CN103774125A - Thermal treatment method of chemical nickel-phosphate plating alloy layer of aluminium alloy - Google Patents
Thermal treatment method of chemical nickel-phosphate plating alloy layer of aluminium alloy Download PDFInfo
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- CN103774125A CN103774125A CN201410046721.6A CN201410046721A CN103774125A CN 103774125 A CN103774125 A CN 103774125A CN 201410046721 A CN201410046721 A CN 201410046721A CN 103774125 A CN103774125 A CN 103774125A
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- aluminum alloy
- aluminium alloy
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- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 50
- 238000007747 plating Methods 0.000 title claims abstract description 38
- 238000007669 thermal treatment Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000000126 substance Substances 0.000 title abstract description 24
- 229910045601 alloy Inorganic materials 0.000 title abstract description 5
- 239000000956 alloy Substances 0.000 title abstract description 5
- 229910000159 nickel phosphate Inorganic materials 0.000 title abstract 3
- JOCJYBPHESYFOK-UHFFFAOYSA-K nickel(3+);phosphate Chemical compound [Ni+3].[O-]P([O-])([O-])=O JOCJYBPHESYFOK-UHFFFAOYSA-K 0.000 title abstract 3
- 238000001816 cooling Methods 0.000 claims abstract description 18
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004327 boric acid Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000002791 soaking Methods 0.000 claims abstract description 11
- LWHQXUODFPPQTL-UHFFFAOYSA-M sodium;2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-pentadecafluorooctanoate Chemical compound [Na+].[O-]C(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F LWHQXUODFPPQTL-UHFFFAOYSA-M 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000011248 coating agent Substances 0.000 claims description 27
- 238000000576 coating method Methods 0.000 claims description 27
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 25
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 230000001681 protective effect Effects 0.000 claims description 15
- 229910001096 P alloy Inorganic materials 0.000 claims description 13
- 229910052759 nickel Inorganic materials 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 230000001737 promoting effect Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 239000003223 protective agent Substances 0.000 abstract 4
- 239000013543 active substance Substances 0.000 abstract 1
- 239000011574 phosphorus Substances 0.000 description 10
- 229910052698 phosphorus Inorganic materials 0.000 description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 229910018104 Ni-P Inorganic materials 0.000 description 5
- 229910018536 Ni—P Inorganic materials 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 4
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910001453 nickel ion Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000010183 spectrum analysis Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- QDWJUBJKEHXSMT-UHFFFAOYSA-N boranylidynenickel Chemical compound [Ni]#B QDWJUBJKEHXSMT-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- -1 boron amide alkane Chemical class 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
Abstract
The invention discloses a thermal treatment method of a chemical nickel-phosphate plating alloy layer of aluminium alloy. The thermal treatment method comprises the following steps: firstly putting an aluminium alloy part in a constant temperature drying oven, heating to 200 DEG C, keeping the temperature constant for 30 minutes, then taking out, and cooling in air; secondly, adding perfluorooctanoic acid sodium salt to a boric acid spirit solution so as to serve as an active agent, stirring so as to form a thermal treatment protective agent, soaking the dried aluminium alloy part in the protective agent for 5-10 minutes at the temperature of 20 DEG C-40 DEG C; and finally putting the aluminium alloy part soaked in the thermal treatment protective agent in a 380 DEG C-450 DEG C muffle furnace for thermal treatment for 40-60 minutes at a constant temperature, then taking out, and carrying out air cooling. According to the thermal treatment method, through protective agent pretreatment, after the amorphous chemical nickel-phosphate plating layer is subjected to non vacuum thermal treatment, Hv is more than or equal to 850 DEG C and the color of the plating layer does not change.
Description
Technical field
The present invention relates to a kind of heat treating method of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy layer.
Background technology
Aluminium alloy has the features such as physical strength is high, density is little, heat-conductivity conducting is good, good toughness, easy processing, thereby in industry, be a most widely used class non-ferrous metal structured material, especially in aerospace, automobile, machinofacture, boats and ships and chemical industry, widely applying.Aluminum alloy surface covers the oxide film of one deck densification, and it can be kept apart aluminium alloy and surrounding environment, avoids oxidized.But this layer of oxide film is vulnerable to the corrosion of strong acid and highly basic, aluminium alloy easily produces intergranular corrosion simultaneously, and surface hardness is low, not wear-resisting.
Along with the development of industrial technology, the continuous expansion of Application Areas, service condition complicated, part prepared by aluminium alloy, as high-end automobile brake spool, refitting equipment connector, cabinet guide rail etc. have proposed surface hardness and the wear resistance requirement more and more done.Therefore to carry out wear resistance and improve hardness processing aluminum alloy surface.Use at present more technique to have: durionise, differential arc oxidation, chemical plating nickel-phosphorus alloy, chemical nickel plating ni-b alloy.(although 15 μ m) have high rigidity (850-1100Hv), owing to having very large environmental pollution, hexavalent chromium is strong carcinogen to aluminium alloy surface electric plating chromium, and country does not advocate, and does not also have sustainable developability.Carry out differential arc oxidation in aluminum alloy surface, can obtain hardness is the inside/outside duplicature of 450Hv and 1600Hv, but differential arc oxidation is only suitable for the component of simple shape, and power consumption is large.Chemical nickel plating has the following advantages: without energising, comparatively environmental protection; Thickness of coating and evenly, processing element is not limited by shape, indeformable, be particularly applicable to complex-shaped, the surface treatment of the high tiny and large component of dark blind hole and accuracy requirement; Have good anti-corrosion resisting property, have good solidity to corrosion in much acid, alkali, salt, ammonia and seawater, its solidity to corrosion is than superior many of stainless steel; Parts after treatment, surface smoothness is high, and surface-brightening does not need mechanical workout and polishing again, the use of can directly installing; The bonding force of coating and matrix is high, incrust, and its bonding force is higher than durionise and ion plating.So chemical nickel plating is the prefered method that improves aluminum alloy surface wear resistance and hardness.At present, conventional chemical Ni-P and two kinds of techniques of chemical nickel boron of mainly containing.Wherein chemical Ni-P can be divided into again low-phosphorous (phosphorous 2-5% mass percent), middle phosphorus (phosphorous 6-9% mass percent), high phosphorus (phosphorous 10-14% mass percent) according to the difference of phosphorus content.Under three kinds of composition plated states, coating is amorphous Ni-P alloy, plated state hardness is respectively 650-800Hv, 500-650Hv, 350-500Hv, the working conditions (Hv >=850) that meets high abrasion, high rigidity also will be heat-treated, but the hardness of low-phosphorous and middle phosphorus chemistry nickel-phosphorus coating does not rise counter falling after thermal treatment, only having high-phosphorus chemical nickel phosphorus coating to heat-treat above at 300 ℃ is to make hardness improve, various experimental results show, optimum treatment process is 400 ℃ of thermal treatment 1h, and the coating hardness obtaining can reach 900-1100Hv.(above-mentioned various nickel-phosphorus coating thickness is 15 μ m, and coating hardness adopts the test of HX1000 microhardness tester, and test condition is: 50g, 15s.) this is that Amorphous Ni-P Alloy layer starts crystallization, diffusion-precipitation Ni at 350 ℃
3p phase, improves coating hardness greatly, and reaches best at 400 ℃/1h, because along with temperature raises or time lengthening, and crystalline state Ni
3p constantly grows up mutually, can make on the contrary coating hardness reduce.(15 μ m) can reach 750-850Hv to the alloy layer that chemical nickel boron obtains under plated state state, substantially can meet wear resistance, but because boron amide alkane reductive agent is more expensive, average cost is 2-3 times of chemical nickel phosphorus plating, and technique is not mature and stable, so not yet heavy industrialization application at present.
By comprehensive comparison, electroless plating Nickel Phosphorus Alloy With High Phosphorus Content also carries out the ideal technology that 400 ℃/1h thermal treatment is acquisition high rigidity, high abrasion aluminium alloy spare and accessory parts.If but part carries out 400 ℃/1h thermal treatment under antivacuum, meeting coating makes surface oxidation variable color, and (experimental data surface temperature exceedes 305 ℃, coating will variable color), this is unallowed for a lot of environments for use, if heat-treated under vacuum environment, so because using and developing of this technique limited again in expensive, the little space of vacuum heat treatment furnace greatly.Therefore, how in non-vacuum environment thermal treatment, to guarantee that coating variable color does not occur and is oxidized and makes coating hardness to bring up to Hv >=850 to have very large research space and Research Significance.
Summary of the invention
The object of this invention is to provide a kind of heat treating method of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy layer, under antivacuum heat treated condition, improve hardness and the wear resistance of aluminum alloy surface chemical Ni-P layer.
A heat treating method after Electroless Nickel Plating of Aluminum Alloy phosphorus alloy, its step is as follows:
1) aluminum alloy surface is carried out chemical plating nickel-phosphorus alloy.
2) aluminum alloy part that is coated with 10-14wt% nickel-phosphorus alloy coating is placed in to thermostatic drying chamber, is heated to 200 ℃, constant temperature 30min, then takes out air cooling.
3) in boric acid spirit solution, add Sodium perfluorooctanoate as promoting agent, after stirring, form thermal treatment protective material, the aluminum alloy part after drying is put into protective material, soak 5-10min, soaking temperature is 20 ℃-40 ℃;
4) by soaking aluminum alloy part after thermal treatment protective material, to put into temperature be the retort furnace of 380 ℃-450 ℃, and constant temperature 40-60min thermal treatment, then takes out air cooling.
According to the present invention, described boric acid spirit solution, boric acid content is 4wt%.
According to the present invention, the Sodium perfluorooctanoate adding in described boric acid spirit solution is 1-5g/L.
Heat treating method of the present invention, can guarantee that chemical nickel phosphorus plating (phosphorous 10-14% mass percent) non-crystalline coating is after antivacuum thermal treatment, Hv >=850, and guarantee that coating color does not change, compared with vacuum heat treatment, can be cost-saving, and break through the less limitation in vacuum oven space, expand the application of high phosphorus chemical plating nickel-phosphorus alloy on aluminum alloy part surface, also expanded the application of aluminium alloy at high performance requirements industrial circle.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described, but non-limitation of the present invention.
Embodiment 1:
The automobile valve core that 180 6061 rodss and bars of aluminium alloy are processed into carries out acidic chemical nickel phosphor plating and covers, and chemical nickel phosphorus plating plating technic parameter is pH value 4.5, nickel ion content 5.6g/L, 90 ℃ of temperature, time 100min.
Aluminum alloy part after 60 platings is placed in to thermostatic drying chamber, is heated to 200 ℃, constant temperature 30min, then takes out air cooling; In the alcohol that is dissolved with 4wt% boric acid, add the Sodium perfluorooctanoate of 1g/L as promoting agent; after stirring, form thermal treatment protective material; aluminum alloy part after drying is put into protective material; soak 5min; soaking temperature is 20 ℃, and by soaking aluminum alloy part after thermal treatment protective material, to put into temperature be the retort furnace of 380 ℃, constant temperature 40min thermal treatment; then take out air cooling.
As a comparison, the aluminum alloy part after 60 platings is directly put into R03 vacuum oven (vacuum tightness 10
-2pa) 380 ℃ of constant temperature 40min thermal treatment, furnace cooling.
As a comparison, it is the retort furnace of 380 ℃ that the aluminum alloy part after 60 platings is directly put into temperature, and then constant temperature 40min thermal treatment take out air cooling.
Adopt XRF2000X ray layer thickness meter to measure thickness of coating, (test condition is: 50g to adopt HV1000 microhardness tester to measure coating hardness, 15s, measuring 3 some positions averages), the EDS energy spectrum analysis coating phosphorus content that adopts InspectF50 field emission scanning electron microscope to be equipped with.
Test result is as shown in table 1:
Embodiment 2:
The automobile valve core that 180 6061 rodss and bars of aluminium alloy are processed into carries out acidic chemical nickel phosphor plating and covers, and chemical nickel phosphorus plating plating technic parameter is pH value 4.8, nickel ion content 5.8g/L, 90 ℃ of temperature, time 100min.
Aluminum alloy part after 60 platings is placed in to thermostatic drying chamber, is heated to 200 ℃, constant temperature 30min, then takes out air cooling; In the alcohol that is dissolved with 4wt% boric acid, add the Sodium perfluorooctanoate of 3g/L as promoting agent; after stirring, form thermal treatment protective material; aluminum alloy part after drying is put into protective material; soak 10min; soaking temperature is 40 ℃, and by soaking aluminum alloy part after thermal treatment protective material, to put into temperature be the retort furnace of 450 ℃, constant temperature 50min thermal treatment; then take out air cooling.
As a comparison, the aluminum alloy part after 60 platings is directly put into R03 vacuum oven (vacuum tightness 10
-2pa) 450 ℃ of constant temperature 50min thermal treatment, furnace cooling.
As a comparison, it is the retort furnace of 450 ℃ that the aluminum alloy part after 60 platings is directly put into temperature, and then constant temperature 50min thermal treatment take out air cooling.
Adopt XRF2000X ray layer thickness meter to measure thickness of coating, (test condition is: 50g to adopt HV1000 microhardness tester to measure coating hardness, 15s, measuring 3 some positions averages), the EDS energy spectrum analysis coating phosphorus content that adopts InspectF50 field emission scanning electron microscope to be equipped with.
Test result is as shown in table 2:
Embodiment 3:
The automobile valve core that 180 6061 rodss and bars of aluminium alloy are processed into carries out acidic chemical nickel phosphor plating and covers, and chemical nickel phosphorus plating plating technic parameter is pH value 4.7, nickel ion content 5.8g/L, 90 ℃ of temperature, time 100min.
Aluminum alloy part after 60 platings is placed in to thermostatic drying chamber, is heated to 200 ℃, constant temperature 30min, then takes out air cooling; In the alcohol that is dissolved with 4wt% boric acid, add the Sodium perfluorooctanoate of 5g/L as promoting agent; after stirring, form thermal treatment protective material; aluminum alloy part after drying is put into protective material; soak 8min; soaking temperature is 30 ℃, and by soaking aluminum alloy part after thermal treatment protective material, to put into temperature be the retort furnace of 400 ℃, constant temperature 60min thermal treatment; then take out air cooling.
As a comparison, the aluminum alloy part after 60 platings is directly put into R03 vacuum oven (vacuum tightness 10
-2pa) 400 ℃ of constant temperature 60min thermal treatment, furnace cooling.
As a comparison, it is the retort furnace of 400 ℃ that the aluminum alloy part after 60 platings is directly put into temperature, and then constant temperature 60min thermal treatment take out air cooling.
Adopt XRF2000X ray layer thickness meter to measure thickness of coating, (test condition is: 50g to adopt HV1000 microhardness tester to measure coating hardness, 15s, measuring 3 some positions averages), the EDS energy spectrum analysis coating phosphorus content that adopts InspectF50 field emission scanning electron microscope to be equipped with.
Test result is as shown in table 3:
Claims (3)
1. a heat treating method for Electroless Nickel Plating of Aluminum Alloy phosphorus alloy layer, is characterized in that comprising the steps:
1) aluminum alloy part that is coated with 10-14wt% nickel-phosphorus alloy coating is placed in to thermostatic drying chamber, is heated to 200 ℃, constant temperature 30min, then takes out air cooling;
2) in boric acid spirit solution, add Sodium perfluorooctanoate as promoting agent, after stirring, form thermal treatment protective material, after drying, aluminum alloy part immerses protective material, soaks 5-10min, and soaking temperature is 20 ℃-40 ℃;
3) by soaking aluminum alloy part after thermal treatment protective material, to put into temperature be the retort furnace of 380 ℃-450 ℃, and constant temperature 40-60min thermal treatment, then takes out air cooling.
2. the heat treating method after a kind of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy according to claim 1, is characterized in that: described boric acid spirit solution, boric acid content is 4wt%.
3. the heat treating method after a kind of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy according to claim 1, is characterized in that: the Sodium perfluorooctanoate adding in described boric acid spirit solution is 1-5g/L.
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| CN201410046721.6A CN103774125B (en) | 2014-02-10 | 2014-02-10 | A kind of heat treatment method of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy layer |
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| CN201410046721.6A CN103774125B (en) | 2014-02-10 | 2014-02-10 | A kind of heat treatment method of Electroless Nickel Plating of Aluminum Alloy phosphorus alloy layer |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105087883A (en) * | 2015-09-25 | 2015-11-25 | 尚成荣 | Protective agent applicable to heat treatment for checking tool used for pedal type sawing machine |
| CN105132660A (en) * | 2015-09-25 | 2015-12-09 | 尚成荣 | Heat processing method of foot-operated type sawing machine fixture |
| CN105238914A (en) * | 2015-09-25 | 2016-01-13 | 尚成荣 | Method for preparing thermal treatment protective agent for detecting tool for detection of foot-pedal sawing machine |
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|---|---|---|---|---|
| EP0023678A1 (en) * | 1979-08-01 | 1981-02-11 | Kennecott Corporation | Process for preparing hard granular activated carbon manufactured from sub-bituminous coal treated with solid boric acid |
| CN1603465A (en) * | 2004-08-31 | 2005-04-06 | 中国兵器工业第五九研究所 | Treatment process for synergistic fluoropolymer coating on magnesium and its alloy |
| CN1609273A (en) * | 2003-05-09 | 2005-04-27 | 昭和电工株式会社 | Corrosion resistant material, and its production method |
| CN101705480A (en) * | 2009-11-03 | 2010-05-12 | 燕山大学 | Chemical modification technology of chemical nickel phosphorus plating alloy coating |
-
2014
- 2014-02-10 CN CN201410046721.6A patent/CN103774125B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0023678A1 (en) * | 1979-08-01 | 1981-02-11 | Kennecott Corporation | Process for preparing hard granular activated carbon manufactured from sub-bituminous coal treated with solid boric acid |
| CN1609273A (en) * | 2003-05-09 | 2005-04-27 | 昭和电工株式会社 | Corrosion resistant material, and its production method |
| CN1603465A (en) * | 2004-08-31 | 2005-04-06 | 中国兵器工业第五九研究所 | Treatment process for synergistic fluoropolymer coating on magnesium and its alloy |
| CN101705480A (en) * | 2009-11-03 | 2010-05-12 | 燕山大学 | Chemical modification technology of chemical nickel phosphorus plating alloy coating |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105087883A (en) * | 2015-09-25 | 2015-11-25 | 尚成荣 | Protective agent applicable to heat treatment for checking tool used for pedal type sawing machine |
| CN105132660A (en) * | 2015-09-25 | 2015-12-09 | 尚成荣 | Heat processing method of foot-operated type sawing machine fixture |
| CN105238914A (en) * | 2015-09-25 | 2016-01-13 | 尚成荣 | Method for preparing thermal treatment protective agent for detecting tool for detection of foot-pedal sawing machine |
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| CN103774125B (en) | 2016-05-04 |
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