharge and bombard purification in advance, activating aluminum alloy surface 15min, and heated sample to 300 ℃;
(2) with N
2Be carrier gas, gas flow rate is 120ml/min, source gas flow ratio: N
2: SiH
4: NH
3=9: 1: 2, control deposition pressure 10Pa, radio frequency power 80w, depositing time 20min obtains containing the upper layer of Al, O, Si, N component.
Step 3: heat diffusion treatment, control sediment chamber temperature is at 450 ℃, and it is constant that pressure keeps, and continues the logical H with 100ml/min
2, insulation 60min impels the activity [Si], [N] atom that are adsorbed on the surface to internal divergence, and generates the Al-Si-O-N ceramic film with the effect of preoxidation stratification, below the furnace cooling to 100 ℃, takes out the alumina-base material that obtains having the Al-Si-O-N rete.Sem analysis shows that thickness is 25 μ m, and rete and matrix bond are good, film smooth surface, densification, and film hardness reaches 175HV, handles through 10 thermal shock quenchings, bubble, peeling, peeling phenomenon do not occur.
Embodiment 5
Step 1: the ADC12 alloy commonly used with industry is matrix, carries out pre-oxidation treatment:
(1) surface contaminants and oxide compound are removed in mechanical polishing;
(2) the ultrasonic wave acetone soln cleans 15min, and deionized water rinsing is removed surface contamination and degreasing degreasing;
(3) alkali electroless oil removing, the 5g/L sodium hydroxide solution, normal temperature washing 5min, in the 200g/L salpeter solution and 5min, rinsed with deionized water, being continuously uniformly until surperficial moisture film, moisture film is that oil removing is clean;
(4) preoxidation, at soda ash: Sodium chromate is 1: 5, and concentration is in the 100g/L solution, preoxidation 5min under 95 ℃ of temperature cleans 15min at the deionized water for ultrasonic ripple then, obtains having the surface tissue of preoxidation film.
Step 2: the ADC12 alloy with preoxidation film carries out the plasma CVD depositing treatment, and preparation contains the upper layer of Al, O, Si, N component:
(1) pretreated sample is packed in the CVD (Chemical Vapor Deposition) chamber, system is evacuated down to 3Pa, logical high-purity H
2Open radio frequency and produce glow discharge and bombard purification in advance, activating aluminum alloy surface 10min, and heated sample to 500 ℃;
(2) with N
2Be carrier gas, SiH
4, NH
3Be reactant gas source, gas flow rate is 200ml/min, gas flow ratio: N
2: SiH
4: NH
3=9: 1: 4, deposition pressure 100Pa, radio frequency power 120w, 500 ℃ of depositing temperatures, depositing time 30min obtains containing the upper layer of Al, O, Si, N component.
Step 3: heat diffusion treatment, control sediment chamber temperature is at 500 ℃, and it is constant that pressure keeps, and continues the logical H with 100ml/min
2, insulation 60min impels the activity [Si], [N] atom that are adsorbed on the surface to internal divergence, and generates the Al-Si-O-N ceramic film with the effect of preoxidation stratification, below the furnace cooling to 100 ℃, takes out the alumina-base material that obtains having the Al-Si-O-N rete.Sem analysis shows the about 30 μ m of thickness, and rete and matrix bond are good, film smooth surface, densification, and film hardness reaches 200HV, handles through 10 thermal shock quenchings, bubble, peeling, peeling phenomenon do not occur.
Claims (3)
1. aluminum base alloy preparation method with the wear-resistant anticorrosion layer of A1-Si-O-N is characterized in that the step of this method is as follows:
Step 1: the aluminum base alloy matrix carries out pre-oxidation treatment
Surface contaminants and oxide compound are removed in (1-1) mechanical polishing;
(1-2) the ultrasonic wave acetone soln cleans 10～15min, and deionized water rinsing is removed surface contamination and degreasing degreasing;
(1-3) with NaOH or KOH electrochemical deoiling, concentration is 2～5g/L, and the oil removing time is 2～10min, and with nitric acid neutralization, concentration of nitric acid is 100～200g/L, in and the time be 2～10min;
(1-4) preoxidation, at soda ash: the Sodium chromate weight percent is 1: 3～5, and concentration is 50～100g/L, 90～100 ℃ of treatment temps, preoxidation time 3～8min, deionized water rinsing dries up, and obtains having the surface tissue of preoxidation film;
Step 2: the aluminum base alloy matrix with preoxidation film carries out the plasma CVD depositing treatment, and preparation contains the upper layer of Al, O, Si and N component
(2-1) pretreated sample is packed in the PECVD CVD (Chemical Vapor Deposition) chamber, system is evacuated down to 3Pa, logical high-purity H
2Open radio frequency, produce glow discharge and bombard purification activation aluminum base alloy surface 10～20min in advance, make its surface active, purification, heat to 300～500 ℃;
(2-2) with N
2Be carrier gas, logical SiH
4And NH
3The work source of the gas, gas flow rate is 120ml/min～200ml/min, source gas flow ratio: N
2: SiH
4: NH
3=9: 1: 2～9, deposition pressure 10～200Pa, radio frequency power 60～150w, depositing time 10～30min obtains containing the upper layer of Al, O, Si and N component;
Step 3: the upper layer aluminum base alloy matrix that contains Al, O, Si and N component carries out heat diffusion treatment
Control sediment chamber temperature is 450-500 ℃, continues the logical H with 50-100ml/min
2, it is constant that pressure keeps, insulation 60min, impel and be adsorbed on surperficial active Si, N atom to internal divergence, and generate the Al-Si-O-N ceramic film with the effect of preoxidation stratification, below the furnace cooling to 100 ℃, take out the aluminum base alloy that obtains having the wear-resistant anticorrosion layer of Al-Si-O-N.
2. a kind of aluminum base alloy preparation method with the wear-resistant anticorrosion layer of Al-Si-O-N according to claim 1 is characterized in that: described source of the gas is through N
2Dilute Si H
4Concentration be 10%, high-purity N H
3Purity be 99.999%, high-purity H
2Purity be 99.999%.
3. a kind of aluminum base alloy preparation method with the wear-resistant anticorrosion layer of Al-Si-O-N according to claim 1 is characterized in that: described PECVD chemical vapor depsotition equipment is that HQ-2 type radio-frequency plasma strengthens chemical vapor depsotition equipment.
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| CN101161857A (en) * | 2007-11-15 | 2008-04-16 | 浙江理工大学 | Aluminum alloy surface treatment method |
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